bluuebunny/crossref_metadata_2025 huggingface dataset:
Characterization of metamict and glassy phosphates using energy-filtered electron diffraction
Authors: Sreeram A. N. , Qin L. C. , Garratt-Reed A. J. , Hobbs L. W.
Published: June 2020

Lead phosphate glasses have been investigated for decades with respect to fundamental glass properties such as glass transition, devitrification, electrical and optical properties. In these glasses, [PO4] tetrahedra, (like [SiO4] tetrahedra in silicates) can link up together by corner sharing oxygen atoms to form polymerized structures upto and including three dimensional glassy networks. Although, little electron diffraction data on amorphous phosphates is available, radial distribution functions have been generated for lime phosphate glasses and amorphous aluminum phosphates using x-ray diffraction techniques. More recently, Sales et al. have examined near surfaces of single crystals of lead pyrophosphate (Pb2P2O7), rendered aperiodic (metamict) by ion implantation, and lead pyrophosphate glass using high-performance liquid chromatography (HPLC), making use of the fact that condensed phosphates do not alter their state of polymerization when dissolved in aqueous solutions.

In our studies, single crystals of Pb2P2O7 were found to be beam stable under 200 keV TEM electrons to an electron fluence > 1027 e/m2 and an ionizing dose > 1014 Gy. This negative radiolytic result leaves ballistic displacement by ions or neutrons as the only route to render the samples metamict.
Digital imaging with field emission scanning electron microscopes (FSEM)
Authors: Peters Klaus-Ruediger , Martin William H. , Oho Eisaku
Published: June 2020

Digital image acquisition and display of field emission scanning electron micrographs face limitations in terms of detail recognition, sampling of high resolution information, image output and storage space for high pixel density images. The image acquisition and image output of a JEOL JSEM-890 “in lens” field emission SEM were digitized and several approaches for adequate access to the scanned electron probe data have been developed. Images are acquired digitally in 3×4 VGA format (in multiples of 640×490 pixels) and stored in a RECOGNITION CONCEPTS INC. image processor (Trapix Plus). The images are displayed on workstation monitors with 1280×1024 format (HITACHI CM2085MU), and image documentation is done by several techniques of varying output quality. Low quality image documentation on plain paper can be obtained using a laser jet printer (HEWLETT PACKARD: Laser Jet III). High quality output is provided by a video printer utilizing special but inexpensive paper (SEIKOSHA VP350H). In addition, conventional analog CRT output and CRT photography on 4×5 inch POLAROID (Type 55 Positive/Negative) film is used.
High-Magnification in-lens field-emission SEM of sectioned biological material
Authors: Apkarian R.P. , Scala C. , Pasquinelli G.
Published: June 2020

Osmium macerated renal specimens are rich in SE-I contrasts at very high magnifications when the ultrathin Chromium (Cr) film/intermediate voltage (15-30 kV) imaging strategy is employed. This technique enables imaging of minute particle domains which contain SE-I edge brightness contrast when staged in an in-lens field emission scanning electron microscope (SEM). The utility of employing methylmethacrylate embedded and sectioned specimens, that were subsequently acetone deembedded and critical point dried on silicon chips, was that they were rendered ideal for ultrahigh resolution SEM studies. The section/SEM method provided an exellent correlate to light microscopy (LM) and transmission electron microscopy (TEM) and may extend topographic image resolution within tissues to the molecular level.

Rat kidney was briefly fixed in 0.5% glutaraldehyde/ 0.5% formaldehyde, postfixed in 1.0% OsO4 and osmium macerated (0.1%) prior to the embedding/sectioning/deembedding/drying procedures. Kidney sections ranging from 80 nm to 1.5 μm on silicon chips were thoroughly degassed and coated with a 1 nm fine grain Cr film in a Denton DV-602 sputter system.
Secondary-Electron imaging by Scintillating Gaseous Detection Device
Authors: Danilatos G. D.
Published: June 2020

The environmental scanning electron microscope (ESEM) incorporates the functions of the conventional SEM while it has the added capability of allowing the examination of virtually any specimen in a gaseous environment. The main modes of imaging are all represented in the ESEM, and some developments with regard to the secondary electron (SE) mode are reported herewith.

The conventional E-T detector fails to operate in the gaseous conditions of ESEM, but this obstacle has been overcome with the advent of a gaseous detection device (GDD). The principle of operation of this device is based on the monitoring of the products of interaction between signals and gas. Initially, the ionization from the signal/gas interaction was used to produce images of varying contrast and, later, the gaseous scintillation, from the same interaction, was also used to produce images. First, a low bias was applied to various electrodes but later a much higher bias was used for the purpose of achieving additional signal gain. By careful shaping and positioning the respective electrode, it was shown that SE imaging is possible in the ESEM. This has been also independently demonstrated by use of a special specimen preparation.
Advantages of Complementary Stereo Images as Viewed with the Low-Temperature Field-Emission SEM
Authors: Wergin William P. , Erbe Eric F.
Published: June 2020

The eye-brain complex allows those of us with normal vision to perceive and evaluate our surroundings in three-dimensions (3-D). The principle factor that makes this possible is parallax - the horizontal displacement of objects that results from the independent views that the left and right eyes detect and simultaneously transmit to the brain for superimposition. The common SEM micrograph is a 2-D representation of a 3-D specimen. Depriving the brain of the 3-D view can lead to erroneous conclusions about the relative sizes, positions and convergence of structures within a specimen. In addition, Walter has suggested that the stereo image contains information equivalent to a two-fold increase in magnification over that found in a 2-D image. Because of these factors, stereo pair analysis should be routinely employed when studying specimens.

