The present paper is about the estimation of lattice deformation from data collected from manufactures directly on site. The aim here is to give evidence that the concept of the Mean Equivalent Lattice (MEL), when applied to “on site X-Ray Diffraction” is the basis for a reliable qualification of the material rheology to external solicitations. Such method allows for the identification of lattice deformations without resorting to the computation of the residual stress with using the elasticity constants (i.e. tensile, shear and rigidity constants E, μ, ν); these elasticity constants descend from the classical theory of solid mechanics, where the continuum mechanics and the material isotropic model are the fundaments. Any MEL deformation is instead related to the variation of the d-spacing among lattice planes which are connected to the anisotropic atomic arrangement. So the macroscopic scale is constituted by a number of MELs and related boundaries. The recent on site X-ray diffraction technology may offer effective and easy solutions, with a significant impact on reliability of results, simplification, economy and time consuming.

A variable frequency ferroelectric polarisation measurement system has been designed and built at the UK's Diamond Light Source. The electric field induced phase transitions in Pb(Zr1−xTix)O3 (PZT) have been used to test the facility via in-situ measurements of electric polarisation and XRD. Stroboscopic and real time data collection methods on polycrystalline samples were employed as a function of frequency to determine the dynamic ferroelectric response. The system has been shown to deliver XRD patterns of good statistical quality measured over 40 points of a ferroelectric PE loop. The system is now available on station I11 as a user facility at the Diamond Light Source.

The growth kinetics of Cu2ZnSnS4 thin films and powders was studied using in-situ synchrotron data. Isothermal and isochronal measurements were performed at the MCX beamline of the Elettra synchrotron (Trieste, Italy). Diffraction line profile analysis was used to follow the changes in the domain size distribution during isothermal measurements, and the change in the mean volume of the domains was studied using the Johnson-Mehl-Avrami equation. The growth was found to be diffusion controlled from small dimensions while the nucleation rate is temperature dependent. An activation energy of 210 kJ/mol could be estimated. In case of the isochronal data, the evolution of inverse of the integral breadth of the diffraction peaks in dependence on temperature was studied using the Ozawa and Šatava equations. The activation energy determined for the growth process is between 112(2) and 145(5) kJ/mol.

In order to investigate the hydrogenation of intermetallic compounds, a gas pressure cell for in situ neutron powder diffraction based on a sapphire crystal tube was constructed. By proper orientation of the single crystal Bragg peaks of the container material can be avoided, resulting in a very low diffraction background. Using a laser heating and gas pressure controller, the hydrogenation (deuteration) of palladium and palladium rich intermetallics was studied in real time up to 8 MPa gas pressure and 700 K. Crystal structure parameters of palladium deuterides could be obtained under various deuterium gas pressures, corresponding to compositional ranges of 0.04≤x≤0.11 for the α-phase and 0.52≤x≤0.72 for the β-phase at 446 K. In situ neutron powder diffraction of the deuteration of a thallium lead palladium intermetallic Tl1-xPbxPd3 shows two superstructures of the cubic closest packing (ccp) to transform independently into a AuCu3 type structure. This proves a direct reaction to the deuterium filled AuCu3 type structure instead of a reaction cascade involving different ccp superstructures and thus gives new insights into the reaction pathways of palladium rich intermetallic compounds.

A time-resolved powder diffraction study of the crystallisation of porous metal organic framework materials with the CPO-27 structure ([M2(dhtp)(H2O)2]·8H2O where, dhtp=2,5-dioxoterephthalate) using the energy dispersive X-ray diffraction method is described. Crystallisation under solvothermal conditions is performed between 70 - 110 °C from clear solutions of metal salts (M=Co2+ or Ni2+) and 2,5-dihydroxyterephthalic acid in a mixture of THF-water in sealed reaction vessels, using both conventional and microwave heating. Integration of Bragg peak areas with time provides accurate crystallisation curves, which are modelled using the method of Gualtieri to determine rate constants for nucleation and for growth and then, by Arrhenius analysis, activation energies. Crystallisation is determined to be one-dimensional, consistent with the elongated morphology of the crystals produced in these reactions. With conventional heating the Co-containing CPO-27 crystallises more rapidly than the isostructural Ni-containing analogue and analysis of the kinetic parameters would suggest a complex multi-step crystallisation process. The effect of microwave heating is upon activation energies: the values for both nucleation and for crystal growth are lowered compared to reactions using conventional heating.

