arXiv subjects

Frédéric De Geuser

Publications and source records attributed to Frédéric De Geuser.

11 recordsLinked to original sources

arXiv2026

Spatial resolution(s) in atom probe tomography

Atom probe tomography (APT) is often quoted to provide "atomic-scale" analysis of materials in three dimensions. Despite efforts to quantify APT's spatial resolution, misunderstanding remain regarding its true spatial performance. If the depth resolution was once reported to be 20 pm, quoting this value outside of its specific context is misleading and should be avoided. The resolution achievable in pure metals, at one specific location within one reconstructed dataset, does not generally apply across materials or analysis conditions, or even throughout a single tomographic reconstruction. Here, we review various efforts at defining and measuring the spatial resolution in the study of single phase and single element materials - i.e. pure metals - in field-ion microscopy (FIM) and APT. We also report on the degradation of the resolution arising from ion optical devices used to improve the mass-resolution. We aim to offer some perspective as to how reported resolutions may be or may not be of any relevance to most of the materials characterisation efforts by APT, including cases of precipitates in a matrix that emphasise the need to consider an effective resolution. Finally, we discuss concepts to improve the spatial accuracy of the technique in a relatively distant future.

cond-mat.mtrl-sci↗

arXiv2023

The human factor: results of a small-angle scattering data analysis Round Robin

A Round Robin study has been carried out to estimate the impact of the human element in small-angle scattering data analysis. Four corrected datasets were provided to participants ready for analysis. All datasets were measured on samples containing spherical scatterers, with two datasets in dilute dispersions, and two from powders. Most of the 46 participants correctly identified the number of populations in the dilute dispersions, with half of the population mean entries within 1.5% and half of the population width entries within 40%, respectively. Due to the added complexity of the structure factor, much fewer people submitted answers on the powder datasets. For those that did, half of the entries for the means and widths were within 44% and 86% respectively. This Round Robin experiment highlights several causes for the discrepancies, for which solutions are proposed.

physics.data-an↗

arXiv2020

Intermixing of Fe and Cu on the atomic scale by high-pressure torsion as revealed by DC- and AC-SQUID susceptometry and atom probe tomography

The capability of high-pressure torsion on the preparation of supersaturated solid solutions, consisting of Cu-14Fe (wt.%), is studied. From microstructural investigations a steady state is obtained with nanocrystalline grains. The as-deformed state is analyzed with atom probe tomography, revealing an enhanced solubility and the presence of Fe-rich particles. The DC-hysteresis loop shows suppressed long range interactions in the as-deformed state and evolves towards a typical bulk hysteresis loop when annealed at 500°C. AC-susceptometry measurements of the as-deformed state reveal the presence of a superparamagnetic blocking peak, as well as a magnetic frustrated phase, whereas the transition of the latter follows the Almeida-Thouless line, coinciding with the microstructural investigations by atom probe tomography. AC-susceptometry shows that the frustrated state vanishes for annealing at 250°C.

cond-mat.mtrl-sci↗

arXiv2020

Metrology of small particles and solute clusters by atom probe tomography

Atom probe tomography (APT) is routinely used for analyzing property-enhancing particles in the nanometer-size range and below, and plays a prominent role in the analysis of solute clusters. However, the question of how well these small particles are measured has never been addressed because of a lack of a reliable benchmark. Here, to address this critical gap, we use an approach that allows direct comparison of APT and small-angle (X-Ray) scattering (SA(X)S) performed on the same material. We introduce the notion of an effective spatial resolution for the analysis of particles, which, importantly in this context, is very different than the technique's inherent spatial resolution. This effective resolution is highly specific to the system being considered, as well as the analysis conditions. There is no hard limit below which the technique will fail, but particles with a radius of order of \textapprox $2σ=1nm$, i.e. \textapprox\num{250} atoms cannot be accurately measured, even though the particles are detected. This thorough metrological assessment of APT in the analysis of particles allows us to discuss the pulse spread function of the technique and the physics underpinning its limits. We conclude that great care should be taken when analysing solute clusters by APT, in particular when reporting particle size and composition.