Imaging complementary faces of a fractured specimen is a second method by which the topography of a specimen can be more accurately evaluated.
Environmental scanning electron microscopy of fresh human gallstones reveals new morphologies of precipitated calcium salts
Authors: Kaufman Howard S. , Lillemoe Keith D. , Mastovich John T. , Pitt Henry A.
Published: June 2020

Gallstones contain precipitated cholesterol, calcium salts, and proteins. Calcium (Ca) bilirubinate, palmitate, phosphate, and carbonate occurring in gallstones have variable morphologies but characteristic windowless energy dispersive x-ray (EDX) spectra. Previous studies of gallstone microstructure and composition using scanning electron microscopy (SEM) with EDX have been limited to dehydrated samples. In this state, Ca bilirubinates appear as either glassy masses, which predominate in black pigment stones, or as clusters, which are found mostly in cholesterol gallstones. The three polymorphs of Ca carbonate, calcite, vaterite, and aragonite, have been identified in gallstones by x-ray diffraction, however; the morphologies of these crystals vary in the literature. The purpose of this experiment was to study fresh gallstones by environmental SEM (ESEM) to determine if dehydration affects gallstone Ca salt morphology.

Gallstones and bile were obtained fresh at cholecystectomy from 6 patients. To prevent dehydration, stones were stored in bile at 37°C. All samples were studied within 4 days of procurement.
The titanic 80 years later: initial observations on the microstructure and biogeochemistry of corrosion products
Authors: Stoffyn Patricia , Buckley Dale E.
Published: June 2020

The “Titanic 91” Expedition, carried out from the Russian Academy of Science vessel “Akademik Keldysh”, recovered artifacts from the wreck of the Titanic using the manned submersible “MIR-2”. Conspicuous corrosion products are iron rusticles resembling stalactites. These rusticles can reach lengths of several tens of cm and grow from various parts of the ship (Fig. 1). The origin of the rusticles and their relation to other corrosion products was investigated using a scanning electron microscope equipped with an x-ray energy dispersive spectrometer and a separate x-ray diffraction system.

Rusticles are formed of a brittle iron oxy-hydroxide shell approximately 100 to 200 μm thick, with a smooth dark red outer surface (toward seawater) and an orange rough inner surface (toward the centre of the rusticle). The core of the rusticle and the inner surface of the shell is made of a reticular framework of spherical aggregates. The small needle-like crystals forming these aggregates (Fig. 2) are goethite (α- FeO(OH)).
Electron microscopy study of reactively sputter-deposited Ti/N films on silicon
Authors: Kannan V. C. , Singh A. K. , Irwin R. B. , Chittipeddi S. , Nkansah F. D. , Cochran W. T.
Published: June 2020

Titanium nitride (TiN) films have historically been used as diffusion barrier between silicon and aluminum, as an adhesion layer for tungsten deposition and as an interconnect material etc. Recently, the role of TiN films as contact barriers in very large scale silicon integrated circuits (VLSI) has been extensively studied. TiN films have resistivities on the order of 20μ Ω-cm which is much lower than that of titanium (nearly 66μ Ω-cm). Deposited TiN films show resistivities which vary from 20 to 100μ Ω-cm depending upon the type of deposition and process conditions. TiNx is known to have a NaCl type crystal structure for a wide range of compositions. Change in color from metallic luster to gold reflects the stabilization of the TiNx (FCC) phase over the close packed Ti(N) hexagonal phase. It was found that TiN (1:1) ideal composition with the FCC (NaCl-type) structure gives the best electrical property.
Influence of columnar and defect microstructures in chromium films on the kinetics of internal stress generation
Authors: Duan J.Z. , Fisher R.M.
Published: June 2020

Vapor-deposited Cr and other thin metal films are widely used in the micro-electronics industry as active circuit elements or intermediate layers to enhance the adhesion of other thin film materials to ceramic substrates or inhibit inter-diffusion. A key factor in the long term reliability of semiconductor devices is adequate adherence of films to various substrates to maintain the electrical integrity of the device. Internal stresses, that exceed the fracture strength of the interface, can cause interfacial fracture and film delamination so that the microstructures and internal stresses that are produced during film formation have been subjects of much research in this laboratory and elsewhere. Conventional and high resolution TEM and SEM studies of Cr films deposited on glass and Si substrates at room and elevated temperatures and at normal and oblique incident angles have shown that Cr forms as well defined columns surrounded by a highly disordered intergranular regions.
Porous silicon pore filling by metal electroplating
Authors: Chuang S.-F. , Kuan T. S. , Lin K.
Published: June 2020

