The hydration of ordinary Portland cements (OPC) was investigated with X-ray powder diffraction (XRPD) technique, mainly using synchrotron radiation. In situ experiments were performed during the first hours of hydration to study the evolution of the crystalline phases in the system. The hydration was carried out with pure water and in the presence of additives such as superplasticizers and setting accelerating agents. As soon as water is added to the cement, ettringite crystallizes. Its evolution appears to be very complex, and lattice parameters change as a function of setting time, indicating a possible chemical evolution of ettringite with time and as a function of pH. CSH (Ca-Si-hydrate) forms after a few hours from the beginning of hydration. CSH can be indirectly quantified and its evolution studied.

The presence of strain distributions within semiconductor features influences many aspects of their behavior. For example, microelectronic technology that incorporates strained silicon improves device performance by increasing carrier mobility in the Si channels. Because current semiconductor fabrication contains multiple levels of metallic and dielectric structures, an understanding of the mechanical response of the constituent elements is critical to the prediction of the overall device performance. In addition, the interaction of strain fields between adjacent structures becomes greater as feature sizes decrease and the corresponding feature density increases. The use of synchrotron-based X-ray methods allows one to determine the interaction between strained features and their environment at a submicron resolution. Real-space mapping of strain distributions in pseudomorphically strained, raised SiGe structures revealed that elastic relaxation extends approximately 20 times the feature thickness from their edges. X-ray topographic methods were also applied to map the substrate deformation induced by overlying SiGe features. A formulation based on the classical Ewald-von Laue theory of dynamical diffraction was derived to match the measured diffraction profiles.

Calibration of powder diffraction experiments using area detectors is essential to extract high quality one-dimensional powder diffraction pattern. Precise calibration necessitates a sensible characterization of the Debye-Scherrer rings formed on the detector plane. An algorithm, designed and developed to automate this process, is described in this paper. All the parameters required for an experimental calibration are extracted using robust pattern recognition techniques. Several image preprocessing methods are employed, reducing the computational cost but retaining high signal quality. A modified version of a one-dimensional Hough transformation is used to determine the final parameters of the ellipses. After extraction, the parameters are optimized using nonlinear least squares fit. The presented algorithm is insensitive to image artefacts and was successfully applied to a large number of calibration images. The performance of the algorithm is demonstrated by the comparison of results obtained from the presented automatic calibration method and an existing manual method.

Transformation behaviors of the technologically important polycrystalline Ti50.75Ni47.75Fe1.50 shape memory alloy were investigated using differential scanning calorimeter (DSC) and powder diffraction techniques. DSC revealed that there are two-stage (i.e., cubic→trigonal→monoclinic) martensitic phase transformations on cooling and a one-step transformation (monoclinic→cubic) on heating. In situ structural refinement of cubic→trigonal→monoclinic on cooling was carried out using the D1A high-resolution neutron powder diffractometer at the Institut Laue-Langevin Neutrons for Science in Grenoble, France. Results showed that the phases involved during the phase transition are consistent with the differential scanning calorimeter cooling curve, and the refined crystal structure parameters obtained from Rietveld refinements with the generalized spherical harmonic description agreed reasonably well with X-ray single-crystal data. Subsequently, a combined neutron and synchrotron structural refinement for each phase was conducted because the trial refinements initially using only the synchrotron data of trigonal phase yielded a false minimum with a somewhat high goodness-of-fit χ2. Results obtained from the combined neutron and synchrotron data of the cubic, trigonal, and monoclinic phases show that the same minimum goodness-of-fit indices were always obtained.

Crystal structure of a new compound KBaB5O9 has been investigated from X-ray powder diffraction data. This compound is isostructural with KSrB5O9 and crystallizes in the monoclinic system with space group P21/c. Unit-cell parameters are a=6.7200(2) Å, b=8.3256(2) Å, c=14.3674(4) Å, and β=92.6103(3) deg. Its structure contains both B3O7 and B3O8 rings, which share a common B atom to form a complex two dimensional network constituting the basic B5O9 unit in the formula. Adjacent networks are bound together by Ba and K atoms, which have eight- and nine-coordinate sites, respectively. In addition, DTA and TGA curves reveal that KBaB5O9 decomposes at 798 °C. Photoluminescence (PL) characteristics of KBaB5O9:Eu3+ have been studied. The PL spectra show the strongest emission at 618 nm and the quench concentration of Eu3+ is 4 at. %.

