The evolution of internal stresses in oxide scales growing on polycrystalline Fe3Al alloy in atmospheric air at 700 °C was determined using in situ energy-dispersive synchrotron X-ray diffraction. Ex situ texture analyses were performed after 5 h of oxidation at 700 °C. Under these conditions, the oxide-scale thickness, as determined by X-ray photoelectron spectroscopy, lies between 80 and 100 nm. The main phase present in the oxide scales is α-Al2O3, with minor quantities of metastable θ-Al2O3 detected in the first minutes of oxidation, as well as α-Fe2O3. α-Al2O3 grows with a weak (0001) fiber texture in the normal direction. During the initial stages of oxidation the scale develops, increasing levels of compressive stresses which later evolve to a steady state condition situated around −300 MPa.

Laboratory X-ray powder diffraction was used to investigate mineralogical compositions of green pigments labeled by suppliers as “green earths.” It was found that glauconite and celadonite—minerals historically considered as the main ingredient of this pigment—were present only in Bohemian green earth, green earth from Thuringen (glauconite), and Bavarian green earth (celadonite). Other investigated pigments consist of mineralogical-component minerals with added synthetic organic colorants. The obtained results may be useful for scientists, restorers, and artists in proper choices of the pigments they use in their works.

In this work synchrotron radiation X-ray diffraction technique was successfully applied for the analysis of pigments found in excavation at Carriqueo rock shelter, Neuquén, Argentina. The pigment samples of orange, red, and brown shades were collected from different levels of this archaeological site and compared with a suspected source of provenance (La Oficina creek). X-ray diffraction patterns of several yellowish, reddish, and red pigments showed the presence of haematite, goethite, kaolinite, and quartz. The majority of Carriqueo collected samples belonged to the same group of the suspected source, having haematite and quartz as main crystalline phases. The results indicate that the raw material from La Oficina is the source of most of the pigments found at Carriqueo. The present work helps us to understand the strategy of supplying raw materials by human groups in the North Patagonia region.

Four new compounds with general formula CdI2-2(NH2-PhX) (Ph represents phenyl radical; X represents Cl or H atoms) were obtained and characterized. Two of them, bisaniline diiodidecadmium(II) — CdI2⋅2[NH2–C6H5] {1} and bis(2-chloroaniline) diiodidecadmium(II) — CdI2⋅2[NH2–C6H4Cl] {2}, crystallize in monoclinic system, whereas another two, bis(3-chloroaniline) diiodidecadmium(II) — CdI2⋅2[NH2–C6H4Cl]{3} and bis(4-chloroaniline) diiodidecadmium(II) hemi(4-chloroanilate) — CdI2⋅2[NH2–C6H4Cl]½[NH2–C6H4Cl] {4}, crystallize in triclinic system. The investigated compounds, from chemical point of view, are similar to the so-called cisplatin—a compound used as a chemotherapy drug to treat many types of cancers. Their syntheses and results of X-ray powder diffraction studies at room and elevated temperatures are described in this paper.

The structural and magnetic properties of the DyCo4−xFexGa compounds with x=0, 0.5, 1, and 1.5 have been investigated by X-ray diffraction and magnetic measurements. Powder X-ray diffraction analysis reveals that each of the DyCo4−xFexGa compounds has a hexagonal CaCu5-type structure (space group P6/mmm). The Fe solubility limit in DyCo4−xFexGa is x<1.5. The higher the value of x, the larger the unit-cell parameters a, c, V, and the 3d-sublattice moment but the smaller the 3d uniaxial anisotropy. Magnetic measurements show that the Curie temperature of DyCo4−xFexGa increases from 498 K for x=0 to 530 K for x=1.5, the compensation temperature Tcomp decreases from 286 K for x=0 to 238 K for x=1.5, and the spin-reorientation transition temperature increases from 403 K for x=0 to 530 K for x=0.5. No spin-reorientation transition was found in the samples with x=1.0 and 1.5. The saturation magnetization of DyCo4−xFexGa measured at 173 K increases but the magnetization measured at 300 K decreases with increasing Fe content x.

X-ray powder diffraction data, unit-cell parameters, and space group for a novel platinum-based anticancer complex cis-[diiodo(1R,2R)-1,2-diaminocyclo-hexane-κN,κN′] platinum(II), Pt(C6H14N2)I2, are presented [a=14.048(4) Å, b=7.588(3) Å, c=11.502(4) Å, β=98.446(5)°, space group C2, cell volume=1212.80 Å3, and Z=4]. All measured lines were indexed and are consistent with the C2 space group. No detectable impurities were observed.