Porous silicon can be used as an insulating material in Si devices and as a membrane for ion or molecule separation. Its recently demonstrated photo- and electro-luminescence properties may find novel applications in optoelectronics. Porous silicon has a large internal surface, and, with its pores filled with conducting materials, can form a capacitor with a high charge storage capacity. Recently, thin metal films have been electroplated on porous silicon substrates. These films were then detached and used as condenser microphone diaphragms. Electroplated metal films can also provide electrical contacts to an electro-luminescent porous silicon structure. In this paper, we report our TEM study of a copper electroplating process. We found that in such a process copper preferentially deposits from the bottom of the pore tips upward and fills the entire length of each pore as well as the horizontal side branches.

Anodization of silicon was performed in an aqueous HF solution to form a porous layer. Silicon substrates used in this experiment were n-type, (l00)-oriented wafers with a doping concentration of 1017 cm−3 and p-type, (l00)-oriented wafers with a doping concentration of 1019 cm-3.
Cathodoluminescence and TEM characterization of defects in III-V materials grown on Ge-terminated Si substrates
Authors: Malta D.P. , Posthill J.B. , Sharps P.R. , Colpitts T.S. , Timmons M.L. , Markunas R.J.
Published: June 2020

The growth of III-V materials on Si has been a major focus in electronic materials research for nearly a decade. The highly complementary properties of this heteroepitaxial system include high mobility and direct band gap in III-V materials and high crystalline quality, low cost and well-established technology of Si. However, the attainment of high crystalline quality III-V materials on Si suitable for minority carrier devices has been inhibited primarily due to the large lattice mismatch (˜4%) and thermal expansion mismatch (factor of ˜3) as well as the problematic nucleation of an ordered semiconductor on an elemental semiconductor. The epitaxial layer can contain threading dislocations, microtwins, stacking faults, antiphase domain boundaries (APBs) and/or have a poor surface morphology. A buffer layer can be added to improve the III-V material quality by accommodating the lattice mismatch at one or more interfaces and/or to provide a more suitable surface for nucleation. We have used TEM in conjunction with scanning cathodoluminescence (CL) intensity mapping for complete and accurate assessment of crystalline quality and defect densities within a range of ˜ 5×102 cm-2 to > 108 cm-2.
Specific site device failure analysis: A case history
Authors: Anderson Ron , Wall Joseph , Klepeis Stanley
Published: June 2020

Failure analysis application of analytical TEM analysis was handicapped in the past by the difficulty associated with specimen preparation of specific devices in complicated integrated circuit arrays. We have published several papers detailing methods for preparing TEM specimens with high specimen preparation spatial resolution in periods of about two to four hours. This paper offers a case history of a TEM failure analysis that combines high spatial resolution specimen preparation and the utilization of chemical junction delineation techniques.

The device failure came to light in a chip tester prior to shipment. Tester electrical diagnostics identified a particular cell within a large array as defective. The fail's electrical signature further narrowed-down the potential candidates to a small number of devices within the cell. The chip was examined in transmission in an IR microscope. Anomalous IR contrast was observed in the emitter of one bipolar device in the suspect region (Fig. 1). A series of conventional light-optical photographs, with increasing magnification, were taken to define the failure location. Using the light-optical photos as a guide, the failed emitter was bracketed with laser craters. The specimen preparation polishing operation used the laser craters to achieve a plane-of-polish through the suspect emitter.
Defect distribution of through-Oxide boron-Implanted silicon with and without fluorine incorporation
Authors: Lam Amy C.
Published: June 2020

Material defects generated during device processing can affect the performance of VLSI/ULSI devices. Ion implantation is the most common method of doping in the semiconductor industry. Implantation is usually performed with the wafers oriented 7° off the incident beam direction and through oxide to minimize the channeling effect. In order to obtain shallow p/n junctions for metal-oxide-semiconductor (MOS) devices, implantation of BF2+ molecular ions into silicon has been reported to have advantages over only B+ implantation. With the incorporation of fluorine, suppression of boron diffusion will be achieved by the emission of vacancies. However, BF2+ are heavy ions and can create considerable residual damage. Instead of BF2+ implantation, boron and fluorine implantations are done separately in our studies. As an alternative to fluorine implantation through oxide, fluorine could be introduced during thermal oxidation of silicon. Boron implantation of 3×l015/cm2 dose follows oxidation. The dosages for separate boron and fluorine implants are l×l015/cm2 and 2×l015/cm2 respectively, to attain the same elemental ratio as for BF2+ implantation.
Effects of elastic anisotropy on CTEM dislocation images in L10 alloys: An assessment of the sensitivity computed images to input parameters
Authors: Singh Abha , King A.H.
Published: June 2020

Ordered alloys have important applications as high temperature structural materials. Grain boundary embrittlement, however, is a major obstacle in their practical applications. The details of grain boundary structure have been suggested to be important in determining the mechanical properties, and it is therefore important to have a better understanding of grain boundary structure in these alloys.

