The monoclinic-to-tetragonal phase transition (~70 °C) in vanadium dioxide (VO2) strongly impacts the infrared properties, which enables its use in applications such as smart window devices. Synthesis of VO2 can be challenging due to the variability of vanadium oxide phases that may be formed. We have employed high-temperature X-ray diffraction (HTXRD) to monitor the reaction process of vanadium oxide precursor powders to form the desired tetragonal VO2 phase. Single-phase tetragonal VO2 was formed within 30 min at 420 °C in flowing N2 gas (~50 ppm O2). The monoclinic-to-tetragonal phase transformation was observed via HTXRD at ~70 °C with the typical ~10 °C hysteresis (i.e. approached from above or below the transition).

Developments in X-ray analysis, and advances in scientific research, have dramatically influenced the types of data now considered suitable for inclusion in the Powder Diffraction FileTM (PDF®). Initially, the PDF was geared towards the identification of unknown crystalline materials by comparison of d-spacings and peak intensities. Today, the International Centre for Diffraction Data (ICDD) maintains and continuously enhances the quality and content of the PDF database to better provide customers and scientists with a comprehensive reference source that supports their needs, and interests. The events that initially led to the inclusion of crystalline polymer data to the PDF have recently been amended to also encompass semi-crystalline and amorphous polymeric materials as well. This paper discusses the resultant updates being made to the PDF in support of this new data form, and also highlights several features and benefits of providing this data to PDF users.

A Debye–Scherrer film that had been stored for several years in an office environment file cabinet was observed to be shriveled and distorted in appearance. An investigation using X-ray diffraction was carried out to determine the cause of the physical change in the film strip. As expected, silver phases were detected, due to the photographic capture layer coated on the surface of all traditional X-ray films. An unexpected result was the presence of cellulose II, an indication that a chemical change had occurred in the original cellulose triacetate (CTA) polymer film base. Laboratory experiments used to demonstrate an accelerated method of deacetylation of CTA were carried out, resulting in phase pure cellulose II. A density functional geometry optimization allowed for the generation of an improved structural model for cellulose II. Calculated and experimental powder patterns for cellulose II have been submitted to the International Centre for Diffraction Data for inclusion in future releases of the Powder Diffraction File.

Two-dimensional X-ray diffraction (XRD2) pattern can be described by the diffraction intensity distribution in both 2θ and γ-directions. The XRD2 images can be reduced to two kinds of profiles: 2θ-profile and γ-profile. The 2θ-profile can be evaluated for phase identification, crystal structure refinement, and many applications with many existing algorithms and software. In order to evaluate the materials structure associated with the intensity distribution along γ-angle, either the XRD2 pattern should be directly analyzed or the γ-profile can be generated by 2θ-integration. A γ-profile contains information on texture, stress, crystal size, and crystal orientation relations. This paper introduces the concept and fundamental algorithms for stress, texture, and crystal size analysis by the γ-profile analysis.

At the Institute of Microstructure Technology (IMT) of the Karlsruhe Institute of Technology (KIT), a new type of refractive X-ray optics has been developed. Owing to its comparably easy fabrication method and the large aperture, the so-called Rolled X-ray Prism Lenses (RXPL) have the potential to be used with X-ray tubes in an industrial environment as a low-cost alternative to existing optics. The lens itself is built out of a micro-structured foil which is cut into shape and rolled around a winding core to form a refracting element for X-rays. The resulting refractive structure can be used as illumination optics. Diffractometry experiments with an NIST 1976a sample were performed and showed up to an 18-fold enhanced integrated intensity compared to that acquired with a steel tube collimator.

