Detecting the Guttman effect with the help of ordinal correspondence analysis in synchrotron X-ray diffraction data analysis.

We propose a method for detecting a Guttman effect in a complete disjunctive table U with Q questions. Since such an investigation is a nonsense when the Q variables are independent, we reuse a previous unpublished work about the chi-squared independence test for Burt's tables. Then, we introduce a two-steps method consisting in plugging the first singular vector from a preliminary Correspondence Analysis (CA) of U as a score x into a subsequent singly-ordered Ordinal Correspondence Analysis (OCA) of U . OCA mainly consists in completing x by a sequence of orthogonal polynomials superseding the classical factors of CA. As a consequence, in presence of a pure Guttman effect, we should in principle have that the second singular vector coincide with the polynomial of degree 2, etc. The hybrid decomposition of the Pearson chi-squared statistics (resulting from OCA) used in association with permutation tests makes possible to reveal such relationships, i.e. the presence of a Guttman effect in the structure of U , and to determine its degree - with an accuracy depending on the signal to noise ratio. The proposed method is successively tested on artificial data (more or less noisy), a well-known benchmark, and synchrotron X-ray diffraction data of soil samples.

Ultrafast transient liquid assisted growth of high current density superconducting films.

The achievement of high growth rates in YBa2Cu3O7 epitaxial high-temperature superconducting films has become strategic to enable high-throughput manufacturing of long length coated conductors for energy and large magnet applications. We report on a transient liquid assisted growth process capable of achieving ultrafast growth rates (100 nm s-1) and high critical current densities (5 MA cm-2 at 77 K). This is based on the kinetic preference of Ba-Cu-O to form transient liquids prior to crystalline thermodynamic equilibrium phases, and as such is a non-equilibrium approach. The transient liquid-assisted growth process is combined with chemical solution deposition, proposing a scalable method for superconducting tapes manufacturing. Additionally, using colloidal solutions, the growth process is extended towards fabrication of nanocomposite films for enhanced superconducting properties at high magnetic fields. Fast acquisition in situ synchrotron X-ray diffraction and high resolution scanning transmission electron microscopy (STEM) become crucial measurements in disentangling key aspects of the growth process.

Microsecond time-resolved X-ray diffraction for the investigation of fatigue behavior during ultrasonic fatigue loading.

A new method based on time-resolved X-ray diffraction is proposed in order to measure the elastic strain and stress during ultrasonic fatigue loading experiments. Pure Cu was chosen as an example material for the experiments using a 20 kHz ultrasonic fatigue machine mounted on the six-circle diffractometer available at the DiffAbs beamline on the SOLEIL synchrotron facility in France. A two-dimensional hybrid pixel X-ray detector (XPAD3.2) was triggered by the strain gage signal in a synchronous data acquisition scheme (pump-probe-like). The method enables studying loading cycles with a period of 50 µs, achieving a temporal resolution of 1 µs. This allows a precise reconstruction of the diffraction patterns during the loading cycles. From the diffraction patterns, the position of the peaks, their shifts and their respective broadening can be deduced. The diffraction peak shift allows the elastic lattice strain to be estimated with a resolution of ∼10-5. Stress is calculated by the self-consistent scale-transition model through which the elastic response of the material is estimated. The amplitudes of the cyclic stresses range from 40 to 120 MPa and vary linearly with respect to the displacement applied by the ultrasonic machine. Moreover, the experimental results highlight an increase of the diffraction peak broadening with the number of applied cycles.

Continuous and Collective Grain Rotation in Nanoscale Thin Films during Silicidation.

Texture evolution is an important issue in materials and nanosciences. Understanding it is fundamental for controlling the final orientation, which in fine controls the desired properties of nanodevices. Here, we reveal the formation of a peculiar texture during the silicidation of nanoscale Pd thin films. We demonstrate that the crystallographic relationship observed between the silicide and the Si(001) substrate, named gyroaxy, evolves continuously and collectively during silicidation. This continuous rotation of the nanosized grains over a wide angular range is proposed to be associated with a diffusional mechanism.

Three-dimensional x-ray Fourier transform holography: the Bragg case.

A novel approach to determine the structure of nanoscale crystals in three dimensions is proposed by the use of coherent x-ray Fourier transform holography in Bragg geometry. The full internal description is directly obtained by a single Fourier transform of the 3D intensity hologram. Together with the morphology, Bragg geometry gives access to the 3D displacement field within the crystal. This result opens great possibilities for the investigation of strain fields inside nanocrystals in a simple way.

X-ray diffraction as a local probe tool.

