The presence of strain distributions within semiconductor features influences many aspects of their behavior. For example, microelectronic technology that incorporates strained silicon improves device performance by increasing carrier mobility in the Si channels. Because current semiconductor fabrication contains multiple levels of metallic and dielectric structures, an understanding of the mechanical response of the constituent elements is critical to the prediction of the overall device performance. In addition, the interaction of strain fields between adjacent structures becomes greater as feature sizes decrease and the corresponding feature density increases. The use of synchrotron-based X-ray methods allows one to determine the interaction between strained features and their environment at a submicron resolution. Real-space mapping of strain distributions in pseudomorphically strained, raised SiGe structures revealed that elastic relaxation extends approximately 20 times the feature thickness from their edges. X-ray topographic methods were also applied to map the substrate deformation induced by overlying SiGe features. A formulation based on the classical Ewald-von Laue theory of dynamical diffraction was derived to match the measured diffraction profiles.

The equation ε(φ, ψ, hkl)=Fij(φ, ψ, hkl)σij can be directly deduced from Hooke’s law. It is shown that the matrix Fij(φ, ψ, hkl) which is usually called X-ray elastic factors, behaves as a second rank tensor. Since this behaviour is the only criterion for the question of whether or not it is a tensor, the F-matrix must be regarded as a second rank tensor. This allows us to make some statements about the structure of the F-matrix on the basis of Neumann’s principle, to find relationships among F-matrices in different measurement directions, and to apply the methods and strategies for the measurement of a second rank tensor. All this is shown in a few examples. It is further shown that a consistent use of the F-matrix can replace all methods for data evaluation which makes use of linear regressions and, in addition, avoids all difficulties and disadvantages of these methods. One of these disadvantages is that the sin2 ψ-method, as well as its derivatives, is generally not correct least square fits of the measured data. This is also shown in an example. The more complicated cases with stress or constitution gradients in the range of the probed volume or stress measurement after plastic deformation are not discussed.

The method of high-energy total elastic X-ray scattering to determine the atomic structure of nanocrystalline, highly disordered, and amorphous materials is presented. The current state of the technique, its potential, and limitations are discussed with two successful studies on the pressure induced phase transition in mackinawite (FeS) and the high-pressure behavior of liquid gallium.

In situ deformation studies of polycrystalline materials using diffraction are an established method to understand elastic and plastic deformation of materials. Studies of active deformation mechanisms, the interplay of deformation with texture, and ultimately the development of predictive capabilities for deformation modeling are an active field of research. Parameters studied by diffraction are typically lattice strains and texture evolution, which coupled with the macroscopic flow curve allow for improved understanding of the micro-mechanics of deformation. We performed a study of the uniaxial deformation of Zircaloy-2 at 2 GPa at the 13-BM-D beamline at the Advanced Photon Source. The deformation-DIA apparatus generates a confining hydrostatic pressure using a cubic anvil setup. Two differential rams allow an increase (compressive load) or decrease (tensile load) of the uniaxial straining in the vertical direction, allowing studies of plastic deformation at high pressures. In this paper, we describe how macroscopic strains, hydrostatic pressure, and uniaxial strains are derived and present some brief results.

XRD analysis of plasma-vapor-deposited ErT2 films during aging (T decay to 3He) reveals an hkl-dependent unit-cell expansion in which (200) grains expand out-of-plane as much as 0.01 Å more than (111) out-of-plane grains. Texture analysis of an aged ErT2 film reveals a bimodal (111)/(200) out-of-plane preferred orientation. sin2 ψ analysis reveals significant in-plane macro-strain due to 3He bubble formation/growth. The mechanistic origins regarding these observations are also discussed.

Silver K edge extended X-ray absorption fine structure (EXAFS) spectroscopy of films containing silver behenate (AgBeh) in the unprocessed, fully processed, and step-processed states has been performed. The results of the EXAFS analysis indicate that the intensity for the real-space peak for the Ag-O distance (∼2.3 Å) decreases while the real-space peak for the Ag-Ag distance (∼2.9 Å) grows with increasing thermal processing of the film. The changes observed in the real-space EXAFS signal indicate the growth of metallic silver at the expense of AgBeh. The X-ray absorption near-edge spectroscopy (XANES) portion of the signal shows that the absorption edge position varies stepwise, with unprocessed films and pure AgBeh having an edge location at 25 506 eV, films processed from steps 1 through 10 have an absorption edge at 25 508 eV, and the fully processed film has an edge location at 25 512 eV.

The painting materials and drawing techniques of a pair of two-panel folding screens entitled Red and White Plum Blossoms by Ogata Korin, a national treasure in Japan, were investigated directly and nondestructively by XRF, X-ray radiography, and high resolution digital imaging. Several assumptions were made about the materials used in the red and white plum trees drawn on the right and left screens, respectively, and the river drawn at the center. By the present investigation, the materials used for the paintings were revealed, and some of them contradicted what have been previously believed.

