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Serial block-face electron microscopy (SBEM) provides nanoscale 3D ultrastructure of embedded and stained cells and tissues in volumes of up to 107 µm3. In SBEM, electrons with 1–3 keV energies are incident on a specimen block, from which backscattered electron (BSE) images are collected with x, y resolution of 5–10 nm in the block-face plane, and successive layers are removed by an in situ ultramicrotome. Spatial resolution along the z-direction, however, is limited to around 25 nm by the minimum cutting thickness. To improve the z-resolution, we have extracted depth information from BSE images acquired at dual primary beam energies, using Monte Carlo simulations of electron scattering. The relationship between depth of stain and ratio of dual-energy BSE intensities enables us to determine 3D structure with a ×2 improvement in z-resolution. We demonstrate the technique by sub-slice imaging of hepatocyte membranes in liver tissue.

Electron beams have made possible the development of the versatile, high performance electron microscopes described in the earlier chapters of this book. Techniques for the generation and application of electron beams are now well documented and understood, and a wide variety of images and data can be produced using readily available instruments. While the scanning electron microscope (SEM) is the most widely used tool for high performance imaging and microanalysis, it is not the only option and may not even always be the best instrument to choose to solve a particular problem. In this chapter we will discuss how, by replacing the beam of electrons with a beam of ions, it is possible to produce a high performance microscope which resembles an SEM in many respects and shares some of its capabilities but which also offers additional and important modes of operation.

Software is an essential tool for the scanning electron microscopist and X-ray microanalyst (SEMXM). In the past, software was an important optional means of augmenting the electron microscope and X-ray spectrometer, permitting powerful additional analysis and enabling new characterization methods that were not possible with bare instrumentation. Today, however, it is simply not possible to function as an SEMXM practitioner without using at least a minimal amount of software. A graphical user interface (GUI) is an integral part of how the operator controls the hardware on most modern microscopes, and in some cases it is the only interface. Even many seemingly analog controls such as focus knobs, magnification knobs, or stigmators are actually digital interfaces mounted on hand-panel controllers that connect to the microscope control computer via a USB interface.

Summary Electron microscopy is an essential tool for the evaluation of microstructure and properties of the catalyst layer (CL) of proton exchange membrane fuel cells (PEMFCs). However, electron microscopy has one unavoidable drawback, which is radiation damage. Samples suffer temporary or permanent change of the surface or bulk structure under radiation damage, which can cause ambiguity in the characterization of the sample. To better understand the mechanism of radiation damage of CL samples and to be able to separate the morphological features intrinsic to the material from the consequences of electron radiation damage, a series of experiments based on high-angle annular dark-field–scanning transmission scanning microscope (HAADF-STEM), energy filtering transmission scanning microscope (EFTEM), and electron energy loss spectrum (EELS) are conducted. It is observed that for thin samples (0.3–1 times λ), increasing the incident beam energy can mitigate the radiation damage. Platinum nanoparticles in the CL sample facilitate the radiation damage. The radiation damage of the catalyst sample starts from the interface of Pt/C or defective thin edge and primarily occurs in the form of mass loss accompanied by atomic displacement and edge curl. These results provide important insights on the mechanism of CL radiation damage. Possible strategies of mitigating the radiation damage are provided. SCANNING 36:338–346, 2014. © 2013 Wiley Periodicals, Inc.

Summary Generally, in scanning electron microscopy (SEM) imaging, it is desirable that a high-resolution image be composed mainly of those secondary electrons (SEs) generated by the primary electron beam, denoted SEI. However, in conventional SEM imaging, other, often unwanted, signal components consisting of backscattered electrons (BSEs), and their associated SEs, denoted SEII, are present; these signal components contribute a random background signal that degrades contrast, and therefore signal-to-noise ratio and resolution. Ideally, the highest resolution SEM image would consist only of the SEI component. In SEMs that use conventional pinhole lenses and their associated Everhart–Thornley detectors, the image is composed of several components, including SEI, SEII, and some BSE, depending on the geometry of the detector. Modern snorkel lens systems eliminate the BSEs, but not the SEIIs. We present a microfabricated diaphragm for minimizing the unwanted SEII signal components. We present evidence of improved imaging using a microlithographically generated pattern of Au, about 500 nm thick, that blocks most of the undesired signal components, leaving an image composed mostly of SEIs. We refer to this structure as a “spatial backscatter diaphragm.” SCANNING 35:1-6, 2013. © 2012 Wiley Periodicals, Inc.