The dependence of polymer properties on their processing history can be used advantageously. Polyethylene terephthalate (PET), a semi-crystalline polymer, exhibits a microstructure reliant on process and thermal history. PET undergoes strain-induced crystallization, making it sensitive to mechanical stretching. As the level of crystallinity in PET governs its mechanical behavior, it is necessary to quantify the effect of crystallinity and molecular orientation for efficient use. The present research is focused on an approach that will aid in correlating the stretch ratio of PET films to the percent crystallinity and mechanical properties. PET films with different local stretch ratios were obtained through bi-axially stretching injection-molded cylinders of increasing thickness and weight. Percent crystallinity of the PET films with different stretch ratios was measured using X-ray diffraction. Film samples were marked with respect to the stretch directions for measuring their longitudinal (primary stretch direction) and transverse mechanical properties. Local molecular orientation in the form of pole figures was mapped using the (100) plane corresponding to the PET lattice. This will help in linking the physical sample directions and processing to the molecular orientation. Associating the mechanical properties with molecular alignment helps in designing production processes that realize the material's structural potential.

This paper summarizes an oral presentation of the same title presented at the occasion of recognizing the “The 100th Anniversary of X-ray Spectroscopy” at DXC 2013. It gives an overview of the development in electronics with focus on (mainly) energy-dispersive X-ray detectors and related data processing. Naturally this has its origin in the early transistors and the first semiconductor junction detectors of the late 1940s. It was followed by refinement of semiconductor detector technology in general and particularly by the invention of Li-drifting and employment of low-noise field effect transistors until such devices matured sufficiently to be marketed by the late 1960s. Further improvement followed in resolution, speed, operability at room temperature, and development of junction arrays with imaging capabilities. An important aspect is the development of related software requiring affordable laboratory computers, programming languages, and databases of fundamental parameters. Today x-ray fluorescence analysis (and not only the energy-dispersive variant) is widely employed as an analytical tool for the traditional technical and industrial applications but notably also, at an expanding rate as well as variety, in other fields including environmental, medical, archaeological, space, arts, and many more.

Residual stress measurements on strongly textured materials using the standard sin2ψ evaluation show significant non-linearities. According to EN 15305 there is currently no existing solution for this problem. A method is presented that solves this problem. It is based on two tools. (i) The use of a one-dimensional detector having a large capture angle that yields the full diffraction profiles at each point of the pole figures. Therefore, some hundreds of d-values can be used for the stress calculation. (ii) Data evaluation with the recently developed generalized sin2ψ method. This has the advantage of being based on a flawless theory (Hooke's law in the special form of Dölle–Hauk's equation) and being able to handle any distribution of measurement directions and any number of measured data. The method was successfully tried out at a sheet of brass with significant texture.

Interest in atmospheric aerosol issues has been increasing worldwide. X-ray fluorescence (XRF) is an important atmospheric aerosol monitoring tool for inorganic component analysis, because XRF is a rapid and easy analysis method. In particular, Energy dispersive X-ray fluorescence (EDXRF) has drawn attention for aerosol analysis. However, EDXRF has difficulties that: (1) many overlapping peaks exist for aerosol filter analysis and (2) many thin-film standard samples are required when an empirical calibration method is employed. Accurate analysis method of aerosol filter samples without the need for large sets of standards by semi-quantitative analysis software RPF–SQX (Rigaku profile fitting–spectra quant X), which includes the exact profile fitting and thin-film fundamental parameter (FP) method, is described using the EDXRF spectrometer equipped with secondary targets and polarized optics.

Calcium monoaluminate is the main phase in calcium aluminate cements and participates in the hydration, forming calcium aluminate hydrates. The amount of incorporation of foreign ions influences the hydration behaviour. Strontium aluminate is an important phase in producing phosphorescent materials when doped with rare-earth elements (REE) such as Eu, Dy, and La. These monoaluminates occur in different forms. Monocalcium aluminate forms a monoclinic and an orthorhombic modification, whereas monostrontium aluminate forms a monoclinic low-temperature and a hexagonal high-temperature form. Monoclinic calcium monoaluminate and monoclinic strontium aluminate form a partial solid-solution series. The hydration behaviour of different solid solutions was also investigated using calorimetry. The newly formed strontium aluminate hydrates could be identified while similar strontium aluminate hydrates are formed. Solid solutions of strontium- and calcium-aluminate hydrates will be investigated.

