We present the first structure determination by surface x-ray diffraction during the restructuring of a model catalyst under reaction conditions, i.e., at high pressure and high temperature, and correlate the restructuring with a change in catalytic activity. We have analyzed the Pt(110) surface during CO oxidation at pressures up to 0.5 bar and temperatures up to 625 K. Depending on the O 2 =CO pressure ratio, we find three well-defined structures: namely, (i) the bulk-terminated Pt(110) surface, (ii) a thin, commensurate oxide, and (iii) a thin, incommensurate oxide. The commensurate oxide only appears under reaction conditions, i.e., when both O 2 and CO are present and at sufficiently high temperatures. Density functional theory calculations indicate that the commensurate oxide is stabilized by carbonate ions (CO 2ÿ 3 ). Both oxides have a substantially higher catalytic activity than the bulk-terminated Pt surface.

The origin of the catalytic activity of gold nanoparticles remains debated despite extensive studies. This in operando work investigates the relationship between catalytic activity and size/shape of gold nanoparticles supported on TiO2(110) during CO oxidation. The nanoparticles were synthesized by vapor deposition in ultrahigh vacuum. Their geometry was monitored in the presence of O2, Ar, or a mixture of O2 + CO and of Ar + CO by grazing incidence small-angle X-ray scattering simultaneously with the catalytic activity. The occurrence of CO oxidation induces a sintering directly correlated to the reaction rate. The catalytic activity is optimum for a nanoparticle’s diameter of 2.1 ± 0.3 nm and a height of about six atomic layers. Below this size, the activity drop corresponds to a height decrease. Rescaling of activities obtained in different experimental conditions shows consistency of these results with published data using both “model” and “real” catalysts.

A white beam microdiffraction setup has been developed on the bending magnet source BM32 at the European Synchrotron Radiation Facility. The instrument allows routine submicrometer beam diffraction to perform orientation and strain mapping of polycrystalline samples. The setup features large source to optics distances allowing large demagnification ratios and small beam sizes. The optics of the beamline is used for beam conditioning upstream a secondary source, suppressing any possible interference of beam conditioning on beam size and position. The setup has been designed for an easy and efficient operation with position control tools embedded on the sample stage, a high magnification large aperture optical microscope, and fast readout detectors. Switching from the white beam mode to the monochromatic mode is made easy by an automatic procedure and allows the determination of both the deviatoric and hydrostatic strain tensors.

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The structure and morphology of Ag deposits grown at room temperature on high-quality MgO͑001͒ surfaces have been investigated in situ, from 0.2 to 300 equivalent monolayers ͑ML͒ of Ag deposited. Surface x-ray diffraction and grazing incidence small angle x-ray scattering parallel and perpendicular to the surface were combined. Nucleation, growth, and coalescence of islands are found from 0.2 ML. The average in-plane width, height, and in-plane separation of growing islands are deduced and are found to reproduce well the Mg 1s x-ray photoemission spectroscopy spectrum previously reported by other authors. The height over width ratio of the islands is ϳ0.37Ϯ0.05 at all stages of the deposit. Ag grows in cube-on-cube epitaxy with respect to the MgO͑001͒ substrate. A very unusual evolution of the state of strain in Ag with increasing amount of Ag deposited is observed. Below 4-6 ML ͑island width smaller than 90 Å͒, the small Ag islands are coherent with the MgO. Below 1 ML ͑island width smaller than 35 Å͒, they have their bulk lattice parameter, and between 1 and 4 ML they become more and more strained by the MgO substrate, with an average lattice parameter intermediate between those of Ag and of MgO. Around 4-6 ML, the islands reach a critical size and misfit dislocations are introduced at the edges. Above 30 ML, the film is almost continuous, and the interfacial misfit dislocations reorder to form a square network, oriented along ͗110͘ directions. Stacking faults appear in Ag at this stage. A small amount of twinned Ag also starts to grow around 4 ML. This unusual evolution of the strain in the Ag islands and the following introduction of misfit dislocations are interpreted on the basis of a one-dimensional Frenkel-Kontorova model involving a very weak Ag-MgO interaction and a weak corrugation of the interatomic potential. Quantitative measurements and analysis of the MgO crystal truncation rods ͑CTR's͒ during growth were shown to provide different structural parameters of the interface that are important for theoretical calculation, especially the epitaxial site, above oxygen atoms of the substrate, and the interfacial distance (2.52Ϯ0.1 Å). The origin of the interference along the CTR's is discussed according to the strain state of the epitaxial Ag. ͓S0163-1829͑99͒14131-6͔ PHYSICAL REVIEW B 15 AUGUST 1999-II VOLUME 60, NUMBER 8 PRB 60 0163-1829/99/60͑8͒/5858͑14͒/$15.00 5858

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The in situ three-point bending of a single self-suspended Au nanowire is visualized by micro Laue diffraction. The nanowire deflection is inferred from the displacement of Laue spots and it is well described by finite element analysis taking into account geometric nonlinearities and the elastic constants of bulk Au.

Quantitative structural information about epitaxial arrays of nanowires are reported for a InAs/InP longitudinal heterostructure grown by chemical beam epitaxy on an InAs (111)B substrate. Grazing incidence X-ray diffraction allows the separation of the nanowire contribution from the substrate overgrowth and gives averaged information about crystallographic phases, epitaxial relationships (with orientation distribution), and strain. In-plane strain inhomogeneities, intrinsic to the nanowires geometry, are measured and compared to atomistic simulations. Small-angle X-ray scattering evidences the hexagonal symmetry of the nanowire cross-section and provides a rough estimate of size fluctuations.