cond-mat.mtrl-sci↗

arXiv2019

Structure and mechanical behavior of ultrafine-grained aluminum-iron alloy stabilized by nanoscaled intermetallic particles

Ultrafine-grained aluminum alloys offer interesting multifunctional properties with a combination of high strength, low electrical resistivity, and low density. However, due to thermally induced grain coarsening, they typically suffer from an intrinsic poor thermal stability. To overcome this drawback, an Al-2%Fe alloy has been selected because of the low solubility of Fe in Al and their highly positive enthalpy of mixing leading to the formation of stable intermetallic particles. The two-phase alloy has been processed by severe plastic deformation to achieve simultaneously submicrometer Al grains and a uniform distribution of nanoscaled intermetallic particles. The influence of the level of deformation on the microstructure has been investigated thanks to transmission electron microscopy and atom probe tomography and it is shown that for the highest strain a partial dissolution of the metastable Al6Fe particle occurred leading to the formation of a Fe super saturated solid solution. The thermal stability, and especially the precipitation of particles from the ultrafine-grained solid solution and the way they pin grain boundaries has been investigated both from static annealing and in-situ transmission electron microscopy experiments. The correlation between microstructural features and microhardness has been established to identify the various strengthening contributions. Finally, it is 2 shown that ultrafine grained high purity Al with less than 0.01 at. % Fe in solid solution could preserve a grain size only 300nm after 1h at 250$^\circ$C.

cond-mat.mtrl-sci↗

arXiv2019

Advanced Non-Destructive in Situ Characterization of Metals with the French Collaborating Research Group D2AM/BM02 Beamline at the European Synchrotron Radiation Facility

The ability to non-destructively measure the structural properties of devices, either in situ or operando, are now possible using an intense X-ray synchrotron source combined with specialized equipment. This tool attracted researchers, in particular metallurgists, to attempt more complex and ambitious experiments aimed at answering unresolved questions in formation mechanisms, phase transitions, and magnetism complex alloys for industrial applications. In this paper, we introduce the diffraction diffusion anomale multi-longueur d'onde (D2AM) beamline, a French collaborating research group (CRG) beamline at the European Synchrotron Radiation Facility (ESRF), partially dedicated to in situ X-ray scattering experiments. The design of the beamline combined with the available equipment (two-dimensional fast photon counting detectors, sophisticated high precision kappa diffractometer, a variety of sample environments, continuous scanning for X-ray imaging, and specific software for data analysis) has made the D2AM beamline a highly efficient tool for advanced, in situ synchrotron characterization in materials science, e.g., single crystal or polycrystalline materials, powders, liquids, thin films, or epitaxial nanostructures. This paper gathers the main elements and equipment available at the beamline and shows its potential and flexibility in performing a wide variety of temporally, spatially, and energetically resolved X-ray synchrotron scattering measurements in situ.

cond-mat.mtrl-sci↗

arXiv2018

Clustering kinetics during natural ageing of Al-Cu based alloys with (Mg, Li) additions

Room temperature solute clustering in aluminium alloys, or natural ageing, despite its industrial relevance, is still subject to debate, mostly due to its experimentally challenging nature. To better understand the complex multi-constituents' interactions at play, we have studied ternary and quaternary subsystems based on the Al-Cu alloys, namely Al-Cu-Mg, Al-Cu-Li and Al-Cu-Li-Mg. We used a recently introduced correlative technique using small-angle neutrons and X-ray scattering (SANS and SAXS) to extract the chemically resolved kinetics of room temperature clustering in these alloys, which we completed with differential scanning calorimetry (DSC) and micro-hardness measurements. The comparison of the clustering behaviours of each subsystem allowed us to highlight the paramount role of Mg as a trigger for diffusion and clustering. Indeed, while a strong natural ageing was observed in the Al-Cu-Mg alloy, virtually none was shown for Al-Cu-Li. A very slight addition of Mg (0.4%) to this system, however, drastically changed the situation to a rapid formation of essentially Cu-rich hardening clusters, Mg only joining them later in the reaction. This diffusion enabling effect of Mg is discussed in terms of diffusion mechanism and complex interactions with the quenched-in vacancies.