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.

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.

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.

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 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.

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.

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]

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]

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.

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.

As noted in the previous section, the present ALIS helium ion source is a descendant of the original work based on FIM technology (for a historical overview see Muller and Tsong 1993) although important research in this area has also been carried out by several other prominent groups (e.g. Orloff and Swanson 1977). In order to be suitable for application, in a high-performance particle beam microscope, the source should ideally not only be bright, but also be as compact as possible to ensure mechanical stability, provide highly stable emission over time periods of several hours, be capable of operating at energies at least in the 10–50 keV range, and be capable of being re-formed and then reused multiple times without a significant change in performance. An overview of history of the helium ion microscope can be found in the literature (Economou 2011), while other technical details can be found in the published patents listed at the end of the bibliography.

The scanning electron microscope (SEM) has become the most widely used high-performance microscope. However because of the fundamental limitations of electron beams the new technology of ion beam microscopy is being developed

Every microscope requires a high brightness, reliable, stable source of illumination in order to function, and both the quality and the quantity of the illumination provided will determine, and ultimately limit, the performance of the instrument. Each type of microscope will have its own type of illuminating source. For a high-performance scanning electron or ion microscope, the most desirable property of the beam source is that the source must have a high brightness.

It has to be expected that both ions and electrons will damage specimens under examination to a greater or lesser degree. Electrons are low in mass but can travel at velocities which are a significant fraction of the speed of light. In general, electrons do not significantly damage metallic or inorganic specimens, but even relatively low doses of electrons can be expected to chemically alter or destroy organic materials such as polymers and biological samples.

Achieving the ultimate limits of lithographic resolution and material performance necessitates engineering of matter with atomic, molecular, and mesoscale fidelity. With the advent of scanning helium ion microscopy, maskless He(+) and Ne(+) beam lithography of 2D materials, such as graphene-based nanoelectronics, is coming to the forefront as a tool for fabrication and surface manipulation. However, the effects of using a Ne focused-ion-beam on the fidelity of structures created out of 2D materials have yet to be explored. Here, we will discuss the use of energetic Ne ions in engineering graphene nanostructures and explore their mechanical, electromechanical and chemical properties using scanning probe microscopy (SPM). By using SPM-based techniques such as band excitation (BE) force modulation microscopy, Kelvin probe force microscopy (KPFM) and Raman spectroscopy, we are able to ascertain changes in the mechanical, electrical and optical properties of Ne(+) beam milled graphene nanostructures and surrounding regions. Additionally, we are able to link localized defects around the milled graphene to ion milling parameters such as dwell time and number of beam passes in order to characterize the induced changes in mechanical and electromechanical properties of the graphene surface.

In this paper we will discuss our recent experimental results, using electron holography and electron interferometry, of studies of ferroelectric domain walls in BaTiO3 and PLZT thin specimens.

The CD-SEM has been the tool of choice for the imaging and metrology of semiconductor devices for the past three decades but now, with critical dimensions at the nanometer scale, electron beam instruments can no longer deliver adequate performance. A scanning microscope using a He+ ion beam offers superior resolution and depth of field, and provides enhanced imaging contrast. Device metrology performed using ion beam imaging produces data which is comparable to or better than that from a conventional CD-SEM although there are significant differences in the experimental conditions required and in the details of image formation. The charging generated by a He+ beam, and the sample damage that it can cause, require care in operation but are not major problems.

An electron holographic method is introduced for the study of ferroelectric domain walls. The method allows not only direct imaging of the domain wall but also the measurement of local spontaneous polarization. Preliminary results of first high-resolution imaging of ferroelectric domain walls by using this technique in BaTiO3 and quantitative measurements of electrostatic field distribution across domain walls are presented.