For the structural characterization of nanoscale objects, X-ray diffraction is widely used as a technique complementing local probe analysis methods such as scanning electron microscopy and transmission electron microscopy. Details on strain distributions, chemical composition, or size and shape of nanostructures are addressed. X-ray diffraction traditionally obtains very good statistically averaged properties over large ensembles-provided this averaging is meaningful for ensembles with sufficiently small dispersion of properties. In many cases, however, it is desirable to combine different analysis techniques on exactly the same nano-object, for example, to gain a more detailed insight into the interdependence of properties. X-ray beams focused to diameters in the sub-micron range, which are available at third-generation synchrotron sources, allow for such X-ray diffraction studies of individual nano-objects.

SrTiO3 displacive transition revisited via coherent X-ray diffraction.

We present a coherent x-ray diffraction study of the antiferrodistortive displacive transition of SrTiO3, a prototypical example of a phase transition for which the critical fluctuations exhibit two length scales and two time scales. From the microbeam x-ray coherent diffraction patterns, we show that the broad (short-length scale) and the narrow (long-length scale) components can be spatially disentangled, due to 100-microm-scale spatial variations of the latter. Moreover, both components exhibit a speckle pattern, which is static on a approximately 10 mn time scale. This gives evidence that the narrow component corresponds to static ordered domains. We interpret the speckles in the broad component as due to a very slow dynamical process, corresponding to the well-known central peak seen in inelastic neutron scattering.

Local structure of a rolled-up single crystal: an X-ray microdiffraction study of individual semiconductor nanotubes.

Crystals with cylindrical symmetry, not existing in nature, are mimicked by the roll-up of single-crystalline and highly strained semiconductor bilayers. Exploiting this, the local structure of such individual rolled-up nanotubes is locally probed and quantified nondestructively by x-ray microbeam diffraction. A comparison to simulations, based on the minimization of the elastic energy, allows us to determine layer thicknesses and lattice parameter distributions within the strongly curved bilayers.

Diffractive refractive optics: the possibility of sagittal focusing in Laue-case diffraction.

The sagittal deviation of a Laue-diffracted X-ray beam caused by the inclination of an exit crystal surface with respect to an entrance crystal surface has been studied both theoretically and experimentally. The use of this effect for sagittal focusing of X-ray synchrotron radiation diffracted by a Laue crystal is suggested. The focusing is based on the refraction effect due to the parabolic profile of an exit or/and entrance surface. The crystal is not bent. In order to achieve a reasonable focusing distance, the crystal should be cut asymmetrically. The experiment was performed at beamline BM5 at the ESRF.

Development of a quantitative energy filtering TEM method to study a reactive NiO/80Ni20Fe interface.

Energy filtering TEM (EFTEM) has been performed on an annealed NiO/80Ni20Fe interface. Chemical maps have been calculated using the three-window technique on the O-K, Fe-L23 and Ni-L23 edges. In this paper we show that relative quantification can be made using reference areas on the images taken from part to part of the interface in well-known composition areas. Partial cross-section ratios sigmaNi(20 eV)/sigmaO(20 eV) and sigmaNi(20 eV)/sigmaFe(20 eV) have been then measured and used to extract the chemical composition of the reactive NiO/80Ni20Fe interface. Fe, Ni and O composition profiles across the interface have been obtained showing the diffusion process which has occurred during annealing. The reliability of the EFTEM measurements has been checked by EEL spectroscopy on the same sample as well as on a reference geological oxide sample (Trevorit: NiFe2O4). The partial cross-section ratios obtained with the two methods (EFTEM and EELS) are in good agreement.

Atomic structure of the polar NiO(111)- p(2x2) surface

Using grazing-incidence x-ray diffraction, the p(2x2) surface structures of the single crystal NiO(111) and a 5 monolayer thick NiO(111) film on Au(111) were both shown to exhibit locally the theoretically predicted octopolar reconstruction, with some important differences. The single crystal exhibits a single Ni termination with double steps. The thin film exhibits both possible terminations (O and Ni) and single steps. These surfaces were found to be nonreactive with respect to hydroxylation.

Magnetization profile of ultrathin FePd films.

The method of circular dichroism in X-ray resonant magnetic scattering is presented which allows a straightforward determination of the magnetization profile of magnetic patterns in ultrathin films. Application to single crystalline FePd layers shows unambiguously the presence of magnetic flux closure domains whose thickness can constitute a significant fraction ( approximately 25%) of the total film.

Chiral magnetic domain structures in ultrathin FePd films

The magnetization profile of magnetically ordered patterns in ultrathin films was determined by circular dichroism in x-ray resonant magnetic scattering (CDXRMS). When this technique was applied to single crystalline iron palladium alloy layers, magnetic flux closure domains were found whose thickness can constitute a large fraction ( approximately 25 percent) of the total film.