Investigation of the solid-liquid phase transition of carbon at 150 GPa with spectrally resolved X-ray scattering

We have resolved the solid-liquid phase transition of carbon at pressures around 150GPa. High-pressure samples of different temperatures were created by laser-driven shock compression of graphite and varying the initial density from 1.30g/cm³ to 2.25g/cm³. In this way, temperatures from 5700K to 14,500K could be achieved for relatively constant pressure according to hydrodynamic simulations. From measuring the elastic X-ray scattering intensity of vanadium K-alpha radiation at 4.95keVat a scattering angle of 126°, which is very sensitive to the solid-liquid transition, we can determine whether the sample had transitioned to the fluid phase. We find that samples of initial density 1.3g/cm³ and 1.85g/cm³ are liquid in the compressed states, whereas samples close to the ideal graphite crystal density of 2.25g/cm³ remain solid, probably in a diamond-like state.

Time-resolved in situ X-ray scattering studies of aqueous hydroxypropylcellulose solutions

The evolution of the global orientation parameter for a series of aqueous hydroxypropylcellulose solutions both during and following the cessation of a steady-state shear flow is reported. Time-resolved orientation measurements were made in situ through a novel X-ray rheometer coupled with a two-dimensional electronic X-ray camera, and using an intense X-ray source at the LURE synchrotron. After the cessation of flow, the global orientation decreases from the steady-state orientation level to zero following shear flow at low shear rate or to a small but finite value after flow at a high shear rate. The decrease of orientation with time shows different behaviour, dependent upon the previously applied shear rate.

Experimental separation of the coherent component of X-ray scattering prior to RDF analysis of non-crystalline polymers

An experimental method is described which enables the inelastically scattered X-ray component to be removed from diffractometer data prior to radial density function analysis. At each scattering angle an energy spectrum is generated from a Si(Li) detector combined with a multi-channel analyser from which the coherently scattered component is separated. The data obtained from organic polymers has an improved signal/noise ratio at high values of scattering angle, and a commensurate enhancement of resolution of the RDF at low r is demonstrated for the case of PMMA (ICI `Perspex'). The method obviates the need for the complicated correction for multiple scattering.

Electronic excitations in solids studied using inelastic x-ray scattering

Inelastic x-ray scattering can be used to study the electronic structure of matter. The x rays scattered from the target both induce and carry information on the electronic excitations taking place in the system. These excitations are the manifestations of the electronic structure and the physics governing the many-body system. This work presents results of non-resonant inelastic x-ray scattering experiments on a range of materials including metallic, insulating and semiconducting compounds as well as an organic polymer. The experiments were carried out at the National Synchrotron Light Source, USA and at the European Synchrotron Radiation Facility, France. The momentum transfer dependence of the experimental valence- and core-electron excitation spectra is compared with the results of theoretical first principles computations that incorporate the electron-hole interaction. A recently developed method for analyzing the momentum transfer dependence of core-electron excitation spectra is studied in detail. This method is based on real space multiple scattering calculations and is used to extract the angular symmetry components of the local unoccupied density of final states.

New computational approaches for inelastic x-ray scattering

Inelastic x-ray scattering spectroscopy is a versatile experimental technique for probing the electronic structure of materials. It provides a wealth of information on the sample's atomic-scale structure, but extracting this information from the experimental data can be challenging because there is no direct relation between the structure and the measured spectrum. Theoretical calculations can bridge this gap by explaining the structural origins of the spectral features. Reliable methods for modeling inelastic x-ray scattering require accurate electronic structure calculations. This work presents the development and implementation of new schemes for modeling the inelastic scattering of x-rays from non-periodic systems. The methods are based on density functional theory and are applicable for a wide variety of molecular materials. Applications are presented in this work for amorphous silicon monoxide and several gas phase systems. Valuable new information on their structure and properties could be extracted with the combination of experimental and computational methods.

The structure of amorphous platinum disulfide as studied by anomalous x-ray-scattering

Anomalous X-ray scattering (AXS) has been applied to study the structure of amorphous platinum disulfide, Pt1-xS2, prepared by the precipitation process. The local atomic arrangement in amorphous Pt1-xS2 was determined by the least-squares variational method so as to reproduce the experimental differential interference function at the Pt L(III) absorption edge by the AXS method as well as the ordinary interference function by MoK alpha. The structural unit in amorphous Pt1-xS2 is found to be a PtS6 octahedron, similar to that in crystalline PtS2. These octahedra share both their corners and edges, while only edge-sharing linkages occur in crystalline PtS2.

