High-resolution powder X-ray diffraction and density functional plane wave pseudo-potential techniques have been used to obtain an optimized structural model of silver arachidate, [Ag(O2C(CH2)18CH3]2. The unit cell is triclinic, space group P-1 with cell dimensions of a = 4.1519(10) Å, b = 4.7055(10) Å, c = 53.555(4) Å, α = 89.473(15)°, β = 87.617(5)° and γ = 76.329(5)°. The structure is characterized by an 8-membered ring dimer of Ag atoms and carboxyl groups joined by four-member Ag–O rings with fully extended zigzag side chains, giving rise to one-dimensional chains along the b-axis.

National Security Technologies (NSTec) has developed calibration procedures for X-ray imaging systems. The X-ray sources that are used for calibration are both diode type and diode/fluorescer combinations. Calibrating the X-ray detectors is a key to accurate calibration of the X-ray sources. Both energy dispersive detectors and photodiodes measuring total flux were used. We have developed calibration techniques for the detectors using radioactive sources that are traceable to the National Institute of Standards and Technology (NIST). The German synchrotron at Physikalische Technische Bundestalt (PTB) was used to calibrate the silicon photodiodes over the energy range from 50 to 60 keV. The measurements on X-ray cameras made using the NSTec X-ray sources included quantum efficiency averaged over all pixels, camera counts per photon per pixel, and response variation across the sensor. The instrumentation required to accomplish the calibrations is described. The X-ray energies ranged from 720 to 22.7 keV. The X-ray sources produce narrow energy bands, allowing us to determine the properties as a function of X-ray energy. The calibrations were done for several types of imaging devices. There were back and front illuminated CCD (charge-coupled device) sensors, and a CID (charge injection device) type camera. The CCD and CID camera types differ significantly in some of their properties that affect the accuracy of the X-ray intensity measurements. All the cameras discussed here are silicon based. The measurements of the quantum efficiency variation with the X-ray energy are compared to the models for the sensor structure. The cameras that are not back-thinned are compared to those that are.

A software for the calculation of diffraction elastic constants (DEC) for materials both with and without preferred orientation was developed. All grain-interaction models that can use the crystallite orientation distribution function (ODF) are incorporated, including Kröner, Hill, inverse Kröner, and Reuss. The functions of the software include: reading the ODF in common textual formats, pole figure calculation, calculation of DEC for different (hkl,φ,ψ), calculation of anisotropic bulk constants from the ODF, calculation of macro-stress from lattice strain and vice versa, as well as mixture ratios of (hkl) of overlapped reflections in textured materials.

The manufacture of ultra-large scale integration technology can impose significant strain within the constituent metallization because of the mismatch in coefficients of thermal expansion between metallization and its surrounding environment. The resulting stress distributions can be large enough to induce voiding within Cu-based metallization, a key reliability issue that must be addressed. The interface between the Cu and overlying capping layers is a critical location associated with void formation. By combining conventional and glancing-incidence X-ray diffraction, depth-dependent stress distributions that develop in Cu films and patterned features are investigated. In situ annealing and as-deposited measurements reveal that strain gradients are created in capped Cu structures, where an increased in-plane tensile stress is generated near the Cu/cap interface. The interplay between plasticity in Cu and the constraint imposed by capping layers dictates the extent of the observed gradients. Cu films possessing caps deposited at temperatures where Cu experienced only elastic deformation did not exhibit depth-dependent stress distributions. However, all capped Cu samples exposed to temperatures that induce plastic behavior developed greater tensile stress at the Cu/cap interface than in the bulk Cu film after cooling, representing a clear concern for the mitigation of metallization voiding.

Total reflection X-ray fluorescence spectrometry (TXRF) was used to analyze residual surface contamination on Genesis solar wind samples and to evaluate different cleaning methods. To gauge the suitability of a cleaning method, two samples were analyzed following cleaning by lab-based TXRF. The analysis comprised an overview and a crude manual mapping of the samples by orienting them with respect to the incident X-ray beam in such a way that different regions were covered. The results show that cleaning with concentrated hydrochloric acid and a combination of hydrochloric acid and hydrofluoric acid decreased persistent inorganic contaminants substantially on one sample. The application of CO2 snow for surface cleaning tested on the other sample appears to be effective in removing one persistent Genesis contaminant, namely germanium. Unfortunately, the TXRF analysis results of the second sample were impacted by relatively high background contamination. This was mostly due to the relatively small sample size and that the solar wind collector was already mounted with silver glue for resonance ion mass spectrometry (RIMS) on an aluminium stub. Further studies are planned to eliminate this problem. In an effort to identify the location of very persistent contaminants, selected samples were also subjected to environmental scanning electron microscopy. The results showed excellent agreement with TXRF analysis.

Micro-X-ray fluorescence (XRF) analysis provides us with elemental maps that are very useful for understanding the samples under test. Usually, scanning-type elemental mapping is performed. That means a sample stage is scanned to a fixed X-ray microbeam. XRF analysis is performed at the scanned points, leading to 2D elemental mapping. One of the drawbacks of this technique is the long acquisition time depending on the area being mapped and the lateral resolution required. Thus, projection-type elemental mapping has been studied. We have studied the projection type XRF imaging by using a straight polycapillary optic combined with an X-ray CCD camera. To obtain the elemental map, we applied a wavelength dispersive spectrometer (WDS). In this paper, we report a newly developed 2D dispersive device. The construction and analytical performance of this X-ray optic will be explained.