Neutron diffraction (ND) was used to investigate the crystallographic preferential orientation (CPO, texture) and structure parameters of four samples of metagabro mylonite collected from the eastern part of the metagabbro sheet at the Stare Mesto belt, Bohemia Massif, Czech Republic. The samples were selected to form a deformation-ordered series with the microstructure varying from non-deformed metagabbro protolith to strongly sheared ultramylonite and amphibole-rich ulramylonite. The specimens used in ND measurements were polished in form of an exact sphere with diameter 50 ± 0.1 mm. The obtained ND patterns were corrected for non-linear background and then evaluated using the Rietveld method implemented in the software package GSAS. Data recorded from powder preparded by milling material from the sampled rocks were used to refine the structure parameters of plagioclase (labradorite structure, triclinic space group C-1) and amphibole (monoclinic space group C2/m). The experiments were performed on the KSN-2 neutron diffractometer situated at the research reactor LVR-15 of the Nuclear Research Institute, plc. Rez, Czech Republic. The data sets of ND patterns measured on each of the four spherical specimens consisted of 90 diagrams collected for different diffraction vectors covering uniformly one orientation hemisphere of the specimen. Based on the collected data, the orientation distribution function (ODF) of crystalline grains was determined by Rietveld harmonic method (coefficients C(l,m,n) of the spherical harmonics expansion determined up to the order L = 8) for the two principal mineral phases - amphibole and plagioclase. The ODF was used to reconstruct (001), (020), (021), (110), (111) (plagioclase) and (001), (11-1), (020), (110), (200) (amphibole) pole figures (PFs). Direct method of ODF calculation implemented in ResMat software package was then used to calculate inverted pole figures (IPFs) of the plagioclase phase. CPO of the amphibole and plagioclase is then discussed in terms of the obtained texture indices and calculated PFs and IPFs and compared with data measured by other methods or available in literature.

This work aims to investigate the hydration behavior and structural properties of two dioctahedral smectites with contrasting location charge (beidellite SbId-1 and montmorillonite SWy-2) according to the nature of the bivalent compensator heavy metal cations (i.e. Hg (II), Ni (II), Ba (II) and Mg (II)). This study is achieved using XRD profile modeling approach based on the simulation of the 00l reflection which allowed us to determine structural characteristics along the c* axis related to the nature, abundance, size, position and organization of exchangeable cation and water molecule in the interlamellar space along the c* axis. The obtained results show that a heterogeneous hydration behavior is systematically observed in all studied samples and the structural models, used to fit samples with tetrahedral charge, are more heterogeneous than smectite with an octahedral sheets substitution. In the case of exchanged beidellite specimen, the proposed models are described by a mixed layer structure with variable abundance containing respectively, dehydrated (0W), mono-hydrated (1W) and bihydrated (2W) layers. Whereas, in the case of the montmorillonite, the absence of 0W hydration state is noted.

To gain accuracy and, hence, physical reality of the data acquired by XRD measurements of fibre textures, a technique is elaborated to achieve experimental values, which are free of extinction effects. Its elaboration is based on combining basic definitions of the extinction theory and texture analysis. This technique is applicable to characterization of metal coatings that appear infinitely thick for X-rays. A nickel sample representing <100> + <221> texture components is used as a model. Resultant derived series of data on pole-density distribution of the {200} diffraction pole figure shows that the data corresponding to the main <100> texture component are strongly affected by extinction. On the contrary, due to definitions that require reduction of the intensity distribution to multiples of random density, the extinction-free values of the volume fraction of texture components do not differ substantially from those calculated by standard methods. Evidently, any of the standard methods for volume fraction measurements provides reasonable data if secondary extinction is even disregarded.

In present investigation, effect of modulation and machining parameters on deformation level of the chips produced during modulation assisted machining (MAM) has been studied. It is shown that disruption in tool-chip contact during modulation assisted machining helps in the formation of discrete chips. Size and shape of the particles produced in MAM can be controlled by varying modulation and machining conditions. Particulates of different shapes and sizes ranging from 100 µm to 5 mm with an aspect ratio of ~10 were produced using MAM. The morphology of the particulates produced was characterized by scanning electron microscope (SEM). Deformation in chip particulates was investigated using X-Ray diffraction. The crystallite size and internal strain in particulates were evaluated using Scherrer and Williamson-Hall methods respectively. The crystallite size of the particulates was found to decrease with decrease in their size, whereas internal strain in particulates was observed to increase with decrease in their size. Furthermore, the length of particulates was observed to decrease with an increase in the ratio of frequency of modulation (fm) to frequency of workpiece rotation (fw). However, the corresponding change in microstrain and crystallite size was insignificant with change in this ratio.

