Characterization of materials used in the digital imaging industry has been performed using micro X-ray diffraction (microXRD) techniques. Case studies are described that demonstrate the use of microXRD for identification of phases, texture, and microstructure morphology of components used in imaging applications.

A state-of-art semiconductor technology-based position sensitive area detector, namely D/teX-25, has recently been developed for high-speed and high-sensitivity X-ray diffraction (XRD) analysis of materials. X-ray powder diffraction intensities obtained by a D/teX-25 detector were found to over 50 times higher than those by a conventional scintillation counter. A D/teX-25 detector mounted on a conventional 2 kW XRD system has been used to collect ultrafast XRD data with scanning speeds up to 160°2θ per minute. Ultrahigh-speed XRD is particularly useful for time-resolved dynamical and in-situ studies. A D/teX-25 detector was successfully used on a Rigaku XRD differential scanning calorimetry (DSC) system for simultaneous measurements of XRD and DSC data under controlled temperature and humidity conditions. This has made possible the study of complex and rapid phase transformations of pharmaceutical terfenadine. The D/teX-25 area detector has also been used for recording two-dimensional XRD patterns showing the particle-size effects on α-quartz powder intensities and to obtain digital X-ray topographic images of a complex dislocation network in a Si wafer.

The Interactive Data Language has been used to produce a software program capable of advanced three-dimensional visualizations of pole figure and θ-2θ data. The data can also be used to calculate quantitative properties such as strain level and to minimize the peak-height texture effects in individual θ-2θ scans. The collection of the large data sets necessary for the analyses is facilitated by use of a position sensitive detector or area detector.

Developments in X-ray analysis hardware and software have combined to dramatically improve the throughput, speed, and accuracy of formulation analyses. We will focus on a complimentary development, the growth and application of a comprehensive database based on the Powder Diffraction File™ (PDF®). The PDF is an edited and standardized combination of several crystallographic databases with ∼497 000 published entries. The comprehensive nature of this database, combined with phase identification and digital pattern simulations, was used to identify complex formulations with crystalline and noncrystalline ingredients. We will show how these parallel developments enhance the ability to correctly identify complex formularies.

A study examining the feasibility, and possible necessity, of using transmission data from capillary mounted samples for quantitative analysis of hydrated cement systems was conducted. In order to obtain true quantitative results, the amorphous contents were determined by the addition of an internal standard. The amorphous content of the starting tricalcium silicate was found to be approximately 21–22 wt %, in close agreement with previously published results. The study revealed that the spherical harmonics preferential orientation correction may not be reliable with unmicronized hydrated cement materials in reflection geometry, as chemically unreasonable progressions in Portlandite content with time were observed. The data obtained from capillary measurements, however, exhibited little or no preferential orientation, and appeared to produce the progression of phase contents expected from the reaction. The use of capillaries would appear to be justified in some circumstances to obtain reliable quantitative results from hydrated cementitious materials. In this particular system, a significant fraction of calcium carbonate was present as aragonite, as well as the more usual calcite.

We discuss the impact of strong absorption for thermal neutrons on data analysis and compare absorption corrections in the GSAS and MAUD Rietveld codes for texture and structural parameter refinement. Diffraction data were collected on the neutron powder diffractometer HIPPO at LANSCE from dysprosium and erbium, which are moderate-to-strong absorbers for thermal neutrons with absorption cross sections of 159 barns for Er and 994 barns for Dy at λ=1.8 Å. Both elements have hexagonal-close-packed (hcp) crystal structures, and the samples were various thicknesses of rolled foils. The orientation distribution functions (ODF) were fit to the same neutron time-of-flight data sets using two very different full pattern Rietveld analysis procedures. Spherical harmonics functions were fit to the textured data using GSAS. These data were also analyzed by the modified direct method E-WIMV using MAUD. The resulting pole figures from the ODFs determined by both Rietveld analysis packages are qualitatively similar, and the textures were confirmed by X-ray diffraction. Additionally, data from orthorhombic dysprosium and erbium fluoride powders show that atomic positions are not sensitive to absorption. We address inconsistencies and methodologies in data analysis when strong absorption is present.