The equation ε(φ, ψ, hkl)=Fij(φ, ψ, hkl)σij can be directly deduced from Hooke’s law. It is shown that the matrix Fij(φ, ψ, hkl) which is usually called X-ray elastic factors, behaves as a second rank tensor. Since this behaviour is the only criterion for the question of whether or not it is a tensor, the F-matrix must be regarded as a second rank tensor. This allows us to make some statements about the structure of the F-matrix on the basis of Neumann’s principle, to find relationships among F-matrices in different measurement directions, and to apply the methods and strategies for the measurement of a second rank tensor. All this is shown in a few examples. It is further shown that a consistent use of the F-matrix can replace all methods for data evaluation which makes use of linear regressions and, in addition, avoids all difficulties and disadvantages of these methods. One of these disadvantages is that the sin2 ψ-method, as well as its derivatives, is generally not correct least square fits of the measured data. This is also shown in an example. The more complicated cases with stress or constitution gradients in the range of the probed volume or stress measurement after plastic deformation are not discussed.

X-ray diffraction pattern from cotton fiber (dch32) grown in the Karnataka state of India has been recorded. Fiber was found to contain 17 Bragg reflections, of which 11 are broadened because of crystal size and intrinsic strain influences. Contributions to integrated intensities from intrinsic strain in the fiber have been estimated using line profile analysis. A molecular model was first constructed with standard bond lengths and angles using helical symmetry and layer-line spacings observed in the X-ray pattern. The model was then refined against observed X-ray data using the linked atom least squares (LALS) method. The refinement has been done with and without the intrinsic strain correction to find the extent of structural changes. These changes have been quantified in terms of bond angles, bond lengths, and torsion angles. Young’s modulus has been estimated for these fibers using the results of line profile analysis, and a broad agreement with the reported physical measurements has been obtained.

The growth temperature dependence of the InN film’s crystalline quality is reported. InN films are grown on sapphire substrates from 570 to 650 °C with low-temperature GaN buffers by metalorganic vapor phase epitaxy (MOVPE). The X-ray rocking curves and reciprocal space mappings of the symmetric reflection (0 0 0 2) and asymmetric reflection (1 0 1 2) are measured with high resolution X-ray diffraction. The results indicate that the crystallinity is sensitive to the growth temperature for MOVPE InN. At growth temperature 580 °C, highly crystalline InN film has been obtained, for which the full-width-at-half-maxima of (0 0 0 2) and (1 0 1 2) rocking curves are 24 and 28 arcmin, respectively. The crystalline quality deteriorates drastically when the growth temperature exceeds 600 °C. Combined with the carrier concentration and mobility, the approach to improve the quality of InN film by MOVPE is discussed.

A series of complex perovskite solid solutions of Ba[(Mg1−xCdx)0.33Nb0.67]O3 have been synthesized by the columbite method. Detailed Rietveld refinement of their X-ray diffraction data show that Ba[(Mg1−xCdx)0.33Nb0.67]O3 has an order trigonal structure. The ordering degree as determined by the B-site occupancies increases with the partial substitution of Cd for Mg. However, a decrease in the ordering degree in the Ba(Cd0.33Nb0.67)O3 sample is observed, which can be attributed to a relatively lower synthesis temperature. All the impurity phases are successfully identified by X-ray quantitative phase analysis. Dielectrics properties at low frequencies for all the Ba[(Mg1−xCdx)0.33Nb0.67]O3 compounds have been measured successfully.

The method of high-energy total elastic X-ray scattering to determine the atomic structure of nanocrystalline, highly disordered, and amorphous materials is presented. The current state of the technique, its potential, and limitations are discussed with two successful studies on the pressure induced phase transition in mackinawite (FeS) and the high-pressure behavior of liquid gallium.

A new structural model is proposed for cubic nitroprussides and the crystal structure for the complex salts of Fe(2+), Co(2+), and Ni(2+) refined in that model. In cubic nitroprussides the building unit, [Fe(CN)5NO]2−, and the assembling metal (M=Fe2+,Co2+,Ni2+), have ¾ occupancy with three formula units per cell (Z=3). This leads to certain structural disorder and to different local environments for the outer metal. The crystallographic results are supported by the Mössbauer and infrared data. The XRD powder patterns, index in a cubic cell (Fm3m space group), show a sinuous background because of diffuse scattering from positional disorder of the metal centers. Because of this, the crystal structures were refined allowing the metal centers to move from the (0,0,0) and (0,0,1/2) positions (away from positional symmetry restrictions). The refinement under these conditions leads to excellent agreement factors (Rwp, Rp, S), good pattern background fitting, and produced a refined structural model consistent with the crystal chemistry of nitroprussides. The studied materials are obtained as hydrates. On heating, the crystal water evolves, and below 100°C an anhydrous phase is obtained, preserving the framework of the original hydrates. The loss of the crystal water leads to cell contraction that represents around 2% of cell volume reduction. On cooling down from room temperature to 77 and 12 K, a slight expansion for the -M-N≡C-Fe-C≡N-M- chain length is observed, suggesting that at low temperature and reduction in the metals charge delocalization on the CN bridges takes place. For M=Fe and Co the crystal structure was also refined for the anhydrous phase at 12, 77, and 300 K.