The electron-optical parameters required to generate an electron hologram are discussed. It is shown that the new generation of commercial field emission transmission electron microscopes (FEG TEM) meet the conditions required. Practical details of the procedures to set up and record a hologram are described. The steps necessary to reconstruct the hologram are also discussed and an outline is provided of a program for the Apple Macintosh™ personal computer which implements these operations. The integrity and accuracy of the reconstruction program has been tested by means of a detailed simulation of high-resolution holograms starting from dynamical multi-slice calculations of the exit wavefront.

Single-wall carbon nanotubes (SWNT) were grown to micron lengths by laser-annealing nanoparticulate soot containing short (∼50 nm long) nanotube “seeds.” The “seeded” nanoparticulate soot was produced by restricting the time spent by an ablation plume inside an 800 °C oven following laser vaporization of a C–Ni–Co target. The soot collected from the laser vaporization apparatus was placed inside graphite crucibles under argon, and heated by a CO2 laser. In situ pyrometry was used to estimate the sample temperature. Length distributions of SWNT bundles in the unannealed and annealed samples were measured by transmission electron microscopy and field emission scanning electron microscopy. Annealing treatments exceeding 1600 °C produced no increase in nanotube length, while lower temperatures in the 1000–1300 °C range were optimal for growth. These experiments indicate that SWNT grow by the conversion of condensed phase nanomaterial during annealing, a similar mechanism to that proposed for growth during normal laser–vaporization production.

Although Scanning Electron Microscopes (SEM) have improved greatly over the last decade the techniques usually employed to measure their performance have not changed significantly in half a century. In particular, describing the imaging performance of an SEM by a single number - its 'resolution' - provides no useful information about its real world imaging capabilities nor about any of the factors that might limit that usefulness of the SEM for tasks such as metrology. The Contrast Transfer Function (CTF) discussed here analyses the way in which the SEM processes signal components of different spatial frequencies. The resultant plot provides information on the noise limited spatial resolution limit, predicts how this will vary with noise level, and provides a powerful general diagnostic capability. This type of measurement, which has become standard practice for transmission electron microscopes, can be performed using the public domain software package IMAGE-J, is rapid, and requires only a specimen offering a broad and flat Fourier spectrum. The capabilities of this approach are demonstrated by a number of examples.

Recent advances in instrumentation have produced the first commercial examples of what can justifiably be called high-resolution scanning electron microscopes. The key components of such instruments are a cold field emission gun, a small-gap immersion probe-forming lens, and a clean dry-pumped vacuum. The performance of these microscopes is characterized by several major features including a spatial resolution, in secondary electron mode on solid specimens, which can exceed 1 nm on a routine basis; an incident probe current density of the order of 10 6 A/cm 2 ; and the ability to maintain these levels of performance over an accelerating voltage range of from 1 to 30 keV. This combination of high resolution, high probe current, low contamination and flexible electron-optical conditions provides many new opportunities for the application of the SEM to materials science, physics, and the life sciences.

The physical dimensions of nanoscale objects are an important indicator of their functionality. However, measuring feature size from a SEM image is difficult not only because of fundamental considerations, such as the nature of beam interactions and the information transfer properties of the microscope, but because the magnification of the SEM image from which a measurement will be made is completely uncalibrated and additionally is subject to local distortions and variations. Nano-gauges fabricated by electron beam lithography - one or two dimensional structures on the size scale of the objects of interest - provide a local length standards within the image field from which the relative size of features can be accurately determined. In order to provide an absolute measurement of size the dimensions of the nano-gauge structure must themselves be calibrated against some primary standard. Because there are no convenient standards of appropriate scale available we propose that this can be done using a moire fringe technique to bridge the gap between the nanoscale and common length standards such as ruled diffraction gratings.

With the semiconductor industry moving into the 65nm technology node, the metrology of the critical dimension (CD) becomes an important part for the industry. Metrology relies not only on the precision, but also on the accuracy of the tools like the high performance CD-SEMs. A major area of concern affecting the accuracy of the high performance CD-SEMs is the magnification calibration. The purpose of the research is to address this area of concern by fabrication of magnification calibration artifact by using direct write electron beam lithography. A calibration artifact has been fabricated in negative resist Hydrogen Silsesquioxane (HSQ) onto a silicon substrate, thereby decreasing the contamination on the substrate. The design of the artifact has been corrected for the proximity effects, giving a 2-D dense grid structure with 100nm pitch. Pitch determination using optical metrology tools and the inbuilt laser interferometer in the electron beam lithography tool is being evaluated for making the artifact traceable to some national standards. Once the traceability is achieved, mass production at low cost using Nanoimprint technology is feasible.

