The possibilities of modelling the diffraction profiles from bimodal microstructure in computer program MSTRUCT are demonstrated on two examples. A special “Double Component” profile effect can be utilized for such problems. At first it was applied to an analysis of a mixture of two nanocrystalline anatase powders with different crystallite sizes and the relative ratio of both components was determined from X-ray diffraction data. In the second case study, diffraction peaks from a pure polycrystalline copper sample treated by equal channel angular pressing were fitted using a two-phase model of large recrystallized defect-free grains and ultrafine crystallites with high dislocation density. The method is shown to be suitable for determination of the relative fraction of the microstructural components as well as other parameters (e.g. dislocation density).

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.

Two additional forms of K2FeF5 are disclosed and characterized by powder diffraction. One (form-IV) adopts a new A2MF5 structural type, space group C2/m, a = 13.0919(2) Å, b = 5.7311(1) Å, c = 7.3114(1) Å, β = 118.241(1), and Z = 4, it is obtained from the thermal evolution of form-III, isostructural with Rb2FeF5, space group Pnma, a = 7.3964(2)  Å, b = 5.6779(1) Å, c = 11.5445(3) Å, and Z = 4. Both forms are compared to two previously reported polymorphs. The III → IV transition is topotactic, conserving the same zigzag cis-connected octahedral (FeF5)n2n− chains after an ~90° rotation and 1/2b translation of half of them.

Ag–reduced graphene oxide (Ag/rGO) nanoparticle composites were synthesized through a facile one-step hydrothermal reaction using GO and silver carbonate (Ag2CO3) as raw materials. The homogeneous silver nanospheres with an average size of 50 nm well dispersed on the surface of rGO were obtained without other additives. During the formation process, GO both promotes the dispersion of Ag2CO3 in aqueous solution and acts as the substrate of silver cations, and the hydrolysis of Ag2CO3 provides silver cations and alkaline condition. Moreover, GO further serves as reducing agent to generate elemental silver in the alkaline condition. The as-prepared materials exhibit excellent surface-enhanced Raman scattering activities when used to detect the Raman signals of R6G absorbed on the Ag/rGO substrate.

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.

In the conventional X-ray reflectivity (XRR) analysis, the reflectivity is calculated based on the Parratt formalism, incorporating the effect of the interface roughness according to Nevot and Croce. However, the results of calculations of the XRR have shown strange outcomes, where interference effects increase at a rough surface because of a lack of consideration of diffuse scattering within the Parratt formalism. Therefore, we have developed a new improved formalism in which the effects of the surface and interface roughness are included correctly. In this study, for deriving a more accurate formalism of XRR, we tried to compare the measurements of surface roughness of the same sample by atomic force microscopy (AFM) and XRR. It is found that the AFM result could not be completely reproduced even with the improved XRR formalism. By careful study of the AFM results, we determined the need for an additional effective roughness term within the XRR simulation that depends on the angle of incidence of the beam.

Ongoing software developments for creating three-dimensional (3D) printed crystallographic models seamlessly from Crystallographic Information Framework (CIF) data (*.cif files) are reported. Color versus monochrome printing is briefly discussed. Recommendations are made on the basis of our preliminary printing efforts. A brief outlook on new materials for 3D printing is given.

The evolution of the 003 reflection of the layered Li(Ni,Co,Mn)O2 (CGR) and Li(Ni,Co,Al)O2 (NCR) cathodes in commercial 18650 lithium-ion batteries during charge/discharge were determined using in situ neutron powder diffraction. The 003 reflection is chosen as it is the stacking axis of the layered structure and shows the largest change during charge/discharge. The comparison between these two cathodes shows that the NCR cathode exhibits an unusual contraction near the charged state and during the potentiostatic step, where the potentiostatic step is recommended by the manufacturer. This feature is not shown to the same degree by the CGR cathode. The behavior is likely related to the compositions of these cathodes, the amount of Li/Ni site mixing and the presence of Al or Mn.

Sterilization of soils and sediments can release them from quarantine restrictions. Gamma irradiation is effective at sterilization but can damage materials and in so doing affect their suitability for environmental research. Duplicate samples of a wide range of mineral soils and sediments were subject to an acetic acid extraction before and after 50 kGy gamma irradiation. This amount of gamma irradiation did not affect the leachability of a range of analytes from the soils and sediments.

