D. Babonneau

FitGISAXS: software package for modelling and analysis of GISAXS data using IGOR Pro

A software package for performing modelling and analysis of GISAXS (grazing-incidence small-angle X-ray scattering) data within the distorted-wave Born approximation has been developed using the IGOR Pro scripting language (http://www.wavemetrics.com). The tool suite uses a slab-model approach with the Abeles matrix method to calculate X-ray reflectivity curves, electric field intensity distributions and GISAXS intensities from supported or buried scatterers arranged in two or three dimensions in a stratified medium. Models are included to calculate the scattered intensity for monodisperse, polydisperse and interacting particles with various size distributions, form factors and structure factors. The source code for the entire package is freely available, allowing anyone to develop additional tools.

Structural study of 3D-hexagonal mesoporous spin-coated sol–gel films

Mesostructured films deposited on glass substrates by spin coating are studied by X-ray diffraction, small angle X-ray scattering using grazing incidence (GISAXS) and high resolution electron microscopy. The films generally present a gradient of ordering from the air/sol interface to the interior of the film, with a 3D-hexagonal mesophase near the surface and a disordered micellar structure at the interior. However, the 3D-hexagonal ordering and the texturing can be extended over all the film thickness by adjusting the composition of the deposited solution. In particular, critical values are clearly observed both for the size of silica units forming the walls in the mesophase and for the film thickness. All these results can be understood from the competition between structuration and gelation of the films during alcohol removal.

Grazing-incidence small-angle X-ray scattering applied to the characterization of aggregates in surface regions

Abstract Ion-beam sputtering deposition has been used to elaborate discontinuous gold and granular carbon–platinum thin films. The morphology of the deposited gold islands and buried platinum clusters so obtained has been studied by grazing incidence small-angle X-ray scattering (GISAXS). The full potentiality of this non-destructive technique at grazing incidence is obtained when it is coupled with a synchrotron radiation beam and two-dimensional detectors. The influence of argon ion-implantation performed during Au or C–Pt growth has been studied. A relevant information to understand and control the structural properties of such materials is then achieved.

Structural and magnetic properties of CoPt mixed clusters

In this present work, we report a structural and magnetic study of mixed Co58Pt42 clusters. MgO, Nb and Si matrix can be used to embed clusters, avoiding any magnetic interactions between particles. Transmission Electron Microscopy (TEM) observations show that Co58Pt42 supported isolated clusters are about 2nm in diameter and crystallized in the A1 fcc chemically disordered phase. Grazing Incidence Small Angle X-ray Scattering (GISAXS) and Grazing Incidence Wide Angle X-ray Scattering (GIWAXS) reveal that buried clusters conserve these properties, interaction with matrix atoms being limited to their first atomic layers. Considering that 60% of particle atoms are located at surface, this interactions leads to a drastic change in magnetic properties which were investigated with conventional magnetometry and X-Ray Magnetic Circular Dichroism (XMCD). Magnetization and blocking temperature are weaker for clusters embedded in Nb than in MgO, and totally vanish in silicon as silicides are formed. Magnetic volume of clusters embedded in MgO is close to the crystallized volume determined by GIWAXS experiments. Cluster can be seen as a pure ferromagnetic CoPt crystallized core surrounded by a cluster-matrix mixed shell. The outer shell plays a predominant role in magnetic properties, especially for clusters embedded in niobium which have a blocking temperature 3 times smaller than clusters embedded in MgO.

Morphology of encapsulated iron nanoparticles obtained by co-sputtering and implantation: a GISAXS study

A grazing incidence small-angle X-ray scattering (GISAXS) study is presented on the morphology of iron nanoparticles buried in carbon matrices, obtained either by ion-beam sputtering co-deposition or by ion-implantation. It is shown that, depending on the experimental synthesis conditions, the shape of the iron nanoparticles is either spherical or elongated perpendicularly to the substrate. The possible growth mechanisms are examined in terms of volume and surface diffusion, defect density, interfacial energy and residual stress.