Conventional g.b and g.b×U techniques for the determination of Burgers vectors of lattice and grain boundary dislocations are limited by the magnitude of the Burgers vectors and spacing of the dislocations. The dislocations may not be detected if the magnitude of the Burgers vectors is less than 0.05nm or the spacings less than one third of the extinction distance. The strengths of grain boundary dislocations are usually very small, therefore in determining the Burgers vectors of grain boundary dislocations, computer image matching techniques are generally used in conjunction with the usual g.b and g.b×U techniques.
Materials-science applications of novel methods for the analysis of electron-diffraction patterns
Authors: Carpenter G.J.C. , Le Page Y.
Published: June 2020

Electron diffraction provides a highly effective method for the identification of microscopic, crystalline phases in the solid state. The following examples are given to illustrate applications of three new analytical methods to typical problems in analytical microscopy of materials.

Phase identification using convergent beam electron diffraction (CBED) patterns can often be simplified when measurements from the zero and high order Laue zones (ZOLZ and HOLZ) are combined to calculate the primitive cell volume, Vc. Defining g1 and g2 as two primitive vectors in the ZOLZ (e.g. two non-collinear spots closest to the transmitted beam) the volume of the primitive reciprocal cell is;

Vc* = g1 × g2 . H,

where H is the reciprocal interplanar spacing calculated from the diameter(s) of the HOLZ ring(s). This calculation can be performed without indexing the pattern. The inverse of Vc* is the volume of the primitive cell, Vc, which is easily compared with literature data for possible phases.
Current performance limits for XEDS in the AEM
Authors: Zaluzec Nestor J.
Published: June 2020

For nearly the last decade, the microanalysis community has heard descriptions of the expected performance benefits of intermediate voltage analytical microscope operation. While it is true that these instruments have improved image resolution and probe forming capabilities, the majority generally perform worse in terms of XEDS analytical sensitivity than their 100 kV counterparts. Figure 1 compares the performance characteristics reported by Williams and Steel in 1987 for thirteen different AEM's, with recent measurements on the ANL AAEM (VG HB 603Z). Here the experimental Cr-K Peak to Background (P/B) ratio measured from the NIST (NBS) 100 nm thin-film standard is plotted as a function of accelerating voltage. From this figure, we see that a marked improvement in the performance of the newest generation of medium voltage AEM's has finally been commercially realized.

While there are several measurements of analytical sensitivity in XEDS, a convenient measure is the Minimum Mass Fraction (MMF).
Compositional imaging in biology: limits and potential
Authors: Somlyo Andrew P. , Shao Zhifeng , Somlyo Avril V.
Published: June 2020

Compositional imaging of cells and organelles in physiological and pathological states is a major challenge and opportunity for structural biology, but its potential for revealing new and significant biological information depends on the attainable sensitivity and spatial resolution. Since most biological materials consist of “trace concentrations” of elements embedded in an organic matrix composed of carbon, nitrogen, and oxygen, the minimal detectable concentration, rather than minimal detectable mass, is often the more important criterion of sensitivity. The past two decades have seen significant progress in the application of analytical electron microscopy [AEM] to biology and, after a brief standstill, the next decade offers further significant advances.

The preparatory method suitable for “high resolution” analysis of most biological materials is now well-established: rapid freezing, followed by cryoultramicrotomy and freeze drying to produce ultra thin specimens. Until recently, electron probe x-ray microanalysis and, related to it, x-ray mapping has been the most successful analytical method.
Micro-Raman spectroscopy applied to polymers
Authors: Meier Robert J.
Published: June 2020

Over the last years micro-Raman spectroscopy has developed to a mature subdiscipline within the field of Raman spectroscopy. Its potential power seems obvious: (a) fluorescence suppression, a major obstacle in many Raman spectra; (b) micro-analysis of samples down to 1 μm lateral resolution yielding molecular information; (c) when using a confocal arrangement with the microscope, in addition to lateral resolution the depth resolution can be enhanced up to the 1 μm level.

We applied micro-Raman spectroscopy over the last few years and recently developed a confocal Raman microscopic set-up. Our main application being in the field of polymers, the first thing to worry about is to what happens to the polymer sample when it is irradiated locally with a high laser power density. One should be warned even long before melting in order to avoid morphological changes because, after all, Raman spectroscopy is a powerful tool to study polymer morphology in detail. We use the Stokes/Anti-Stokes intensity ratio for determining the sample temperature.
Molecular imaging by Raman microscopy
Authors: Batchelder D.N. , Smith B.J.E. , Webster S. , Cheng C.
Published: June 2020

The optical microscope relies on spatial variations of refractive index, absorption and reflectivity in a specimen in order to produce the modulation in light intensity necessary to form the magnified image. The ability to identify the materials which comprise the specimen is very limited as these properties are generally not material specific. By contrast the Raman spectrum of a material is usually not only sufficient to give positive identification, but detail in the spectrum can often be used to assess the physical state of the material. Thus images recorded in light scattered in a particular Raman band should be very informative about the distribution of different molecular species.