Anomalous X-ray scattering study of local structures in the superionic conducting class (CuI)(0.3)(Cu2O)(0.35)(MoO3)(0.35)

The anomalous X-ray scattering (AXS) method using Cu and Mo K absorption edges has been employed for obtaining the local structural information of superionic conducting glass having the composition (CuI)(0.3)(Cu2O)(0.35)(MoO3)(0.35). The possible atomic arrangements in near-neighbor region of this glass were estimated by coupling the results with the least-squares analysis so as to reproduce two differential intensity profiles for Cu and Mo as well as the ordinary scattering profile. The coordination number of oxygen around Mo is found to be 6.1 at the distance of 0.187 nm. This implies that the MoO6 octahedral unit is a more probable structural entity in the glass rather than MoO4 tetrahedra which has been proposed based on infrared spectroscopy. The pre-peak shoulder observed at about 10 nm(-1) may be attributed to density fluctuation originating from the MoO6 octahedral units connected with the corner sharing linkage, in which the correlation length is about 0.8 nm. The value of the coordination number of I- around Cu+ is estimated as 4.3 at 0.261 nm, suggesting an arrangement similar to that in molten CuI.

Local environmental structures of Mo in the superionic conducting glass (AgI)(0.6)(Ag2MoO4)(0.4) by anomalous X-ray scattering

The anomalous X-ray scattering (AXS) method using Mo K absorption edges has been employed for obtaining the local structural information of superionic conducting glass having the composition (AgI)(0.6)(Ag2MoO4)(0.4). The possible atomic arrangements in the near-neighbor region of this glass were estimated by coupling the results with the least-squares variational analysis so as to reproduce the differential intensity profile for Mo as well as the ordinary scattering profile. The coordination number of oxygen around Mo is found to be about 4 at the distance of 0.180 mn. This implies that the most probable structural entity in the glass is the MoO4 tetrahedral unit which has been proposed based on infrared spectroscopy. The value of the coordination number of I- around Ag+ is estimated as 4.4 at 0.287 nm, suggesting an arrangement similar to that of crystalline or molten AgI.

Anomalous X-ray scattering study of local structures in the superionic conducting glass (AgBr)0.4 (Ag2O)0.3 (GeO2)0.3

The local structural information in the near-neighbor region of superionic conducting glass (AgBr)0.4(Ag2O)0.3(GeO2)0.3 has been estimated from the anomalous X-ray scattering (AXS) measurements using Ge and Br K absorption edges. The possible atomic arrangements in the near-neighbor region of this glass were obtained by coupling the results with the least-squares variational method so as to reproduce two differential intensity profiles for Ge and Br as well as the ordinary scattering profile. The coordination number of oxygen around Ge is found to be 3.6 at a distance of 0.176 nm, suggesting the GeO4 tetrahedral unit as the probable structural entity in this glass. Moreover, the coordination number of Ag around Br is estimated as 6.3 at a distance of 0.284 nm, suggesting an arrangement similar to that in crystalline AgBr.

Dispersion of polymer grafted nanoparticles in polymer nanocomposite films: Insights from surface x-ray scattering and microscopy

Dispersion of nanoparticles in polymer nanocomposite films determines the application potential of these systems as novel materials with unique physical properties. Grafting polymers to, mostly inorganic, nanoparticles has been suggested as an effective strategy to enhance dispersion and hence the efficacy of materials. In this review, we discuss the various parameters which control dispersion of polymer grafted nanoparticles in polymer nanocomposite films. We discuss how surface x-ray scattering and microscopy can provide complementary and unique information in thin polymer nanocomposite films to unravel the subtle interplay of entropic and surface interactions, mediated by confinement, that leads to enhanced dispersion of the nanoparticles in these films. (C) 2014 AIP Publishing LLC.

DETERMINATION OF SURFACE-ROUGHNESS OF INP (001) WAFERS BY X-RAY-SCATTERING

The surface roughness of polished InP (001) wafers were examined by x-ray reflectivity and crystal truncation rod (CTR) measurements. The root-mean-square roughness and the lateral correlation scale were obtained by both methods. The scattering intensities in the scans transverse to the specular reflection rod were found to contain two components. A simple surface model of surface faceting is proposed to explain the experimental data. The sensitivities of the two methods to the surface structure and the role of the resolution functions in the CTR measurements are discussed.

X-RAY-SCATTERING FROM A ROUGH-SURFACE AND DAMAGED LAYER OF POLISHED WAFERS

Theoretical and experimental investigations were performed to show the application of x-ray crystal truncation rod scattering combined with x-ray reflectivity in the measurements of surface roughness and near-surface damage of mechanochemically polished wafers. By fitting the measured crystal truncation rod curves it has been shown that polished wafers are divided into three parts -irregular steps on the surface, a damaged thin layer beneath the surface and a perfect bulk. The results show that the root mean square of the surface roughness of mechanochemically polished Fe-doped and/or S-doped InP wafers is one to two atom layers, and that the lateral correlation length of the surface roughness is about 3000-7500 Angstrom. The thickness of the damaged region is found to be about 1000 atom layers.

INPLANE X-RAY-SCATTERING OF EPITAXIAL STRUCTURES

A new approach for in-plane X-ray scattering from the cleavages of epitaxial films or superlattices, where the scattering vectors are parallel to the interfaces, is proposed. This method can be employed to determine directly the in-plane X-ray strains and other atomic registry along the interfaces of the epitaxial structures.