In this study, we use X-ray diffraction (XRD) and micro-Raman spectroscopy (MRS) to measure internal strains in sensors embedded in polymer matrix composites. Two types of strain sensors embedded in either chopped graphite fiber∕epoxy matrix composite (MRS) or unidirectional graphite fiber∕polyimide matrix composite (XRD) were investigated. For XRD measurements, the sensors were in the form of spherical aluminum inclusions with diameters ranging from 1 to 20 μm. Due to large cross section area of an incident X-ray beam, only average stresses are reported using the XRD approach. Complementary to XRD experiments, MRS was pursued to measure internal strains in Kevlar-49 fibers embedded in chopped graphite fiber∕epoxy matrix composite. In recent years, MRS as an experimental tool for microstrain measurements has drawn considerable attention mostly due to its excellent spatial resolution. The resolution of MRS typically ranges between 1 and 10 μm, which means that strains can be measured in individual sensors. The principle of this method relies on a change of certain molecular vibration frequencies as a result of an applied stress. Several examples are presented and discussed to demonstrate the potential of combining micro and macrostrain measurements and modeling to capture the stress distribution in heterogeneous materials.

In this study, the effects of growth interruptions on the formation of the interfaces in GaAs∕AlAs multilayers are investigated. For that purpose, a series of different samples has been manufactured with molecular-beam epitaxy. The introduction of growth interruptions of 50 s after the deposition of the layer leads to a change in the morphological properties of the interfaces, in particular their correlation length. These modifications due to the growth interrupt are analyzed with diffuse X-ray scattering. As a result of the measurements, an extension of the lateral correlation length can be proved. By contrast, the vertical correlation of the interfaces is not affected.

For research facilities with access to synchrotron X-ray sources, X-ray absorption microtomography (XMT) has evolved from an experimental imaging method to a specialized, if not yet routine, microscopy for imaging the three-dimensional (3D) distribution of linear attenuation coefficients and, in some cases, elemental concentration with micron spatial resolution. Recent advances in source and detector design have produced conventional X-ray source instruments with comparable spatial resolution but with lower throughput and without element specific imaging. Both classes of instrument produce 3D images for analysis. We discuss an integrated approach for the implementation of analytical XMT to support basic research into the structure-property relationships of a variety of materials. The essential components include instrumentation for collecting quantitative 3D images, a 3D image processing environment to address questions as to the quantity, composition, geometry, and relationships among the features in one or more images, and visualization to provide insight and communicate results. We give examples of image analysis of resolved and unresolved pore spaces of sandstones.

X-ray imaging techniques based on Compton backscatter permit inspection and screening of sea containers, a wide variety of vehicles, luggage, and even people. In contrast to more commonly used transmission images, backscatter imaging involves positioning both source and detection apparatus on only one side of a target object. This presents the user with inspection opportunities in situations that may be extremely difficult, if not impossible, for transmission systems that require access by the detector subsystem to the opposing side of the target. The backscatter image is somewhat akin to a photograph of the contents of a closed container, taken through the container walls. Techniques for producing X-ray images based on Compton scattering will be discussed, along with wide-ranging examples of how systems based on these principles are used to perform inspections for both security applications and for the detection of contraband materials at ports and borders. Potential applications in the area of nondestructive evaluation will also be considered. Differences in the type of information displayed by transmission and backscatter images will be highlighted, and tradeoffs between backscatter image quality and interpretability, scan speed, effective penetration, and X-ray tube voltage will also be discussed. The method used in scanning the target object results in an extremely low radiation dose, a result that significantly broadens the application spectrum for this imaging technique.