A series of Dy2Co17−xGax polycrystalline samples with x from 0 to 7 were prepared by arc melting. X-ray powder diffraction analysis indicated that these compounds have the hexagonal Th2Ni17 structure for x≤3 and the rhombohedral Th2Zn17 structure for 3.5≤x≤7. The lattice parameters a and c increase linearly with the gallium content until x=5.3. With further increasing the gallium content x up to 7, the lattice parameter c slightly decreases, whereas the lattice parameter a increases more quickly than that for 0≤x≤5.3. The unit-cell volume shows an approximately linear increase of 6.1 Å3/Ga for 0≤x≤3.0 and 10.1 Å3/Ga for 3.5≤x≤7.0, respectively. Rietveld refinement of the Dy2Co11.7Ga5.3 compound reveals that the Ga atoms occupy all the 6c, 9d, 18f, and 18h sites and preferentially occupy the 6c site. The Curie temperature and the saturation magnetization of the rhombohedral Dy2Co17−xGax compounds decrease almost linearly with increasing Ga content.

In situ deformation studies of polycrystalline materials using diffraction are an established method to understand elastic and plastic deformation of materials. Studies of active deformation mechanisms, the interplay of deformation with texture, and ultimately the development of predictive capabilities for deformation modeling are an active field of research. Parameters studied by diffraction are typically lattice strains and texture evolution, which coupled with the macroscopic flow curve allow for improved understanding of the micro-mechanics of deformation. We performed a study of the uniaxial deformation of Zircaloy-2 at 2 GPa at the 13-BM-D beamline at the Advanced Photon Source. The deformation-DIA apparatus generates a confining hydrostatic pressure using a cubic anvil setup. Two differential rams allow an increase (compressive load) or decrease (tensile load) of the uniaxial straining in the vertical direction, allowing studies of plastic deformation at high pressures. In this paper, we describe how macroscopic strains, hydrostatic pressure, and uniaxial strains are derived and present some brief results.

X-ray powder diffraction technique and the Rietveld refinement method have been used successfully for the qualitative and quantitative analyses of Pingguo bauxite from Guangxi, China. Qualitative phase analysis shows that the Pingguo bauxite contains diaspore (AlOOH), hematite (Fe2O3), goethite (FeOOH), anatase (TiO2), and kaolinite (Al2(Si2O5)(OH)4). Quantitative Rietveld refinement shows that the weight concentrations of diaspore, goethite, hematite, anatase, and kaolinite for the Pingguo bauxite are 71.9(4)%, 7.0(8)%, 11.3(7)%, 6.5(6)%, and 3.3(9)%, respectively.

A polycrystalline sample of YbCoO3 was prepared using a water-soluble complex method at relatively low temperatures. Common chelating ligands such as citric acid were employed for the synthesis of complex-based precursors, followed by thermal decomposition of the precursors at high temperatures. X-ray diffraction data were collected and the crystal structure was refined by the Rietveld method. The structure of YbCoO3 can be described as a sesquioxide C-M2O3-like structure with space group Ia-3 and unit-cell parameter a=10.4470 (2). The Yb3+ and the Co3+ cations are found to preferentially occupy the two nonequivalent 8d and 24d sites, respectively. The two independent atoms Yb/Co have octahedral coordination; however, the degrees of distortion of their coordination polyhedron are different. The relationship between the title compound and the orthorhombic Perovskite structure of YbCoO3 reported in the literature is established.

Crystal structures of (NH4)2KWO3F3 at 298 K and 113 K were solved from X-ray powder diffraction data and refined by the Rietveld technique. The compound is isostructural with elpasolite K2NaAlF6 at room temperature with space group Fm-3m, a=8.95850(5) Å, V=718.961(7) Å3, Z=4, Dx=3.363 g/cm3, and MW=364.02. The structure was refined over 18 parameters to Rwp=12.6%, Rp=10.9%, Rexp=5.03%, and RB=3.27% from 40 independent reflections. (NH4)2KWO3F3 was transformed upon cooling to a ferroelastic monoclinic phase with space group P21/n, a′=6.3072(3) Å, b′=6.3028(3) Å, c′=8.9882(3) Å, β′=90.242(2)°, V=357.30(3) Å3, Z=2, and Dx=3.383 g/cm3. The low-temperature structure at 113 K was refined over 28 parameters to Rwp=20.9%, Rp=21.3%, Rexp=12.5%, and RB=6.93% from 453 independent reflections.