Stability of Na-titanate-based nanotubes at high temperature and pressure is investigated using X-ray diffraction and energy-dispersive X-ray diffraction (EDXRD). Our results show that the nanotubes can be stable at ~400 °C. Higher temperature annealing of nanotubes result in opening and flattening of the nanotubes, and subsequent structural transformation to Na2Ti6O13-based structure via an intermediate phase with Na0.23TiO2-like structure. In situ EDXRD using diamond anvil cell indicates that the nanotubes collapse at about 15 GPa, and are finally transformed into an amorphous phase at about 30 GPa. The nanotubes kept in an amorphous state were further compressed to 50 GPa according to our in situ EDXRD observation. Titanate nanotubes are mechanically stronger than carbon nanotubes under static compression.

A confocal micro-X-ray fluorescence (XRF) method with a vacuum chamber was used for investigation of underfilm corrosion that occurs on a painted steel sheet used for automotive applications. A painted steel sheet was prepared by applying electrodeposition coating onto an electro-galvanized steel sheet with a zinc phosphate conversion coating. The spatial resolution of the confocal micro-XRF was about 10.9 ?m at an energy of 17.4 keV. The phosphorus signal from the zinc phosphate layer was able to be observed nondestructively by measuring under the vacuum condition. Each layer of the painted steel sheet was observed from the depth profile analysis of the characteristic elements of each layer. The painted steel sheet was scratched to expose the substrate surface, and then the sheet was then immersed in a NaCl solution for 10 days. The in-depth elemental map of Ti of the corroded steel sheet revealed blister-type corrosion around the scratch. The in-depth elemental maps of Zn and P suggested that the zinc phosphate layer dissolved from the scratched part into the NaCl solution.

The human eye is continuously exposed to the environment yet little is known about how much of toxins, specifically heavy metals are present in its different parts and how they influence vision and acuity. To shed light into this subject, aqueous humor and lens samples were collected from 14 cataract patients to study the presence and concentration of selected metals in the eye. Subjects undergoing routine cataract surgery were consecutively enrolled for study by simple random sampling. Prior to surgery, subject demographic were compiled. The surgical procedure involved small incision cataract removal using phacoemulsification. During the procedure, a small aliquot of aqueous humor was retained for analysis, whereas homogenized lens fragments were obtained during phacoemulsification. A balanced salt solution was used as control for each set of samples. Both ocular specimens were analyzed by total reflection X-ray fluorescence spectrometry after dilution and addition of an internal standard. The data obtained show substantial variations in elemental signature between the two media (aqueous humor and lens) and the patients themselves. Most commonly found heavy metals in both types of media were chromium and manganese. Barium was found in the lens, but not in aqueous tissue, whereas nickel was found only in the aqueous humor. Concentrations were generally higher in aqueous samples. Further study and increased sample size are required to more accurately elucidate the relationship between systemic and ocular metal accumulation and the impact of metal accumulation on measures of visual function and ocular disease.

Analytical polarized energy-dispersive X-ray fluorescence (PEDXRF) spectrometry (PEDXRFS) represents a substantial advancement over conventional XRF. The higher signal-to-noise commensurate with background lowering and better energy resolution, permits trace analysis for elements with Z ≥ 11. Concomitantly, improvements in analytical software based on the fundamental parameters (FP) approach have improved accuracies and precisions for standard-less analysis (SLA). Two ceramic and soil standard reference materials (SRMs), 98a-Plastic Clay and GSS-1 powders, differed in their intrinsic matrix properties of grain size, bulk, and surface monolayer densities as well as the elemental concentrations. The SRMs were analyzed as powder and as pellets compacted under the same pressure conditions to double the bulk density. Different geometries represented by the sample cup (10, 15, and 24 mm) and pellet (10, 15, and 25 mm) diameters with the same sample thickness (with differing masses and aspect ratios), as well as (for powder samples only) identical low masses (0.5 g) but with varying thicknesses, were analyzed. PEDXRFS combined with TURBOQUANT® (TQ) as SLA-FP enables good quantitative analysis for powders (Z ≥ 13) even for masses significantly lower than recommended, for soil–ceramic samples. Pellets (Z ≥ 12) yielded the best accuracy factor (AF) at high aspect ratio and thicknesses of the matrix analytical depth. Binder in pellets depreciates the AF. TQ needs to adequately quantitate matrix interferences effects, to improve accuracy in the analysis of low atomic numbers, e.g. Na and Mg.