A scanning ion microscope (SIM) is analogous to a scanning electron microscope (SEM) but utilizes a beam of helium ions, with energy of 10 to 25 keV , instead of electrons. The SIM potentially offers several advantages for device critical dimension metrology as compared to the more familiar CD-SEM. These include a high brightness source which is sub-nanometer in size, an enhanced secondary electron yield, restricted beam penetration, and superior image contrast and information content. Possible problems include pervasive positive charging, ion implantation, and a lack of detailed experimental and theoretical knowledge about low energy ion interactions with solids. Comparison of line profiles across structures made by electron induced and ion induced secondary electrons show that there are some significant differences between them which arise from the different modes of interaction in the two cases. As a result the algorithms employed for line width determination will require revision in order to produce data which is consistent with CD-SEM data.

It is important to be able to quantify the imaging performance of CD-SEMs for such purposes as verifying the specification, rechecking after a routine maintenance, or for tool matching. To perform tests such as these it is necessary to have both appropriate software for image analysis and suitable test samples. A package of 2-D Fourier transform and analysis software, designed as a plug-in for the shareware IMAGE-Java program, has been developed and is freely available on line. The requirement for a reproducible and well characterized sample has been met by using direct-write electron beam lithography to fabricate suitable Fresnel zone plate structures.

The performance of the conventional low‐energy CD‐SEM is limited by the aberrations inherent in the probe forming lens. Multi‐pole correctors are now available which can reduce or eliminate these aberrations. An SEM equipped with such a corrector offers higher spatial resolution and more probe current from a given electron source, and other aspects of the optical performance are also improved, but the much higher numerical aperture associated with an aberration corrected lens results in a reduction in imaging depth of field.

Because a photomask is typically a block of quartz partially covered a thin metal coating it charges significantly under an electron beam making CD metrology difficult and often imprecise. A solution to this problem can be found by performing the measurement in the presence of a low pressure of gas in a variable pressure scanning electron microscope (VPSEM). The gas is ionized by the emitted secondary electrons so producing both positive and negative ions which drift to the charged surface and neutralize it. This process is self controlling and requires no critical adjustments by the operator. With charging removed metrology can then be performed over a wide range of beam energies using either secondary or backscattered electron signals with excellent precision and accuracy. The presence of the gas atmosphere also eliminates beam induced contamination effects. If a chemically active precursor gas is injected into the system then the electron beam can also be used to edit and repair damaged masks.

Lithographic processes for printing device structures on integrated circuits (ICs) are the fundamental technology behind Moore's law. Next-generation techniques like maskless lithography or ML2 have the advantage that the long, tedious and expensive process of fabricating a unique mask for the manufactured chip is not necessary. However, there are some rather daunting prblems with establishing ML2 as a viable commercial technology. The data rate necessary for ML2 to be competitive in manufacturing is not feasible with technology in the near future. There is also doubt that the competing technologies for the writing mechanisms and corresponding photoresist (or analogous medium) will be able to accurately produce the desired patterns necessary to produce multi-layer semiconductor devices. In this work, we model the maskless printing system from a signal processing point of view, utilizing image processing algorithms and concepts to study the effects of various real-world constraints and their implications for a ML2 system. The ML2 elements are discrete devices, and it is doubtful that their motion can be controlled to the level where a one-for-one element to exposed pixel relationship is allowable. Some level of sub-element resolution can be achieved with gray scale levels, but with the highly integrated manufacturing practices required to achieve massive parallelism, the most effective elements will be simple on-ofrf switches that fire a fixed level of energy at the target medium. Consequently gray-scale level devidces are likely not an option. Another problem with highly integrated manufacturing methods is device uniformity. Consequently, we analyze the redundant scanning array concept (RSA) conceived by Berglund et al. which can defeat many of these problems. We determine some basic equations governing its application and we focus on applying the technique to an array of low-energy electron emitters. Using the results of Monte Carlo simulations on electron beam profiles, we determine an empirical "impulse response" for each emitter and thus determine how each emission manifests itself in the final printed lithographic pattern. We apply methods to determine the best printable image for a variety of RSA geometries, including different levels of redundancy and achieved printer element spacing. We use concepts of total printing error to help quantify the printing quality. Through simulation, we report the effects of dead or missing elements. We also present some error analysis to account for non-ideal array positioning. Ultimately, we believe that printing quality should be the grounds for determining the necessary data rates to support competitive manufacturing with ML2 devices.