The dichlorodioxido(4,4′-dimethoxycarbonyl-2,2′-bipyridyl)molybdenum(VI) complex was prepared from molybdenum(VI) dichloride dioxide and 4,4-dimethoxycarbonyl-2,2-bipyridyl in CH2Cl2 obtaining a clear green solution. The molybdenum complex was separated by precipitation with ethyl ether. The XRPD pattern for the new compound showed that the crystalline compound belongs to the monoclinic space group P21/c (No 14) with refined unit-cell parameters a = 12.104(1) Å, b = 14.933 (2) Å, c = 11.010 (2) Å and ß = 115.409° (9). The volume of the unit cell is V = 1797.6 (3) Å3.

The importance of software continues to grow for all areas of scientific research, no less for powder diffraction. Knowing how to program a computer is a basic and useful skill for scientists. This paper explains the three approaches for programming languages and why scripting languages are preferred for non-expert programmers. The Python-scripting language is extremely efficient for science and its use by scientists is growing. Python is also one of the easiest languages to learn. The language is introduced, as well as a few of the many add-on packages available that extend its capabilities, for example, for numerical computations, scientific graphics, and graphical user interface programming. Resources for learning Python are also provided.

Commercial atomoxetine hydrochloride crystallizes in the orthorhombic space group P212121 (#19), with a = 7.362 554(12), b = 13.340 168(27), c = 16.701 887(33) Å, V = 1640.421(5) Å3, and Z = 4. The structure was solved and refined using synchrotron powder diffraction data, and Rietveld and density functional techniques. The most prominent feature of the structure is zigzag chains of N–H···Cl hydrogen bonds along the a-axis. The powder pattern has been submitted to the ICDD for inclusion in future releases of the Powder Diffraction File™.

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.

4-hydroxy-3-methoxyphenyl-4-hydroxycoumarin chalcone (C19H14O6) was synthesized by the Claisen–Schmidt reaction with the condensation of 3-acetyl-4-hydroxycoumarin with 4-hydroxy-3-methoxybenzaldehyde (vanillin). The new compound was characterized by Fourier transform infrared microscopy, UV–vis 1H, and 13C NMR spectroscopy and its crystal structure was ab initio determined from laboratory X-ray powder diffraction data. The crystal structure is monoclinic with unit-cell parameters a = 14.3181(4), b = 8.040 71(9), c = 13.5524(3), β = 100.3559(13)°, V = 1534.84(6) Å3, and space group P21/c.

The crystal structure of the novel metal organic framework (MOF) Zn(C3H5NO2S)2 is described. This MOF can serve as a model for active sites in metalloproteins, on diverse activities such as structural or catalytic functions. Each half of the amino acid act as a bidentate ligand to one Zn and as a monodentate ligand to another Zn, while the disulphide bond presents an important structural function, stabilizing the crystal packing. The structure has been obtained ab initio from synchrotron X-ray powder diffraction data. The compound crystallizes in the orthorhombic system (space group P212121), with a = 20.0906(7), b = 9.5842(3), c = 5.018 89(13), and V = 966.40(5) Å3, with Z = 4. The structure was determined using a direct space approach, by means of the Monte Carlo technique, followed by Rietveld refinement.

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.

X-ray diffraction and scattering on a single multipurpose X-ray platform have been used to probe the structure, composition, and thermal behavior of TiO2 nanoparticles ranging in size from 1 to 10 nm. Ambient and non-ambient Bragg diffraction, small-angle X-ray scattering (SAXS), as well as total scattering and pair-distribution function (PDF) analysis are combined to obtain a comprehensive picture of the samples. At these ultrasmall particle-size dimensions, SAXS and PDF prove powerful in distinguishing the salient features of the materials, in particular the size distribution of the primary particles (SAXS) and the identification of the TiO2 polymorphs (PDF). Structural features determined by X-ray scattering techniques are corroborated by high-resolution transmission electron microscopy. The elemental make-up of the materials has been measured using X-ray fluorescence spectrometry and energy-dispersive X-ray analysis.

Experimental X-ray powder diffraction data, unit-cell parameters, and space group for norethindrone, C20H26O2, are reported [a = 20.7484(12) Å, b = 12.1678(9) Å, c = 6.5561(2) Å, α = β = γ = 90°, unit-cell volume V = 1655.17(16) Å3, Z = 4 and space group P212121]. All measured lines were indexed and are consistent with the P212121 space group. No detectable impurity was observed.

Commercial dutasteride crystallizes in the orthorhombic space group P212121 (#19), with a = 7.587 44(3), b = 9.960 80(5), c = 33.500 42(12) Å, V = 2531.862(17) Å3, and Z = 4. The structure was solved and refined using synchrotron powder diffraction data, Rietveld, and density functional techniques. The most prominent feature of the structure is a zigzag chain of strong N–H···O = C hydrogen bonds along the a-axis. The powder pattern has been submitted to ICDD for inclusion in future releases of the Powder Diffraction File™.