A very efficient analytical method using an automated fusion machine as sample preparation tool and a wavelength-dispersive X-ray fluorescence (WDXRF) spectrometer for the determination of all the elements of interest for the iron ore industry has been optimized from the ISO 9516-1 standard method. This updated method allows for the simplification of both laboratory and spectrometry processes and so, in comparison with the original International Organization for Standardization (ISO) method, becomes less restrictive in practice. This method was used to prepare a large variety of iron ores and exploration samples from all over the world. Results of the prevailing XRF application based on pure oxide standards as described in the ISO standard method are compared to the results of a unique XRF calibration application based on certified reference materials (CRMs) for iron ores and iron ores exploration materials. The universal sample preparation fusion method for iron ores and exploration samples developed during the first phase of this project was used to select and evaluate a set of CRMs. Selected throughout the world from well-recognized sources, the chosen set of CRMs allows a wide coverage for all the elements of interest of the iron ore industry, excluding tin oxide. This fusion method allows a matrix match for materials from different origins. A critical evaluation of precision and accuracy has been performed against the ISO standard method. Reference materials not included in the calibration (control samples) was also investigated for accuracy evaluation. Furthermore, comparisons will be made between the data collected from this fusion method implemented in combination with a Bruker S4 Explorer WDXRF Spectrometer, and the analytical requirements of ISO. All deviations from the prevailing standard method parameters (calibration, standards, flux, Fluxer, etc.) will also be pointed out and discussed.

As a consequence of substantial advances in computer-aided design and manufacturing technology, engineering parts are no longer restricted to combination of simple geometrical shapes. Implementing complex curved surfaces in engineering components in combination with finite-element geometry optimization has become a prevalent means of designing a part. Measuring residual stresses using X-ray diffraction (XRD) on complex curved surfaces requires further development of current measurement methods. Here we investigate how a laboratory XRD system equipped with a five-axis stage and two-dimensional detector can execute sin2ψ residual stress measurements on curved surfaces. Shadowing that blocks the diffracted beam to reach the detector was avoided using proper rotations and tilting of the sample. A standard video-laser alignment system commonly used to manually place the sample in the center of diffraction was used to also generate virtual maps of the sample's curved surfaces on a fine mesh grid. The geometry was then used for setting the required rotations and tilt angles. A set of diffraction frames collected using this method on a model zirconia dental ceramic, afforded the opportunity to superimpose phase and stresses on a complex geometry. This is a step forward for the XRD technology, and its usefulness applies to many different industries.

The title compound 1-N-(3-pyridylmethyl)aminonaphthalene hydrochloride (C16H15N2Cl) was obtained by a reaction of α-naphthylamine (1) and N-pyridincarboxaldehyde (2) in anhydrous ethanol in the first step. The formed imine (3) was reduced with sodium borohydride in anhydrous methanol to give the product 1-N-(3-pyridylmethyl)aminonaphthalene (4). Finally, the hydrochloride was prepared by addition of a hydrochloric acid–ethyl acetate solution (ratio 1:3) with constant stirring and maintaining the temperature between 0 and 5 °C, obtaining a yellow polycrystalline solid corresponding to the respective derivative (5). The X-ray powder diffraction pattern for the new compound (5) was obtained. The compound (5) crystallizes in a monoclinic system with the space group P21/m (No. 11) and refined unit-cell parameters: a = 16.257 (8) Å, b = 9.236 (7) Å, c = 13.221 (6) Å, β = 94.87° (5), Z = 6, and V = 1978 (1) Å3.

Experimental X-ray powder diffraction data, unit-cell parameters, and space group for [C6Trop]+[PF6]−, C14H27NOPF6, are reported [a = 16.1879(6) Å, b = 11.4271(2) Å, c = 10.3966(5) Å, α = 66.4949(3)°, β = 94.5589(0)°, γ = 93.3092(4)°, unit-cell volume V = 1923.17 Å3, Z = 1, and space group P1]. No detectable impurities were observed.