Voltage profiles of the source-drain region of a CMOS transistor with 75nm gate architecture taken from an off-the-shelf Intel PIII processor are presented. The sample preparation using a dual beam system is discussed as well as details of the electron optical setup of the microscope. Special attention is given to the analysis of the reconstructed holograms.

Laser vaporization (LV) is a remarkably versatile technique for the catalytically-aided synthesis of nanomaterials, such as single-wall carbon nanotubes (SWNT). SWNT show remarkable promise for future generations of electronics and structural materials, however their application and commercialization has been hampered by a lack of control over the synthesis process, and low production quantities. Time-resolved in situ spectroscopic investigations of the laser-vaporization SWNT-synthesis process are described which are yielding some of the first direction determinations of carbon nanotube growth mechanisms and rates necessary to evaluate strategies for controllable synthesis and large-scale production. Our measurements indicate that SWNT grow over extended annealing times during the LV process by the conversion of condensed phase nanoparticle feedstock. These measurements were extended to grow carbon nanotubes by CO2- laser-annealing heat treatments of carbon and metal nanoparticle mixtures, offering an alternative synthesis approach to vapor- phase methods. These results present opportunities for scaled-up production of nanomaterials compatible with commercial high- power-laser technology.© (2002) COPYRIGHT SPIE--The International Society for Optical Engineering. Downloading of the abstract is permitted for personal use only.

Conventional scanning electron microscopes are now close to the limit of their performance for tasks such as the metrology of sub-micron design rule devices. In order to overcome these limits we have designed, and are presently testing, a low voltage point source microscope operated with a nanotip field emitter and without any electron optical lenses. The microscope is designed such that can be operated in the transmission mode as well as in a reflection mode. The ultra-sharp field emitter delivers emission currents of several nanoamps at energies less than 100 eV. The magnification of the object wave is achieved by placing the specimen in the divergent electron beam from the nanotip and observing the object wave using a microchannel plate (MCP) at a great distance from the sample. Images obtained that way are out of focus images. As no lenses are present a special 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. Electrons diffracted at an edge of the specimen cause Fresnel fringes in the image plane. An electrically charged holey carbon foil acts in the same way on the electrons as the Youngs double slit experiment and results in an interference pattern consisting of parallel fringes. A comparison between the transmission mode and the perfection mode shows great similarities with respect to the magnification and the interference pattern. An electron gun needed in the transmission mode is the most important difference between the two modes of operation. The experimental results at a reflection of 45 degrees are in good agreement with our simulation. Following our simulations a reflection angle of 90 degrees is most promising for easiest image interpretation.

We show simulation images of projection microscope, which uses parallel beam to the sample, detecting secondary electrons, photoelectrons and mirror electrons using electrons and UV/X-ray sources as probe beam. The results show we can see image for square and dense line patterns without charging and damage in the objects. This research can be used for quantitative analysis for projection microscope using multi beam source to get comprehensive information of many characteristics of objects as well as topographic information.

Conventional scanning electron microscopes are now close to the limit of their performance for tasks such as the metrology of sub-micron design rule devices. In order to overcome these limits we are investigating the use of in-line electron holography for device metrology. The in-line holograms are formed in a point projection microscope using ultra-low energy electrons (50-250eV) emitted from a nano-tip electron source. Holograms in the transmission mode and in the reflection mode of the microscope as well are possible. Since these in-line holograms are equivalent to out of focus micrographs acquired in a transmission electron microscope with a field emission gun we can reconstruct the original wave front by means of Fourier optics. The resolution of the point projection microscope is given by the sharpness of the emitter. We investigate the electric potential of the emitter using off-axis electron holography in a transmission electron microscope and compare the results to simulations obtained by solving the appropriate Laplace equation.