cond-mat.mtrl-sci↗

arXiv2018

Segregation assisted grain boundary precipitation in a model Al-Zn-Mg-Cu alloy

Understanding the composition evolution of grain boundaries and grain boundary precipitation at near-atomic scale in aluminum alloys is crucial to tailor mechanical properties and to increase resistance to corrosion and stress corrosion cracking. Here, we elucidate the sequence of precipitation on grain boundaries in comparison to the bulk in a model Al-Zn-Mg-Cu alloy. We investigate the material from the solution heat treated state (475{\textdegree}C), through the very early stages of aging to the peak aged state at 120{\textdegree}C and further into the overaged regime at 180{\textdegree}C. The process starts with solute enrichment on grain boundaries due to equilibrium segregation accompanied by solute depletion in their vicinity, the formation of Guinier--Preston (GP) zones in the solute-enriched grain boundary regions, and GP zones growth and transformation. The equilibrium segregation of solutes to grain boundaries during aging accelerates this sequence compared to the bulk. Analysis of the ~10 nm wide precipitate-free zones (PFZs) adjacent to the solute-enriched grain boundaries 2 shows that the depletion zones are determined by (i) interface equilibrium segregation; (ii) formation and coarsening of the grain boundary precipitates and (iii) the diffusion range of solutes in the matrix. In addition, we quantify the difference in kinetics between grain boundary and bulk precipitation. The precipitation kinetics, as observed in terms of volume fraction, average radius, and number density, is almost identical next to the depletion zone in the bulk and far inside the bulk grain remote from any grain boundary influence. This observation shows that the region influenced by the grain boundaries does not extend beyond the PFZs.

cond-mat.mtrl-sci↗

arXiv2018

Parameter free quantitative analysis of atom probe data by correlation functions: Application to the precipitation in Al-Zn-Mg-Cu

Atom probe tomography enables precise quantification of the composition of second phase particles from their early stages, leading to improved understanding of the thermodynamic and kinetic mechanisms of phase formation and quantify structure-property relationships. Here we demonstrate how approaches developed for small-angle scattering can be adapted to atom probe tomography. By exploiting nearest-neighbor distributions and radial distribution function, we introduce a parameter free methodology to efficiently extract information such as particle size, composition, volume fraction, number density and inter-particle distance. We demonstrate the strength of this approach in the analysis of a precipitation-hardened model Al-Zn-Mg-Cu high-strength lightweight alloy.

cond-mat.mtrl-sci↗

arXiv2018

High throughput evaluation of the effect of Mg concentration on natural ageing of Al-Cu-Li-(Mg) alloys

The effect of Mg content on the natural ageing of Al-Cu-Li-(Mg) alloys has been investigated on a compositionally graded material made by linear friction welding, allowing to probe Mg contents between 0 and 0.4 at.%. High throughput time-and space-resolved characterization of natural ageing kinetics has been achieved using small-angle X-ray scattering, supplemented by differential scanning calorimetry. Natural ageing results mainly in the formation of Cu-rich clusters whose characteristics strongly depend on the presence of Mg. Larger precipitates of 2 nm size also form to a lesser extent above a Mg concentration of 0.1 at.%.

cond-mat.mtrl-sci↗

arXiv2016

Reflections on the projection of ions in atom probe tomography

There are two main projections used to transform, and reconstruct, field ion micrographs or atom probe tomography data into atomic coordinates at the specimen surface and, subsequently, in three-dimensions. In this article, we present a perspective on the strength of the azimuthal equidistant projection in comparison to the more widely used and well-established point-projection(or pseudo-stereographic projection), which underpins data reconstruction in most software packages currently in use across the community. After an overview of the reconstruction methodology, we demonstrate that the azimuthal equidistant is more robust with regards to errors on the parameters used to perform the reconstruction and is therefore more likely to yield more accurate tomographic reconstructions.

physics.ins-det↗