We have developed a Raman microscope which uses multilayer dielectric filters to select the Raman band with which the image is formed. The optical quality of the filters is sufficiently high so as not to degrade the image forming capabilities of the microscope. The filters typically have a pass band of 20 cm-1 and are wavelength tuned by rotation.
Use of a Gram-Schmidt response function in infrared microspectroscopic imaging
Authors: Carl Richard T. , Weesner Forrest J.
Published: June 2020

The technique of infrared microspectroscopic imaging has found application in a variety of fields including coating technology, semiconductor manufacturing, and polymer science. The typical infrared microspectroscopic imaging experiment consists of collection of a four dimensional array of data (X, Y, frequency, intensity) followed by data reduction. In previous reports, this data reduction to three dimensions has been performed by monitoring the intensity or peak area of a specific frequency in the final transformed spectrum. This technique has been referred to as Functional Group Imaging (FGI).

This paper reports on the application of an interferograms based data reduction routine to infrared microspectroscopic imaging. The Gram-Schmidt (GS) orthogonalization procedure, popularized in application to GC-IR data, was used to measure the infrared response across the surface of the samples. The details of the vector algebra used in the GS calculations may be found elsewhere. Briefly, a set of interferogram segments is selected to form an orthonormalized basis set describing background conditions.
Rare-earth fluorescence in Raman microprobe spectra of glasses and ceramics
Authors: Etz Edgar S. , Blackburn Douglas H.
Published: June 2020

We are reporting on spectroscopic observations, made with the Raman microprobe, of fluorescence emissions by several rare earth, or lanthanide ions (Ln3+), in several types of ordered and disordered solids. These studies are an extension of earlier work on the luminescence properties of mainly two ions, Eu3+ and Er3+, as components of silicate glasses and of various ceramics related to high-temperature superconducting systems. Concerning the Y-Ba-Cu-O system, where yttrium has been replaced by one of the lanthanide elements (Ln = Nd, Sm, Eu, Dy, Ho, Er), our aim is to relate the observed optical spectra (Raman and fluorescence) to the composition and structure of the solids derived from the phase diagram. For this system, the Raman spectra of most of the compounds are well understood. Much less is known about the fluorescence spectra of the rare-earth substituted analogs and their relation to composition and structural order. The luminescence emissions of many of the Ln3+ ions can serve as useful spectroscopic probes of the structure of the host compound, of differences in bonding, and in the charge environment.
The examination of glass surfaces using time of flight mass spectrometries
Authors: Evans B. , Farnworth M. A. , Johnson A. E.
Published: June 2020

The surface composition of glass has a substantial impact on its end use, being a key factor in coating adherence, durability, and product life time. There is a continuing need to provide information on the precise composition of the exterior surface and to examine how this varies with time and exposure to weathering conditions.

The influence of water on the surface composition is of critical importance and of the techniques available to examine the surface, secondary ion mass spectroscopy has a range of advantages because of its high sensitivity and its ability to monitor Hydrogen in addition to all the other elements. It can also provide information on the presence of specific organic molecules on the surface.

Early work by Surman and Vickerman established that the preferred method of examining glasses in static SIMS was by means of a fast atom beam since this reduces the problems of charging associated with insulating surfaces and that reasonable quantification could be obtained if suitable standards were used.
X-ray microanalysis of frozen plant cells and tissues
Authors: Boekestein Abraham , Clerkx Anke C.M. , Verkerke Ruud , Ammann Norbert , Baayen Robert P.
Published: June 2020

The determination of concentrations of relatively freely diffusable ions in localized compartments of botanical tissues has become an essential technique in plant physiology . In order to analyze approximately the in vivo elemental concentrations, the scanning electron microscope has been adapted to facilitate the observation of frozen-fractured botanical cross-sections, thus enabling electronprobe X-ray microanalysis of the exposed surface. Although the analysis technique seems to have come in its productive years, it still has a number of unsolved problems, which are both related to the preparation of frozen-hydrated specimens and to the analysis method itself.

The most important problem in quantitative X-ray microanalysis of frozen-hydrated biological specimens, is the avoidance of ice crystallization artefacts. This phenomenon is rather critical in botanical tissue preparation because plant cells are relatively big and almost entirely occupied by a central vacuole. In this situation ice crystals can grow to large dimensions and disturb the originally homogeneous ion content.
Ion microprobe imaging of biological samples
Authors: Slodzian Georges
Published: June 2020

Microanalysis of biological samples by using secondary ion emission is a challenging problem because it requires high lateral resolving power, high sensitivity and high selectivity simultaneously. In this paper, the limits and the possibilities of the method will be examined regardless of the sample preparation conditions that is from a simple instrumentalist's point of view.