Single-wall carbon nanotubes are formed by Nd:YAG laser vaporization of a graphite/(1 at. % Ni, 1 at. % Co) target into flowing argon (500 Torr) within a quartz tube furnace (1000 degree(s)C). Here, this process is investigated for the first time with time-resolved laser-induced luminescence imaging and spectroscopy of Co atoms, C 2 and C 3 molecules, and clusters. These measurements under actual synthesis conditions show that the plume of vaporized material is segregated and confined within a vortex ring which maintains an approximate 1 cm 3 volume for several seconds. Using time-resolved spectroscopy and spectroscopic imaging, the time for conversion of atomic and molecular species to clusters was measured for both carbon (200 microsecond(s) ) and cobalt (2 ms). This rapid conversion of carbon to nanoparticles, combined with transmission electron microscopy analysis of the collected deposits, indicate that nanotube growth occurs during several seconds of time from a feedstock of mixed nanoparticles in the gas-suspended plume. By adjusting the time spent by the plume within the high- temperature zone using these in situ diagnostics, single- walled nanotubes of controlled length were grown at an estimated rate of 0.2 micrometers /s. Ex situ annealing of short, 100-200 nm-long SWNT seeds collected after limited growth inside the hot oven resulted in continued growth of longer SWNT bundles, supporting the condensed phase conversion mechanism for SWNT growth.

The continued dominance of electron-beam instruments as the tool of choice for metrology is threatened by the requirements demanded for sub-100nm device structures. The key factors required for effective metrology are identified, the limitations of existing instruments are considered, and a new type of microscope tool for metrology which avoids this limitation is proposed.

Laser vaporization (LV) is a remarkably versatile technique for the catalytically-aided synthesis of nanomaterials, such as single-wall carbon nanotubes (SWNT). SWNT show remarkable promise for future generations of electronics and structural materials, however their application and commercialization has been hampered by a lack of control over the synthesis process, and low production quantities. Time-resolved in situ spectroscopic investigations of the laser-vaporization SWNT-synthesis process are described which are yielding some of the first direct determinations of carbon nanotube growth mechanisms and rates necessary to evaluate strategies for controllable synthesis and large-scale production. Our measurements indicate that SWNT grow over extended annealing times during the LV process by the conversion of condensed phase nanoparticulate feedstock. These measurements were extended to grow carbon nanotubes by CO2-laser-annealing heat treatments of carbon and metal nanoparticle mixtures, offering an alternative synthesis approach to vapor-phase methods. These results present opportunities for scaled-up production of nanomaterials compatible with commercial high-power laser technology.Laser vaporization (LV) is a remarkably versatile technique for the catalytically-aided synthesis of nanomaterials, such as single-wall carbon nanotubes (SWNT). SWNT show remarkable promise for future generations of electronics and structural materials, however their application and commercialization has been hampered by a lack of control over the synthesis process, and low production quantities. Time-resolved in situ spectroscopic investigations of the laser-vaporization SWNT-synthesis process are described which are yielding some of the first direct determinations of carbon nanotube growth mechanisms and rates necessary to evaluate strategies for controllable synthesis and large-scale production. Our measurements indicate that SWNT grow over extended annealing times during the LV process by the conversion of condensed phase nanoparticulate feedstock. These measurements were extended to grow carbon nanotubes by CO2-laser-annealing heat treatments of carbon and metal nanoparticle mixtures, offering an alt...

Extended abstract of a paper presented at Microscopy and Microanalysis 2010 in Portland, Oregon, USA, August 1 – August 5, 2010.

Electron holography performed in a transmission electron microscope, has been used to measure the width of 90° domain walls in tetragonal BaTiO3, and to determine the magnitude and distribution of the polarization across these walls. The walls are found to be between 15 and 25 A in width. The polarization and its measured variation are in good agreement with other estimates. Fringe splitting has been observed in some holograms and it is suggested that this is due to the presence of charged oxygen vacancies on the walls.