Al–2.5% Mg alloy exhibits the Portevin–Le Chatelier (PLC) effect at room temperature for a wide range of strain rates. Tensile test has been carried out on a flat Al–2.5% Mg alloy sample at a strain rate of 3.7×10−6 s−1. The strain rate was chosen so that the type C PLC band appears in the sample. X-ray diffraction profile has been recorded from the gauge length portion of the deformed sample to investigate the microstructure of the PLC band. Analysis revealed that the dislocation density is much higher within the band compared to the undeformed sample even at small strain. The PLC band in this alloy possesses an equal fraction of screw and edge dislocations.

Strain field distribution in a naval platform under dry-dock conditions is complex and represents the cumulative response from residual stress (“locked in” during fabrication of materials and formation of the structure) and static loading stress (e.g., dry-dock loading). The magnitude and distribution of stress fields are a significant concern for the Canadian Navy, where the superposition of applied stresses on residual stresses may adversely affect the performance, safe operational envelope, and service life of naval platforms. Stress analysis was conducted on Canada’s VICTORIA Class submarines using a portable miniature X-ray diffractometer (mXRD) under dry-dock conditions. This paper introduces the concept of “residential stress” as it applies to submarine platforms and discusses the methodology for performing stress analysis with a portable mXRD. The evolution of residential stress during routine pressure hull repairs to Canada’s VICTORIA Class submarines is discussed. In particular, the recent replacement of the diesel exhaust hull and back-up valves on one of the submarines, as well as a pressure hull plate extraction-insertion-weld procedure on another, is discussed.

Transparent p-type conducting Ga-doped SnO2 thin films were prepared using reactive rf-magnetron sputtering. Good p-type conduction was directly realized without the need of postdeposition annealing. The p-type conductivity was found to be very sensitive to the growth condition and process, suggesting that the carrier behavior is strongly related to the fine microstructure of the films. The microstructures of the films were characterized using synchrotron X-ray diffraction and specular reflectivity techniques. The valence state of the Ga dopant was measured from X-ray photoelectron spectra to explain the origin of net holes presented in the films.

CaMnO3 is a parent compound for numerous multicomponent manganese perovskite oxides. Its crystallographic data are of primary importance in the science and technology of functional CaMnO3-based materials. In the present study, data were collected for a CaMnO3 sample at 302 K. The crystal structure refinement yields accurate absolute values of lattice parameters, a=5.281 59(4) Å, b=7.457 30(4) Å, and c=5.267 48(4) Å, leading to orthorhombic distortion of (c/a, √2c/b)=(0.997 33,0.998 95). The orthorhombic distortion of the CaMnO3 structure is discussed on the basis of comparison of our unit-cell size with data already published. At a graphical representation of the distortion, it is observed that there is a considerable scatter of the distortion values among the literature data but, interestingly, a considerable fraction of experimental results (including the present one) for stoichiometric samples are grouped around the distortion (c/a, √2c/b)=(0.9973,0.9990), which lies close to a maximum in the extent of orthorhombicity. The influence of off-stoichiometry on the orthorhombic distortion is discussed on the basis of available experimental data. Simulations, employing a mean-field approach for low temperatures, predict an increase in cell volume and structural distortions with the concentration of oxygen vacancies when the additional electrons are localized on the manganese. A simple model of delocalization produced the opposite effect, which is expected to combine with lattice vibrations to recover the cubic phase at high temperatures.

New XRD total pattern fitting software MSTRUCT was used to study the microstructure of magnetron-deposited TiO2 thin films. MSTRUCT is an extension of the FOX program for structure determination from powder diffraction data. MSTRUCT makes corrections for refraction and absorption, residual stress, and preferred orientation that are necessary for thin-film analysis using the parallel-beam geometry and an asymmetric detector scan with small angles of incidence. The program also corrects for crystallite size broadening in terms of log-normal distribution, two models of strain (phenomenological and dislocation models), as well as the influence of stacking faults in the most common cubic and hexagonal structures. The microstructure results obtained by this study show that during crystallization of the amorphous TiO2 films, tensile stresses were generated resulting in anisotropic shifts of diffraction peaks. This was confirmed by in situ crystallization and direct stress measurements. The consideration of the stress effect in terms of the weighted Reuss-Voigt model improved the fits significantly. The stresses were found to depend systematically on the TiO2 film thickness, and their values determined by total pattern fitting agree well with the values measured directly by XRD stress analysis.

The ICDD sponsored a round robin on the quantitative Rietveld phase analysis of pharmaceuticals. 11 participating laboratories from the pharmaceutical community submitted both raw data and processed quantitative results. The purpose of the round robin was to evaluate current practices in laboratories, so procedures and methods were not specified, but they were recorded. Cluster analysis tools were applied to all the data sets and their use helped identify the root causes of several types of errors in specimen preparation, data treatment, and Rietveld analysis. The authors considered this round robin to be difficult. Sample homogeneity was an issue and molecular orientation was observed in many data sets. Each material studied has structural polymorphs so the selection of starting parameters and their refinement was nontrivial. Similar to prior round robins on inorganic materials and minerals, this round robin identified operator errors as the major contributor to poor results. Four laboratories achieved excellent results on all phases in all three samples, with accuracy within relative errors of 5% to 10%.