Any mass spectrometric method is destructive which means here that a given volume of the sample has to be sputtered to produce an adequate secondary ion signal. The size of this volume depends upon the atomic concentrations, the atomic density, the useful yield and the magnitude of the desired signal. To take an example, with an useful yield of 1% it would be necessary to sputter 300 atoms M to get an average signal of 3 ions (±) related to M. Such a signal would allow to detect the presence of element M with about 95% certainty (probability of getting one ion at least).
How SIMS microscopy can be used in medicine
Authors: Fragu Philippe
Published: June 2020

The identification, localization and quantification of intracellular chemical elements is an area of scientific endeavour which has not ceased to develop over the past 30 years. Secondary Ion Mass Spectrometry (SIMS) microscopy is widely used for elemental localization problems in geochemistry, metallurgy and electronics. Although the first commercial instruments were available in 1968, biological applications have been gradual as investigators have systematically examined the potential source of artefacts inherent in the method and sought to develop strategies for the analysis of soft biological material with a lateral resolution equivalent to that of the light microscope. In 1992, the prospects offered by this technique are even more encouraging as prototypes of new ion probes appear capable of achieving the ultimate goal, namely the quantitative analysis of micron and submicron regions. The purpose of this review is to underline the requirements for biomedical applications of SIMS microscopy.

Sample preparation methodology should preserve both the structural and the chemical integrity of the tissue.
Application of quantitative microscopy to specialty metals
Authors: Vander Voort George F.
Published: June 2020

Quantitative microscopy methods have been utilized for the characterization of specialty metal microstructures for many years. Initially, most work was more qualitative than quantitative because all methods were manual. However, since the introduction of more capable image analyzers in the 1980s, with vastly improved computer software and hardware, automated techniques have gained favor. With the implementation of automated image analysis equipment, users have quickly realized that specimen preparation techniques must be improved and also automated. The primary applications of quantitative microscopy methods in the specialty steel industry are: inclusion ratings, grain size measurement, volume fraction determination, and carbide distribution studies.

The American Society for Testing and Materials (ASTM) has been a leader in the development of microscopical test methods, chiefly through Committee E-4 on Metallography, which recently celebrated its 75th anniversary. Other technical societies, companies, organizations in other countries, and international organizations have also made notable contributions. ASTM standards are developed by volunteers from industry (both producers and purchasers), equipment manufacturers and academia using a consensus approach requiring voting at three levels.
Quantitative EPMA of nitrogen : A tricky element in the electron-probe microanalyzer
Authors: Bastin G.F. , Heijligers H.J.M.
Published: June 2020

Among the ultra-light elements B, C, N, and O nitrogen is the most difficult element to deal with in the electron probe microanalyzer. This is mainly caused by the severe absorption that N-Kα radiation suffers in carbon which is abundantly present in the detection system (lead-stearate crystal, carbonaceous counter window). As a result the peak-to-background ratios for N-Kα measured with a conventional lead-stearate crystal can attain values well below unity in many binary nitrides . An additional complication can be caused by the presence of interfering higher-order reflections from the metal partner in the nitride specimen; notorious examples are elements such as Zr and Nb. In nitrides containing these elements is is virtually impossible to carry out an accurate background subtraction which becomes increasingly important with lower and lower peak-to-background ratios. The use of a synthetic multilayer crystal such as W/Si (2d-spacing 59.8 Å) can bring significant improvements in terms of both higher peak count rates as well as a strong suppression of higher-order reflections.
Quantitative electron probe microanalysis of lithium-aluminum-borate glasses: a feasibility study
Authors: Marinenko Ryna B.
Published: June 2020

During the last few years both the instrumentation and data reduction procedures for analysis of low atomic number elements have substantially improved. For WDS analysis, synthetic multilayered crystals (LDE) designed specifically for the detection of low atomic number elements have surpassed the performance of the stearate and MYR crystals, showing much enhanced peak-tobackground ratios for boron, carbon, oxygen, and nitrogen. In addition, the cost of computers and computer memory has been reduced significantly, thus enabling scientists in our field to reevaluate conventional data reduction procedures for quantitative analysis. Assumptions and approximations can now be replaced in computer programs by the complete calculation and/or data base. A number of improved approaches to quantitation have resulted as well as a new interest in quantitating the low atomic number elements. Excellent results have been achieved by Bastin, Pouchou and Pichoir, Armstrong, and others.

In 1984 a group of Standard Reference Materials (SRM's) called Glasses for Microchemical Analysis were issued by the National Bureau of Standards, NBS(now the National Institute for Standards and Technology, NIST).
An improved interference correction for trace element analysis
Authors: Donovan John J. , Snyder Donald A. , Rivers Mark L.
Published: June 2020

We present a simple expression for the quantitative treatment of interference corrections in x-ray analysis. WDS electron probe analysis of standard reference materials illustrate the success of the technique.

