X-ray powder diffraction data for the trigonal form of disilver trihydrogen paraperiodate, Ag2H3IO6, are reported. The cell parameters are a=5.941 89(3), c=12.7253(1) Å, V=389.089(6) Å3, and ρ=5.65 g cm−3 for Z=3. A full-profile Rietveld refinement confirms the monophasic nature of the sample and the presence of two-dimensional corrugated layers of the A2BO6 type linked by hydrogen bonds. Short unsupported Ag–Ag contacts (about 3.02 Å) of the argentophilic type are also shown.

The incommensurately modulated structure of Bi2Sr2Eu1.3Ce0.7Cu2O10.17, with a = 5.4752(4) Å, b = 5.4522(3) Å, c = 17.860(1) Å, Z = 2, was refined by the GJANA program [Gao et al., Acta Cryst. A 49, 141 (1993)] from X-ray powder data in C:C2mb: 111 four-dimensional space group (Rov = 0.064, Rm = 0.041, Rsat = 0.202, Rp = 0.049, Rwp = 0.065). Displacive modulation parameters of all cations and oxygen atoms in the Bi-layer were involved in the refinement. Obtained results including the modulation parameters are in agreement with those found for the similar phase Bi2Sr1.7Nd1.8Ce0.5Cu2O10+δ from single-crystal data [Mironov et al., J. Solid State Chem. 109, 74 (1994)].

X-ray powder diffraction data for the orthorhombic natural amino acid djenkolic acid, C7H14N2O4S2, is described in this paper. The orthorhombic cell parameters are: a=8.12 Å, b=12.16 Å, and c=5.38 Å

X-ray diffraction and neutron spectra present a peak assembly whose maxima are centered at angles corresponding to Bragg's law.

Analysis of diffracted intensity profiles in each peak can be used to estimate such morphologic characteristics of the samples as preferred orientation (Brindley and Kurtosy, 1961; Martin, 1966); crystallite sizes (Scherrer, 1919; Warren and Averbach, 1950; Wilson, 1962; and Guérin et al., 1986); and crystal shapes (Wilson, 1949). Such analysis can also be used to estimate the determination of residual stress and lattice defects (Warren and Averbach, 1950; Wilson, 1963). In such studies, a detailed analysis of the diffraction distribution is required and consequently adjustment of intensity values must be carried out, as they are affected by systematic errors in the measuring apparatus (for detailed description, see Klug and Alexander, 1974 and Wilson 1967).

The transition between tetragonal and cubic phases in nanostructured ZrO2-Sc2O3 solid solutions by high-temperature X-ray powder diffraction using synchrotron radiation is presented. ZrO2-8 and 11 mol% Sc2O3 nanopowders that exhibit the t′- and t″-forms of the tetragonal phase, respectively, were synthesized by a stoichiometric nitrate-lysine gel-combustion route. The average crystallite size treated at 900°C was about 25 nm for both compositions. Our results showed that t′-t″ and t″-cubic transitions take place for the 8 and 11 mol% Sc2O3 samples, respectively.

Slags sourced from a derelict zinc–lead–copper–silver–tungsten mine were examined for their bulk elemental composition and mineralogy. pH, oxidation–reduction potential, and the leachability of selected elements (sulphur, calcium, iron, copper, zinc, and lead) were assessed during a 130-day deionised water extraction conducted under oxic conditions. Slags were rich in silicon, iron, copper, zinc, and lead, hosted within minerals including quartz (SiO2), goethite [FeO(OH)], augite [Ca(Mg,AI,Fe)Si2O6], and lead (Pb0). Leachates from the slags increased in analyte concentration throughout the 130-day experiment, with iron, copper, zinc, and lead attaining >5 mg l−1 in some samples. These findings indicate that this pyrometallurgical waste should not be considered environmentally inert, as leachates emanating from them in the field might pose a significant risk to the environment.

Synchrotron-based X-ray microbeam measurements were performed on silicon-on-insulator (SOI) features strained by adjacent shallow-trench isolation (STI). Strain engineering in microelectronic technology represents an important aspect of the enhancement in complementary metal-oxide semiconductor device performance. Because of the complexity of the composite geometry associated with microelectronic circuitry, characterization of the strained Si devices at a submicron resolution is necessary to verify the expected strain distributions. The interaction region of the SOI strain extended the SOI film thickness from the STI edge at least 25 times. Regions of 65-nm-thick SOI less than 3 μm wide exhibited an overlap in the strain fields because of the surrounding STI. Microbeam mapping of arrays containing submicron SOI features and embedded STI structures revealed the largest out-of-plane strains because of the close proximity of superimposed strain distributions induced by the STI.