Numerous methods are available to forensic scientists for detecting fingerprints in which the prints are treated with various agents to enhance the visual contrast between the print and the surface. In the present work, the spatial elemental imaging capabilities of micro-X-ray fluorescence (MXRF) were used to visualize fingerprint patterns based on inorganic elements present in the prints. A major advantage of using MXRF is that the prints are left unaltered for other analyses, such as deoxyribonucleic acid extraction or for archiving. Most of the fingerprints which were examined were imaged from the potassium and chlorine present in the print residue. Among the various prints studied, lower count rates were also observed in the elemental maps of Ca, Al, Na, Mg, Si, P, S, and the X-ray source scatter. A sebaceous oily fingerprint left by one subject was successfully imaged by MXRF, but sebaceous prints left by a different person were undetectable, indicating that print elemental composition may be person and/or diet dependent. Prints containing substances that might be found in real-world cases were also visualized including sweat, lotion, saliva, and sunscreen.

An electron probe X-ray microanalysis (EPMA) technique using an energy-dispersive X-ray detector with an ultrathin window, designated low-Z particle EPM, has been developed. The low-Z particle EPMA allows the quantitative determination of concentrations of low-Z elements, such as C, N, and O, as well as higher-Z elements that can be analyzed by conventional energy-dispersive EPMA. The quantitative determination of low-Z elements (using full Monte Carlo simulations, from the electron impact to the X-ray detection) in individual environmental particles has improved the applicability of single-particle analysis, especially in atmospheric environmental aerosol research; many environmentally important atmospheric particles, e.g. sulfates, nitrates, ammonium, and carbonaceous particles, contain low-Z elements. The low-Z particle EPMA was applied to characterize loess soil particle samples of which the chemical compositions are well defined by the use of various bulk analytical methods. Chemical compositions of the loess samples obtained from the low-Z particle EPMA turn out to be close to those from bulk analyses. In addition, it is demonstrated that the technique can also be used to assess the heterogeneity of individual particles.

The versatility of confocal micro X-ray fluorescence (MXRF) in analyzing thin films on semiconductor wafers is demonstrated. Unlike conventional MXRF, confocal MXRF can depth profile sample layers and reduce spectral background. Nondestructive quantification of the silicon dioxide concentration in hafnium silicate thin films is an example of one application demonstrating the advantage of confocal MXRF. Additionally, the growth of titanium nitride films on various high-k gate dielectric substrates was analyzed with confocal MXRF due to its ability to detect sub-nm film thickness changes.

One of the main threats to human health from heavy metals is associated with the exposure to lead (Pb). In vivo X-ray fluorescence analysis (XRF) of human bone is a widely used technique to determine the total Pb body burden. The intention of this work was to study the feasibility of in vivo L-shell XRF measurements of Pb in bone using X-ray tubes as excitation sources. Parameter studies using direct tube excitation with various anode materials (Mo and W) and filters as well as different secondary targets and low-Z polarizers were performed with regard to the lowest limits of detection (LLD) achievable for Pb in bone matrix. A breakthrough for the development of a portable spectrometer was achieved by using an air-cooled low-power (50 W) Pd anode X-ray tube, Mo secondary target, and a Peltier-cooled silicon drift detector. LLDs for Pb in bone were determined from measurements on a plaster-of-paris standard without overlying tissue equivalent material and found to be around 0.6 μg∕g.

Rapid and accurate methods are becoming available to calculate all of the relevant physical effects that contribute to an energy-dispersive X-ray fluorescence (EDXRF) spectrum, rather than just the characteristic line intensities given by the traditional fundamental parameters method. To evaluate the utility of such methods, we have calculated the full spectra of several compounds covering a wide range of compositions. The calculated spectra are compared directly with measured spectra. They include scattering of the X-ray tube lines and continuum, the Compton profile, and the detector response. Our results indicate that it is now possible to compute the full spectrum from an EDXRF system with very good accuracy.

Low energy characteristic X-ray emission from Al2O3 monocrystalline specimens is measured under bombardment of 100 keV Xe+ ions. The electric field influence on emission of the X-rays of constitute elements in the specimens was investigated. The energy dispersive X-ray spectroscopy spectra show that the characteristic X-ray of Al-Kα seems to be depressed by the applied dc voltages, while the peak intensity of O-Kα was not notably influenced. The O-Kα peaks were broadened and the total counts increased as a higher dc bias was applied. It is possible that a dc electric field parallel to the target surface may influence the X-ray emission from it under ion bombardment.