Atomic imaging of oxide-supported metallic nanocrystals.

The nucleation of noble metal nanoparticles on oxide surfaces can lead to dramatic enhancements in catalytic activity that are related to the atomic-scale formation of the nanoparticles and interfaces. For the case of submonolayer Pt deposited on the 2×1 SrTiO(3)(001) surface atomic-force microscopy shows the formation of nanoparticles. We use X-ray standing wave (XSW) atomic imaging to show that these nanoparticles are composed of Pt face-centered-cubic nanocrystals with cube-on-cube epitaxy laterally correlated to the substrate unit cell. The phase sensitivity of the XSW allows for a direct measurement of the interface offset between the two unit cells along the c-axis. Different Pt coverages lead to differences in the observed XSW image of the interfacial structure, which is explained by a proposed model based on the Pt-Pt interaction becoming stronger than the Pt-substrate interaction as the global coverage is increased from 0.2 to 0.6 ML.

Cosputtered composition-spread reproducibility established by high-throughput x-ray fluorescence.

We describe the characterization of sputtered yttria-zirconia composition spread thin films by x-ray fluorescence (XRF). We also discuss our automated analysis of the XRF data, which was collected in a high throughput experiment at the Cornell High Energy Synchrotron Source. The results indicate that both the composition reproducibility of the library deposition and the composition measurements have a precision of better than 1 atomic percent.

High energy x-ray diffraction/x-ray fluorescence spectroscopy for high-throughput analysis of composition spread thin films.

High-throughput crystallography is an important tool in materials research, particularly for the rapid assessment of structure-property relationships. We present a technique for simultaneous acquisition of diffraction images and fluorescence spectra on a continuous composition spread thin film using a 60 keV x-ray source. Subsequent noninteractive data processing provides maps of the diffraction profiles, thin film fiber texture, and composition. Even for highly textured films, our diffraction technique provides detection of diffraction from each family of Bragg reflections, which affords direct comparison of the measured profiles with powder patterns of known phases. These techniques are important for high throughput combinatorial studies as they provide structure and composition maps which may be correlated with performance trends within an inorganic library.

A methodology for measuring in situ lattice strain of bulk polycrystalline material under cyclic load.

The material response of polycrystalline materials under cyclic loading is not fully understood. Even during uniaxial loading, individual grains embedded within the polycrystalline material can experience complicated strain histories. By quantifying the deformation state at the crystal level, we can begin to understand the conditions that lead to fatigue failure. An in situ powder diffraction method was developed and employed at the Cornell High Energy Synchrotron Source to measure the aggregate crystal response at various points in a material's life using synchrotron x ray. A set of experiments was conducted using a load frame capable of exerting cyclic uniaxial loads on a specimen. A high speed x-ray shutter was developed to synchronize the x-ray beam and the loading cycle. Using the high speed shutter, the evolution of the lattice strains for the families of crystallographic planes was measured while the aggregate was under cyclic uniaxial loading, thus monitoring a live evolution of lattice strain in a cyclically loaded specimen. The methodology is demonstrated using uniaxial cyclic specimens machined from oxygen free conductivity (OFHC) copper sheet.

Dynamics of bimodal growth in pentacene thin films.

Previous studies have established that pentacene films deposited on silicon oxide consist of a substrate-induced "thin-film" phase, with the bulk phase of pentacene detected in thicker films only. We show that the bulk phase nucleates as early as the first monolayer, and continues to nucleate as film growth progresses, shadowing the growth of the thin-film phase. Moreover, we find that the transition between the "thin-film" and the bulk phase is not a continuous one, as observed in heteroepitaxial systems, but rather the two phases nucleate and grow independently.

Multilayer X-ray optics at CHESS.

Almost half of the X-ray beamlines at the Cornell High Energy Synchrotron Source (CHESS) are based on multilayer optics. ;Traditional' multilayers with an energy resolution of DeltaE/E approximately 2% are routinely used to deliver X-ray flux enhanced by a factor of 10(2) in comparison with standard Si(111) optics. Sagittal-focusing multilayers with fixed radius provide an additional factor of 10 gain in flux density. High-resolution multilayer optics with DeltaE/E approximately 0.2% are now routinely used by MacCHESS crystallographers. New wide-bandpass multilayers with DeltaE/E = 5% and 10% have been designed and tested for potential applications in macromolecular crystallography. Small d-spacing multilayers with d < or = 20 A have been successfully used to extend the energy range of multilayer optics. Analysis of the main characteristics of the Mo/B4C and W/B4C small d-spacing multilayer optics shows enhancement in their performance at higher energies. Chemical vapour deposited SiC, with a bulk thermal conductivity of a factor of two higher than that of silicon, has been successfully introduced as a substrate material for multilayer optics. Characteristics of different types of multilayer optics at CHESS beamlines and their applications in a variety of scattering, diffraction and imaging techniques are discussed.

Crystallographic data collection using a 0.22% bandwidth multilayer.

To bridge the gap between traditional multilayer and crystal optics a high-resolution multilayer monochromator with a bandwidth of 0.22% has been designed and installed on a bending-magnet beamline (F3) at the Cornell High Energy Synchrotron Source (CHESS) to provide an unfocused monochromatic X-ray beam for protein crystallography experiments. Crystallographic data of excellent quality from a medium-sized protein, Concanavalin A, were collected and processed using standard crystallographic programs. The data were successfully used for a structure solution and refinement. The flux from the multilayer monochromator is enhanced, relative to that from a flat Si(111) monochromator, by a factor of 5; consequently, data collection is faster and/or smaller samples may be used. At the same time, the bandwidth is narrow enough to avoid streaked spots. This experiment suggests that multilayer optics may play a valuable role in satisfying the demands of the structural biology community for rapid X-ray data collection, particularly at under-utilized bending-magnet beamlines.