X-ray diffraction imaging (XRDI) (topography) measurements of silicon die warpage within fully packaged commercial quad-flat no-lead devices are described. Using synchrotron radiation, it has been shown that the tilt of the lattice planes in the Analog Devices AD9253 die initially falls, but after 100 °C, it rises again. The twist across the die wafer falls linearly with an increase in temperature. At 200 °C, the tilt varies approximately linearly with position, that is, displacement varies quadratically along the die. The warpage is approximately reversible on cooling, suggesting that it has a simple paraboloidal form prior to encapsulation; the complex tilt and twisting result from the polymer setting process. Feasibility studies are reported, which demonstrate that a divergent beam and quasi-monochromatic radiation from a sealed X-ray tube can be used to perform warpage measurements by XRDI in the laboratory. Existing tools have limitations because of the geometry of the X-ray optics, resulting in applicability only to simple warpage structures. The necessary modifications required for use in situations of complex warpage, for example, in multiple die interconnected packages are specified.

Validating phase quantification procedures of powder X-ray diffraction (XRD) data for an implementation in an ISO/IEC 17025 accredited environment has been challenging due to a general lack of suitable certified reference materials. The preparation of highly pure and crystalline reference materials and mixtures thereof may exceed the costs for a profitable and justifiable implementation. This study presents a method for the validation of XRD phase quantifications based on semi-synthetic datasets that reduces the effort for a full method validation drastically. Datasets of nearly pure reference substances are stripped of impurity signals and rescaled to 100% crystallinity, thus eliminating the need for the preparation of ultra-pure and -crystalline materials. The processed datasets are then combined numerically while preserving all sample- and instrument-characteristic features of the peak profile, thereby creating multi-phase diffraction patterns of precisely known composition. The number of compositions and repetitions is only limited by computational power and storage capacity. These datasets can be used as input files for the phase quantification procedure, in which statistical validation parameters such as precision, accuracy, linearity, and limits of detection and quantification can be determined from a statistically sound number of datasets and compositions.

A provisional setup for X-ray microprobe experiments at 35 keV is described. It is based on compound refractive lenses (CRLs) for nanofocusing and a Vortex silicon drift detector with 2 mm sensor thickness for increased sensitivity at high energies. The Microprobe experiment (PETRA III) generally uses Kirkpatrick-Baez mirrors for submicrometer focusing in the energy range of 5–21 keV. However, various types of scanning X-ray microscopy experiments require higher excitation energies. The CRL optics were characterized by X-ray ptychography and X-ray fluorescence (XRF) knife edge scans on a siemens star pattern and showed beam sizes down to 110 nm. The performance of the new setup for microscopic X-ray diffraction (XRD)–XRF scanning X-ray microscopy measurements at 35 keV is demonstrated on a cross-section of a painting fragment.

A commercial Empyrean X-ray diffractometer was adapted for combined grazing incidence X-ray fluorescence analysis (GIXRF) measurements with X-ray reflectivity (XRR) measurements. An energy-dispersive silicon drift detector was mounted and integrated in the angle-dependent data acquisition of the Empyrean. Different monochromator/X-ray optics units have been compared with the values obtained by the Atominstitut GIXRF + XRR spectrometer. Data evaluation was performed by JGIXA, a special software for combined GIXRF + XRR data fitting, developed at Atominstitut. A sample consisting of a ~50 nm nickel layer on a silicon substrate was used to compare the performance criteria (i.e. divergence and intensity) of the incident beam optics. An Empyrean X-ray diffractometer was successfully refitted to measure both GIXRF and XRR data.

The I13 transmission X-ray microscope at Diamond Light Source (DLS) has been designed to cover a broad range of energies and field of views. The beamline operates on an undulator source, and a multilayer monochromator can be used to work at a larger bandwidth to enable faster acquisitions. The experimental design includes large working distances for the optics to allow installing in situ sample environments. This paper presents the current state of the experimental system and shows some of the latest results.

The ICDD's Powder Diffraction File™ (PDF®) is a database of inorganic and organic diffraction data used for phase identification and materials characterization by powder diffraction. The PDF has been available for over 75 years and finds application in X-ray, synchrotron, electron, and neutron diffraction analyses. With entries based on powder and single crystal data, the PDF is the only crystallographic database where every entry is editorially reviewed and marked with a quality mark that alerts the user to the reliability/quality of the submitted data. The editorial processes of ICDD's quality management system are unique in that they are ISO 9001:2015 certified. Initially offered as text on paper cards and books, the PDF evolved to a computer-readable database in the 1960s and today is both computer and web accessible. With data mining and phase identification software available in PDF products, and the databases’ compatibility with vendor (third party) software, the 1 000 000+ published PDF entries serve a wide range of disciplines covering academic, industrial, and government laboratories. Details describing the content of database entries are presented to enhance the use of the PDF.