For the analytical line of wavelength λ of any element A which lies near or on any characteristic line of another element B, the observed x-ray counts at We use to denote x-ray counts excited by element i in matrix j (u=unknown; s=analytical standard; ŝ=interference standard) at the wavelength of the analytical line of A, λA (Fig. 1). Quantitative analysis of A requires an accurate estimate of These counts can be estimated from the ZAF calculated concentration of B in the unknown C,Bu measured counts at λA in an interference standard of known concentration of B (and containing no A), and ZAF correction parameters for the matrices of both the unknown and the interference standard at It can be shown that:
Energy-Loss functions of Au derived by Monte Carlo analysis of angle-resolved Reels spectra
Authors: Yoshikawa Hideki , Shimizu Ryuichi
Published: June 2020

It is very well understood for free electron like metals that photoelectrons undergo not only bulk excitation but also surface excitation. For transition metals the contribution of surface excitation has not yet fully been discussed, and optical loss function has been widely used for background analysis of x-ray photoelectron spectroscopy (XPS).

In the previous work we proposed to derive the energy loss function which reproduced the XPS 4f spectrum very well by using the Monte Carlo simulation. This Monte Carlo simulation code describes elastic scattering process by Mott scattering cross-section and inelastic scattering process by differential inelastic mean free path (DIMFP) calculated from energy loss function. Optical loss function and this adjusted loss function obtained for Au are represented by dashed and solid lines in Fig.l, respectively. The intensity of the adjusted loss function is largely enhanced in the low-energy region comparing to the optical loss function. This sort of the enhancement in low energy region for noble metals have also been reported recently by Yubero et al.
Applications of SIMS to electronic materials and devices
Authors: Corcoran S.F.
Published: June 2020

Over the past decade secondary ion mass spectrometry (SIMS) has played an increasingly important role in the characterization of electronic materials and devices. The ability of SIMS to provide part per million detection sensitivity for most elements while maintaining excellent depth resolution has made this technique indispensable in the semiconductor industry. Today SIMS is used extensively in the characterization of dopant profiles, thin film analysis, and trace analysis in bulk materials. The SIMS technique also lends itself to 2-D and 3-D imaging via either the use of stigmatic ion optics or small diameter primary beams.

By far the most common application of SIMS is the determination of the depth distribution of dopants (B, As, P) intentionally introduced into semiconductor materials via ion implantation or epitaxial growth. Such measurements are critical since the dopant concentration and depth distribution can seriously affect the performance of a semiconductor device. In a typical depth profile analysis, keV ion sputtering is used to remove successive layers the sample.
Linewidth measurements of metallization coated with insulator on microelectronic circuits using Energy-Dispersive Xray Analysis (EDXA)
Authors: Sartore R.
Published: June 2020

Evaluation of quality and conformance to target production specifications for microelectronic devices frequently require measurements of the feature sizes of the critical conductive elements for the circuits. Further, failure analysis dictates critical dimension measurements to trace cause of failure for device. To date, the commercial critical dimension (CD) measurement systems are based on the secondary electron (SE) imaging techniques and analysis. In a failure analysis or quality evaluation laboaratory the microelectronic circuits received are mostly already fully fabricated, with passivation and insulator layers in place. The CD measuremment systems based on SE will not give accurate results unless the top insulating layer is removed. Layer removal is a destructive process and also difficult for devices that has several metallization levels. To address the destructive analysis and layer removal problems, a CD measurement technique has been developed that uses energy dispersive x ray analysis to measure critical feature sizes under a insulating layer.
Comparative mineral chemistry of IDPs, micrometeorites and meteorite matrices
Authors: Klöck Wolfgang
Published: June 2020

Chondritic porous aggregates are one subclass of Interplanetary Dust Particles (IDPs). The remaining classes presently identified are hydrated IDPs consisting mainly of serpentine or smectite. We have been investigating mineral compositions in these types of IDPs, in micrometeorites from Antarctica and compared them to mineral compositions in finegrained meteorite materials, like matrices and chondrule dust mantles from several meteorite classes. Based on our mineral analyses we subdivide anhydrous IDPs into three types. Type I contains olivines and/or pyroxenes having very variable iron contents from Fa 0 to Fa 35 and Fs 0 to Fs 30. Mineral phases in these particles are truly unequilibrated. Mineral grains in several particles of type I IDPs were found to contain solar flare tracks (pers. comm. John Bradley, McCrone Associates, Chicago). Almost all type I IDPs studied contain low-iron manganese enriched (LIME) olivines and/or pyroxenes.
Meteoroid residue in craters from earth orbiting spacecraft
Authors: Brownlee D.E. , Bradley J.
Published: June 2020

The extraterrestrial meteoroid residue found lining impact craters in metal targets recovered from space is highly variable in both quantity and type. In typical craters only a minor amount of reside is found and for these craters it is evident that most of the impacting projectile was ejected during crater formation. Less than 10% of the craters >100μm contain abundant residue consistent with survival of a major fraction of the projectile. In these cases the residue can be seen optically as a dark liner and it can easily be analyzed by SEM-EDX techniques. Because they are rare, the craters with abundant residue must be a biased sampling of the meteoroids reaching the earth. Factors that favor residue retention are low impact velocity and material properties such as high melting point. In general the SEM-EDX observations of crater residues are consistent with the properties of chondritic meteorites and interplanetary dust particles collected in the stratosphere.
Use of oriented polycrystalline films in x-ray optics
Authors: Wittry D. B. , Chang W. Z. , Barbee T. W.
Published: June 2020

X-ray diffractors having doubly curved crystal planes can have a high collection efficiency for radiation from a point source and can provide point-to-point focusing of monochromatic x rays as shown by some of the authors. These kinds of diffractors can be used to form x-ray microprobes that can give lower detection limits than electron microprobes or to make wavelength dispersive spectrometers with better signal and signal/background ratio than conventional ones employing the Johann or Johansson geometry. However, fabrication of diffractors of the desired geometry by the use of bent crystals has been difficult. In this paper, we explore the use of oriented polycrystalline films to fabricate doubly curved diffractors for x rays of short wavelength.