Co-sputtering C-Cu thin film synthesis : microstructural study of copper precipitates encapsulated into a carbon matrix

Abstract Co-sputtered C-Cu thin film depositions have been performed in the temperature range 80-873 K, the atomic carbon concentration varying from 16% to 96%. To characterize the microstructure of the C-Cu thin films, transmission electron microscopy, extended X-ray absorption fine structure and grazing incidence small angle X-ray scattering experiments have been used. During the deposition process, a demixing occurs of the carbon and copper species due to their very low solubilities that leads to the formation of nanometric copper precipitates homogeneously distributed in a more or less graphitic matrix. These precipitates have an elongated shape in the direction of the thin film growth. When the deposition was performed at 273 K for copper atomic concentrations CCu > 55%, as well as for all thin films synthesized at 573 K whatever the CCu value, the formation of graphene layers parallel to the surface of the copper precipitates was observed so that an encapsulation of the Cu aggregates in carbon cages...

Morphological characterization of ion-sputtered C–Ag, C/C–Ag and Ag/C films by GISAXS

A carbon–silver thin film (33 at.% Ag and thickness of 2100 A) has been synthesized by co-sputtering of a C–Ag target and characterized by grazing-incidence small-angle X-ray scattering (GISAXS), a technique that gives a considerably enhanced surface sensitivity. Experiments have been carried out at or near the critical angle of the layer. It is shown that, because C and Ag show no mutual solubility, a demixing occurs during the co-deposition process and silver clusters form within an amorphous carbon matrix. Using different incident angles of the X-ray beam, it is demonstrated that two populations of clusters are present in the layer: some large and nearly spherical on the surface, others smaller and elongated along the direction of the growth of the thin film in the bulk. In the case of a C/C–Ag bilayer, the surface diffusion is avoided just after the co-deposition process and it is shown that only the small and elongated clusters in the bulk are formed. In the case of a very thin Ag/C layer, there is only surface diffusion and it is shown that large silver islands are formed on the carbon surface. Such experiments demonstrate that the growth mechanism that takes place during the co-deposition process involves mainly a surface diffusion of silver and carbon atoms, as opposed to a volume diffusion.

Microstructural study of a C–Fe alloy synthesized by ion-beam sputtering co-deposition

A carbon–iron thin film, composition 46 at. % Fe and thickness 26 nm, was synthesized by ion-beam sputtering with a substrate temperature of 573 K. The microstructure of the film was characterized by transmission electron microscopy and small-angle x-ray scattering under grazing incidence. It consisted of iron-rich particles, with an average in-plane diameter of 3.2 nm, uniformly dispersed in a graphite-like carbon matrix. These particles were elongated along the in-depth direction, that of the thin-film growth. After annealing at 623 K for 1 h, no modification in the microstructure of the film was observed. The present study shows that the co-sputtering of graphite and iron performed at low temperature in comparison with the conventional arc discharge method, is a useful synthesis method to obtain thin films of encapsulated nanoparticles which have a good thermal stability.

Copper coverage effect on tungsten crystallites texture development in W/Cu nanocomposite thin films

Morphological and crystallographic structures of multilayered W/Cu nanocomposite thin films elaborated by physical vapor deposition were studied by varying copper and tungsten thicknesses. Sample examinations were performed by x-ray diffraction (XRD), grazing incidence small-angle x-ray scattering and transmission electron microscopy (TEM). Samples were found to be composed of copper nanoparticles, homogeneously dispersed in planes parallel to the film-substrate interface and periodically separated by tungsten layers along the growth direction. Our observations revealed an original texture development of the tungsten matrix from a mixture of unexpected α-W⟨111⟩ and α-W⟨110⟩ components to unique α-W⟨110⟩ component as the copper coverage passes a thickness threshold of 0.6 nm. Local TEM texture stereology investigations revealed simultaneous columnar growth of both preferential orientations posterior to polycrystalline development while XRD reveals strong compressive residual stresses in both texture compon...

Structure of Glancing Incidence Deposited TiO2 Thin Films as Revealed by Grazing Incidence Small-Angle X-ray Scattering

For the first time, grazing incidence small-angle X-ray scattering (GISAXS) analysis is used to characterize the morphology of TiO(2) thin films grown by glancing angle physical vapor deposition (GLAD). According to cross-section scanning electron microscopy (SEM) images, the films consist of near isotilted TiO(2) columns of different length and width depending on film thickness. The obtained GISAXS patterns show a characteristic asymmetry with respect to the incidence plane, which is associated with the tilted geometry of the TiO(2) columns. The patterns also show the existence of two populations of columns in these GLAD-TiO(2) films. The population of the thinnest columns appears related to the first grown layer and is common for all the films investigated, while the second population of columns grows with the thickness of the films and has been related to wider columns formed by shadowing at the expense of the initially formed columns.