Techniques for estimation of element levels directly in humans (noninvasive in vivo) or in samples (in vitro) from humans are reviewed. Toxic, nonessential, trace elements may cause temporary or permanent damage to various organs and tissues in humans. There is thus a need to control the concentrations. Knowledge of the relations between toxic effects and element concentration may be extracted from measurements in humans as well as in samples from humans and her environment. Applications traditionally include occupationally exposed subjects, but an increasing research area is studies of members of the general population and of patients undergoing therapy for malignant and other diseases. Most in vivo XRF studies deal with lead in bone and cadmium in kidneys. For retired lead workers, a clear association has been demonstrated between bone lead and blood lead, due to endogenous lead excretion from the skeleton. A study of mercury in vivo showed that the technique is capable of detecting mercury in heavily exposed worker’s kidneys. In vivo XRF in cancer and rheumatology patients has helped to understand how platinum and gold are retained in the human body. The newest in vivo applications include zinc in prostate gland and arsenic in skin.

We report on the use of a microcalorimeter X-ray detector with a transition edge sensor in an electron probe to perform quantitative analysis. We analyzed two bulk samples of multielement glasses that have been previously characterized by chemical methods for use as standard reference materials. The spectra were analyzed against standards using three different correction schemes. In one of the standards, the reference line was easily resolved despite its proximity within 45 eV of another line. With the exception of direct measurements of oxygen (a particularly challenging element), the results are in agreement with the certified characterization to better than 1% absolute or 8% relative. This demonstrates the potential of microcalorimeter detectors as replacements for conventional energy dispersive detectors in applications requiring high energy resolution.

European Community Directive 2002∕95∕EC restricts the use of certain hazardous substances in electrical and electronic equipment. In particular, restrictions are placed on lead, mercury, cadmium, hexavalent chromium, and bromine (in polybrominated biphenyls or polybrominated diphenyl ethers). XRF is a convenient method for detecting the presence and measuring the amounts of these elements. Reliably quantifying all of these elements in plastics typically requires a large number of standards that are not yet readily available. Because of the light element matrix, using a “standardless” fundamental parameters method requires some reliance on the primary beam scatter, complicating the analysis algorithm and increasing the uncertainty. We have tested a simplified fundamental parameters method that determines the matrix via difference, requiring only one standard. The method was tested on a series of reference materials containing all of the regulated elements in a variety of plastic resins. One multi-element reference standard was used. It was necessary to include all of the additives in the specimens to achieve good quantitative accuracy. In addition, the scattered primary intensity was used in one set of tests to compensate for variations in specimen thickness. This thickness compensation was necessary to get acceptable results for Cd. Results were very promising, with average relative errors and relative standard deviations of about 10%.

The value assignment of candidate Standard Reference Material (SRM®) 57b Silicon Metal provided an opportunity to develop an alkali reaction procedure as a precursor to borate fusion for the preparation of test specimens from the metal powder for X-ray fluorescence spectrometry (XRF). Suggested for this purpose by Blanchette in a 2002 Advances in X-ray Analysis article [45, 415–420 (2002)], the alkali reaction uses LiOH∙H2O to convert Si to Li2SiO3. Lithium silicate is fused with lithium borate flux without damage to platinum ware. Once specimens are fused and cast as beads, calibration standards are prepared to closely match the compositions of the specimens, allowing a linear calibration for each analyte. The XRF method yields results that are directly traceable to the mole through NIST SRM spectrometric solutions. The method was validated in two ways. First, the reaction was used on older SRMs for Si metal: SRM 57 and SRM 57a. Second, XRF results for candidate SRM 57b were compared to results obtained using prompt gamma-ray activation analysis (PGAA) and inductively coupled plasma optical emission spectrometry (ICPOES). Bias tests show the XRF results are accurate for the elements Al, S, Ca, Ti, Cr, Mn, Ni, Cu, and Zr. Levels of S, Ca, Cr, and Cu in candidate SRM 57b are near the limits of quantification of the borate fusion method. Iron results may be subject to a low bias. Phosphorus is not quantitatively retained during the alkali reaction and borate fusion. These elements, plus B, which cannot be determined after borate fusion, are listed in manufacturing specifications for Si metal.

A novel method for preparing thin films was investigated for quantifying gallium and iron in plutonium solutions using WDXRF. This technique was developed to eliminate the potential for radioactive liquid to leak into the spectrometer, decrease specimen preparation time, and minimize waste. Samples were cast in μL quantities onto Kapton, and a surfactant was added to disperse the solution uniformly across the Kapton. After drying the specimens, they were sealed in a cell for analysis. Results to date indicate the method can provide a relative precision of ∼0.5% for gallium and ∼2% for iron, which is more than sufficient for routine sample analyses.