The silver (Ag) powder was synthesized in a mechanochemical (MC) process by inducing a solid-state displacement reaction between silver chloride (AgCl) and copper (Cu). This process was carried out in argon atmosphere conditions using a planetary ball mill. The reaction caused the mixture of AgCl and Cu to change the composition of the mixture to Ag and copper chloride (CuCl). CuCl was separated from MC product by leaching with ammonium hydroxide. Thus, Ag powder was obtained as the final product. Stearic acid (C18H36O2) was used as the additive to improve dispersion of Ag powder during the MC process. The ground powders, formed in the presence and absence of additive, were characterized by X-ray diffraction (XRD) and scanning electron microscope (SEM). The XRD determined that the reaction between AgCl and Cu was completed in 18 h milling. SEM and particle size analysis examinations revealed that the size of the particles in the synthesized metallic Ag powder was in the range of 30–300 nm.

Calcium sodium iminodisulphonate trihydrate was first described by Divers and Haga [J. Chem. Soc. 943–968, (1892)]. It has recently been found as one of several crystalline products resulting from the removal of sulphur dioxide from flue gas. It has not so far been included in the ICCD powder diffraction file.

A combination of neutron diffraction, synchrotron X-ray diffraction, and high-resolution extended X-ray absorption fine structure measurements has been used to clarify the correlations between long- and local-range structural distortions across the spin-state transition in powders of LaCoO3 and La0.5Sr0.5Co0.75Nb0.25O3. The analysis of the diffraction data has revealed that the isotropic thermal parameters of Co–O bond abnormally increase below 100 K in both samples, while the temperature dependence of the average Co–O bond lengths is linear from 10 to 300 K. We also have found that the Co–O bond lengths are larger in La0.5Sr0.5Co0.75Nb0.25O3, as compared with the ones in LaCoO3. The X-ray absorption data showed an anomalous decrease of the Co–O bond lengths only for LaCoO3, in contrast to the bond length values obtained by diffraction. The structural anomalies observed by spectroscopy measurements are discussed in terms of the spin-state transition model.

The structure of the new Y0.8Ca0.2Ba1.8La0.2Cu3Oy (YBLCO) compound was obtained at 298 K from X-ray powder diffraction data and refined by the Rietveld technique. YBLCO has a structure isotypical with YBa2Cu3Oy (YBCO) at room temperature. The crystal data are: Y0.81Ca0.19Ba1.8La0.2Cu3O7.08, Mw=657.69, orthorhombic system, space group Pmmm, a=3.8731(1) Å, b=3.8249(1) Å, c=11.6602(3) Å, V=172.740(13) Å3, Z=1, dx=6.325 g/cm3; the structure was refined with 37 parameters to Rwp=7.66%, Rp=5.86%, and Rexp=5.11% for 2001 data points. Moreover, the proportions of Ca and La were refined to be 0.19 and 0.2, in agreement with the stoichiometric proportion of 0.2.

The structure of a chemical-vapor-deposited (CVD) diamond thin film on a Mo substrate was studied using quasi-parallel X-ray and glancing incidence techniques. Conventional X-ray diffraction analysis revealed that the sample consists of a diamond thin film, a Mo2C transition layer, and Mo substrate. The Mo2C transition layer was formed by a chemical reaction between the diamond film and the Mo substrate during the CVD process. A method for layer-thickness determination of the thin film and the transition layer was developed. This method was based on a relationship between X-ray diffraction intensities from the transition layer or its substrate and a function of grazing incidence angles. Results of glancing incidence X-ray diffraction analysis showed that thicknesses of the diamond thin film and the Mo2C transition layer were determined successfully with high precision.

Activation energies for the intermixing reaction of textured metal-metal multilayer thin films have been determined using X-ray diffraction analysis. Kinetic data were collected utilizing an area detector so as to reduce intensity bias from changes in out-of-plane texture during the intermixing reaction. Activation energies for Al/Pt, Ni/Ti, and Co/Al metal-metal multilayer thin films have been determined as 95.4(2) kJ/mol, 201(13) kJ/mol, and 247(19) kJ/mol, respectively.

Two examples of anionic complexes having vapochromic behavior are investigated: [K(H2O)][Pt(ppy)(CN)2] “Pt(ppy)” and [K(H2O)][Pt(bzq)(CN)2] “Pt(bzq)”, where ppy = 2-phenylpyridinate and bzq = 7,8-benzoquinolate. These monohydrate-potassium salts exhibit a change in color from purple to yellow [Pt(ppy)] and from red to yellow [Pt(bzq)] upon heating to 110 °C, and they transform back into the original color upon absorption of water molecules from the environment. Available only in the form of polycrystalline samples, no structural information on such compounds is accessible, due to highly overlapping peaks in powder diffraction profiles. We use in situ Pair Distribution Function measurements on powder samples to investigate the dynamics of the structural changes induced by temperature variations. By means of a multivariate approach, we were able to extract dynamic structural information from collected profiles without using prior knowledge on the static crystal structure of the compounds. The critical temperature and the characteristics of the vapochromic transition have been identified, as well as the main structural changes causing it.