Linear Friction Welding (LFW) has tremendous potential for joining components from similar and dissimilar materials, avoiding material melting and introducing minimal distortion and only moderate levels of residual stress. However, the significant amount of attendant shear introduces preferred crystal orientations that have not yet been well studied. The “one-shot” approach to the interpretation of multi-element energy-dispersive X-ray powder diffraction data allows preferred orientation analysis without any sample preparation (cutting or polishing) or sample rotation. The key step for texture analysis by X-ray powder diffraction is the derivation of the orientation distribution function (ODF) from experimental data. Matlab toolbox “MTEX” provides a powerful function “calcODF” based on the harmonics method for this purpose. In the study reported in this paper, energy dispersive X-ray diffraction patterns were collected using the “horseshoe” multi-element energy-dispersive Ge detector installed on the JEEP beamline at Diamond Light Source. A single exposure was used for each gauge volume of interest, and a line was scanned across an Aluminum 2024 alloy LFW sample. The patterns were converted into raw pole figures through single peak fitting and equal area projection. The ODF calculation was performed based on these pole figures using Matlab toolbox “MTEX”. As a result, full pole figures obtained after ODF calculation were obtained. These are presented and discussed. The results show that the thermal-mechanical processes that occur during the LFW process lead to significant modification of the orientation distribution, but cause only moderate changes in the texture index.

The Sr analogue of the mineral fresnoite (Sr2TiSi2O8) is of interest as a potential storage medium for radioactive Sr from nuclear waste. No high or low temperature crystal structure information is known on this phase. Therefore high-resolution synchrotron X-ray powder diffraction measurements have been done on a synthetic sample of Sr-fresnoite in the temperature range 87-1223K. This was done as a test experiment using the HRPD beamline P02.1 at PETRA-III, DESY. Synchrotron X-ray wavelengths of 0.2067(3)Å (293K and 573-1223K) and 0.2079(3)Å (87-499K) were used. Powder diffraction data were collected with a counting time of 30s using a PerkinElmer XRD 1621 flat panel image plate detector. CeO2 was included as an internal standard to calibrate the sample to detector distance. The P4bm tetragonal crystal structure of fresnoite (Ba2TiSi2O8) was used as a starting model for Sr-fresnoite. Small amounts of SrTiO3 and SrSiO3 were also found as impurities in this sample; therefore four-phase Rietveld refinements were done. The P4bm fresnoite structure is retained over the temperature range 87-1223K.

PyFAI is an open-source Python library for Fast Azimuthal Integration which provides 1D- and 2D-azimuthal regrouping with a clean programming interface and tools for calibration. The library is suitable for interactive use in Python. In optimising the speed of the algorithms there has been no compromise on the accuracy compared to reference software. Fast integrations are obtained by the combination of an algorithm ensuring that each pixel from the detector provides a direct contribution to the final diffraction pattern and an OpenCL implementation that can use graphics cards for acceleration. This contribution describes how the algorithms were modified to work better in parallel.

Recent results of focusing and reflectivity properties of the dispersive double-bent-crystal monochromator have shown that it could be succesfully used in high resolution neutron diffraction experiment. By using a standard polycrystalline sample of α-Fe, the resolution of the diffraction performance in the vicinity of the scattering angle 2θS = 90o for the neutron wavelength λ= 0.162 nm was tested in detail. It has been found that for thin (1.3 mm) bent second crystal the angular resolution represented by FWHM of diffraction profiles was 1x10−3 rad for 211 and 200 reflections and about 3x10−3 rad for 220 reflection.

The current report describes the installation and the preliminary commissioning of the Material Science Powder Diffraction (MSPD) beamline at the Spanish synchrotron ALBA-CELLS. The beamline is fully dedicated to powder diffraction techniques and consists of two experimental stations positioned in series: a High Pressure/Microdiffraction station and a High Resolution/High Throughput powder diffraction station.