Oriented polycrystalline films (OPF) have been of interest for many applications, e.g., magnetic recording media, non-linear optical device components, inexpensive large-area substrates for semiconductor device fabrication, etc. These films consist of small monocrystalline grains that have a high degree of preferential orientation of one crystallographic axis relative to the substrate surface.
X-ray diffraction properties of curved crystal diffractors
Authors: Chang W. Z. , Wittry D. B.
Published: June 2020

Since Du Mond and Kirkpatrick first discussed the principle of a bent crystal spectrograph in 1930, curved single crystals have been widely utilized as spectrometric monochromators as well as diffractors for focusing x rays diverging from a point. Curved crystal diffraction theory predicts that the diffraction parameters - the rocking curve width w, and the peak reflection coefficient r of curved crystals will certainly deviate from those of their flat form. Due to a lack of curved crystal parameter data in current literature and the need for optimizing the choice of diffraction geometry and crystal materials for various applications, we have continued the investigation of our technique presented at the last conference. In the present abstract, we describe a more rigorous and quantitative procedure for measuring the parameters of curved crystals.

The diffraction image of a singly bent crystal under study can be obtained by using the Johann geometry with an x-ray point source.
Bence-albee after 25 years: A new superior α-factor correction procedure for the quantitative analysis of oxides and silicates
Authors: Armstrong John T.
Published: June 2020

One of the most cited papers in the geological sciences has been that of Albee and Bence on the use of empirical " α -factors" to correct quantitative electron microprobe data. During the past 25 years this method has remained the most commonly used correction for geological samples, despite the facts that few investigators have actually determined empirical α-factors, but instead employ tables of calculated α-factors using one of the conventional "ZAF" correction programs; a number of investigators have shown that the assumption that an α-factor is constant in binary systems where there are large matrix corrections is incorrect (e.g, 2-3); and the procedure’s desirability in terms of program size and computational speed is much less important today because of developments in computing capabilities. The question thus exists whether it is time to honorably retire the Bence-Albee procedure and turn to more modern, robust correction methods. This paper proposes that, although it is perhaps time to retire the original Bence-Albee procedure, it should be replaced by a similar method based on compositiondependent polynomial α-factor expressions.
Quantitative x-ray microfluorescence analysis of small areas and individual particles
Authors: Pella P. A. , Lankosz M. , Holynska B.
Published: June 2020

During the past few years, rapid progress has been made in the development of collimated x-ray sources which permit energy-dispersive x-ray analysis of small areas with dimensions below 100 μm. An x-ray microfluorescence spectrometer developed at NIST employs a commercial low-power (50 WATTS) x-ray tube providing a small focused x-ray beam (0.25 × 0.25 mm). The x-ray beam size was further reduced with a Mo collimator tipped with a Pt foil having a 70μm hole in the center. The x-ray beam profile was measured by step scanning across Cu wires 50 μm in diameter in both X and Y directions. The cross section of the beam was approximated by a Gaussian function with a FWHM of 43 μm. A schematic diagram of the spectrometer which is capable of operation in vacuum is shown in Figure 1.

Other features include a close coupled source-sample-detector for optimum count rate, a motorized x-y stage, and a color video camera for continuous viewing of the sample at normal incidence.
Defect analysis using a third-generation x-ray microdiffractometer with total reflection capillary x-ray optics
Authors: York Brian R.
Published: June 2020

We have built a third generation X-Ray Micro-Diffractometer (XRMD) which is capable of examining the structure of single grains as small as 3 microns by utilizing, in part, cylindrical or conical glass capillaries as x-ray focusing optics. The idea of using capillaries as total reflection focusing optics for x-ray diffraction is not new. However, these capillaries were usually of poor quality with inner diameters nominally larger than 10 microns, and due to the general unavailability of scanning XRMDs, and high brilliancy sources, they were used primarily with back reflection cameras. Cylindrical precision bore capillaries with thick internal walls, smooth enough to be suitable for use as total reflection x-ray focusing elements, are now commercially available in long sections with inner diameters as small as 10 microns. A methodology was established to fabricate, in-house, conical capillaries with inner diameters less than 3 microns and various taper geometries. Using such focusing elements the gain in the diffracted intensity, over that achievable using a simple aperture approach, could be varied up to 4X and 30X for cylindrical and conical capillaries respectively, by varying the capillary geometry, and are discussed below.