A new nickel zinc chromate with the composition of (NH4OH)3/2NiZn2Cr2O9⋅2H2O was synthesized by hydrothermal method. The compound was characterized by XRD, TGA, and XRF. X-ray powder diffraction data show that the crystal system of the title compound is hexagonal with space group R-3m, z=3, and unit-cell parameters: a=5.9794 and c=21.4875 Å.

A new classification of opals through X-ray powder diffraction (XRPD) methodology, by analysing 75 new samples of opal came from different worldwide areas, is introduced. A brief historical summary of the application of XRPD analysis on opals and the most important XRPD results reported in literature were compared with the newly obtained XRPD data. A simple method for the classification of opals on the basis of their degrees of structural order-disorder calculated from the diffraction data is proposed. In addition, a clear boundary, which has not been previously described by others in literature, related to the presence (or absence) of two-peak characteristic of the cristobalite phase is identified. This boundary allows for a discrimination of opals C from CT.

Mixed solvent of ethanol and water using FeSO4⋅7H2O and (NH2)2CS as precursors with polyvinylpyrrolidone as surfactant was used to synthesize cubic FeS2 (pyrite) crystals. Crystalline phase and surface morphologies of the crystals were characterized by X-ray diffraction and scanning electron microscopy, respectively. Volume ratio of solvent, reaction temperature, reaction time, and sulfur source were found to be the key parameters for the formation of pure pyrite crystals. Optimal micron-size pyrite crystals were successfully grown from a mixed solvent of ethanol and water with a volume ratio of 3:2, heated to a reaction temperature of 180 °C, and maintained for 36 h with thiourea as the sulfur source.

A useful procedure is described to rapidly obtain Bragg-reflection intensities from the FULLPROF suite, and the Bragg intensities can then be input into the GEST and the PECKCRYST programs for crystal-structure determination of small molecules. An example on using the new procedure for the structure determination from powder diffraction determination of hydrochlorothiazide (C7H8ClN3O4S2) is presented, and the powder-structure results obtained by the PECKCRYST program are in good agreement with previously reported single-crystal results.

The increasing use of microanalysis techniques to analyze particles has demanded more rapid phase identification methods for samples in the 10 μm size range. The XRD analysis of such particles is routinely accomplished using a Rigaku combination instrument combined with particle handling methods. Several case studies show the variety of material analysis problems that can be solved with this technique including identification of multiple mineral phases, corrosion components, and paint samples.

A 2-2-type nanostructure bilayer film of CoFe2O4/Pb(Zr0.52Ti0.48)O3 was successfully prepared on the (111)Pt/Ti/SiO2/Si substrate. The Pb(Zr0.52Ti0.48)O3 layer in the bilayer film is (111) oriented and is a mixture of tetragonal and monoclinic phases. The results from an in situ X-ray diffraction analysis of the multiferroic bilayer film under statistic magnetic field indicate that the monoclinic-tetragonal phase transition was induced by magnetostriction of the CoFe2O4 layer. A large magnetoelectric effect was obtained probably because of the different polarization directions of the tetragonal and monoclinic phases.

Verification tests of the forward modeling technique for near-field high energy X-ray diffraction microscopy are conducted using two simulated microstructures containing uniformly distributed orientations. Comparison between the simulated and reconstructed microstructures is examined with consideration to both crystallographic orientation and spatial geometric accuracy. To probe the dependence of results on experimental parameters, simulated data sets use two different detector configurations and different simulated experimental protocols; in each case, the parameters mimic the experimental geometry used at Advanced Photon Source beamline 1-ID. Results indicate that element orientations are distinguishable to less than 0.1°, while spatial geometric accuracy is limited by the detector resolution.

One of the advantages of a multidetector neutron time-of-flight diffractometer such as the high pressure preferred orientation diffractometer (HIPPO) at the Los Alamos Neutron Science Center is the capability to measure efficiently preferred orientation of bulk materials. A routine experimental method for measurements, both at ambient conditions, as well as high or low temperatures, has been established. However, only recently has the complex data analysis been streamlined to make it straightforward for a noninitiated user. Here, we describe the Rietveld texture analysis of HIPPO data with the computer code Materials Analysis Using Diffraction (MAUD) as a step-by-step procedure and illustrate it with a metamorphic quartz rock. Postprocessing of the results is described and neutron diffraction results are compared with electron backscatter diffraction measurements on the same sample.