R. Lardé

Depth resolution function of the laser assisted tomographic atom probe in the investigation of semiconductors

The investigation of boron delta layers by tomographic atom probe (3DAP) is used to demonstrate that a depth profiling resolution of 0.9 nm (full width at half maximum) can be achieved. Results are compared with measurements provided by secondary ion mass spectrometry. The steepness is found to be below 1 nm/decade. In addition, silicon atomic planes are resolved in the real space demonstrating an in-depth spatial resolution of the 3DAP below 0.2 nm.

Evidence of superparamagnetic co clusters in pulsed laser deposition-grown Zn0.9Co0.1O thin films using atom probe tomography.

Nanosized Co clusters (of about 3 nm size) were unambiguously identified in Co-doped ZnO thin films by atom probe tomography. These clusters are directly correlated to the superparamagnetic relaxation observed by ZFC/FC magnetization measurements. These analyses provide strong evidence that the room-temperature ferromagnetism observed in the magnetization curves cannot be attributed to the observed Co clusters. Because there is no experimental evidence of the presence of other secondary phases, our results reinforce the assumption of a defect-induced ferromagnetism in Co-doped ZnO diluted magnetic semiconductors.

Si nanoparticles in SiO2 An atomic scale observation for optimization of optical devices

Three-dimensional imaging of silicon nanoclusters array in silicon-rich silicon oxide layers was evidenced and studied. The atom probe tomography technique allows to give the composition of the nanoclusters and the composition of the interface with the silica matrix. These results give new insights for the understanding of the properties of Si-based photonic devices.

Boron distribution in the core of Si nanowire grown by chemical vapor deposition

The boron dopant distribution in Si nanowires grown by the Au-catalyzed chemical vapor deposition is characterized by laser-assisted atom probe tomography. A convenient and an effective method for performing the atom probe tomography of an individual nanowire is developed. Using this technique, we demonstrate that when Si nanowires are doped with boron at high silane partial pressure, the radial distribution of boron atoms is rather inhomogeneous. Much more boron atoms incorporate at the periphery than in the center, with the concentration increasing by an order of magnitude as the distance from the nanowire axis increases from zero to only 15 nm. A theoretical model is presented that is capable of describing the observed spatial inhomogeneity of boron dopant. We also consider different kinetic pathways of boron incorporation and discuss the values of diffusion length and diffusion coefficients obtained by fitting the experimental data.

A structural investigation of SmCo5/Fe nanostructured alloys obtained by high-energy ball milling and subsequent annealing

SmCo5/Fe nanostructured alloys with 20 wt% Fe, obtained by high-energy ball milling of SmCo5 and Fe powders, were investigated by 57Fe Mossbauer spectrometry, x-ray diffraction and tomographic atom probe. The Mossbauer analysis reveals that during the first stages of milling, an interdiffusion of Co and Fe occurs, leading both to the formation of α-Fe(Co) regions in α-Fe and to the introduction of Fe in SmCo5 regions. Annealing at temperatures up to 650 °C for 0.5 h promotes interdiffusion further leading to the formation of a unique α-Fe(Co) phase and a Fe-richer Sm(Co,Fe)5 phase. The Co/Fe interdiffusion is confirmed by tomographic atom probe analysis. The data are discussed and compared with the results of previous magnetic measurements.

Growth of Si nanowires on micropillars for the study of their dopant distribution by atom probe tomography

This article reports on the growth of Au islands on the Si(111) surface as a function of the Au evaporation rate and the temperature of the surface in ultrahigh vacuum. By controlling the density of the Au islands and their size, it is possible to subsequently grow single vertically oriented Si nanowires on top of (111)-oriented silicon micropillar and analyze their chemical composition at the atomic scale with the femtosecond laser assisted tomographic atom probe. Three-dimensional images of the atom distribution in the nanowire, in particular, the distribution of boron impurities, are obtained and compared to the intended impurity concentration.

Investigation at the atomic scale of the Co spatial distribution in Zn(Co)O magnetic semiconductor oxide

A sputtered Zn0.95Co0.05O layer was chemically analyzed at the atomic scale in order to provide an accurate image of the distribution of Co atoms in the ZnO matrix. The investigation of the magnetic properties shows that the as-deposited Zn0.95Co0.05O is ferromagnetic at room temperature. Atom probe tomography reveals a homogeneous distribution of all chemical species in the layer and the absence of any Co clustering. This result proves that the ferromagnetic properties of this magnetic semiconductor cannot be attributed to a secondary phase or to metallic Co precipitates within the layer.

Evidence of atomic-scale arsenic clustering in highly doped silicon

Low temperature (675 °C) epitaxial in situ doped Si layers (As, 1.5 at. %) were analyzed by atom probe tomography (APT) to study clustering in a highly arsenic-doped silicon layer. The spatial distribution of As atoms in this layer was obtained by APT, and the distance distribution between first nearest neighbors between As atoms was studied. The result shows that the distribution of As atoms is nonhomogeneous, indicating clustering. Those clusters, homogeneously distributed in the volume, are found to be very small (a few atoms) with a high number density and contain more than 60% of the total number of As atoms.

Nanoscale evidence of erbium clustering in Er-doped silicon-rich silica

Photoluminescence spectroscopy and atom probe tomography were used to explore the optical activity and microstructure of Er3+-doped Si-rich SiO2 thin films fabricated by radio-frequency magnetron sputtering. The effect of post-fabrication annealing treatment on the properties of the films was investigated. The evolution of the nanoscale structure upon an annealing treatment was found to control the interrelation between the radiative recombination of the carriers via Si clusters and via 4f shell transitions in Er3+ ions. The most efficient 1.53-μ m Er3+ photoluminescence was observed from the films submitted to low-temperature treatment ranging from 600°C to 900°C. An annealing treatment at 1,100°C, used often to form Si nanocrystallites, favors an intense emission in visible spectral range with the maximum peak at about 740 nm. Along with this, a drastic decrease of 1.53-μ m Er3+ photoluminescence emission was detected. The atom probe results demonstrated that the clustering of Er3+ ions upon such high-temperature annealing treatment was the main reason. The diffusion parameters of Si and Er3+ ions as well as a chemical composition of different clusters were also obtained. The films annealed at 1,100°C contain pure spherical Si nanocrystallites, ErSi3O6 clusters, and free Er3+ ions embedded in SiO2 host. The mean size and the density of Si nanocrystallites were found to be 1.3± 0.3 nm and (3.1± 0.2)×1018 Si nanocrystallites·cm−3, respectively. The density of ErSi3O6 clusters was estimated to be (2.0± 0.2)×1018 clusters·cm−3, keeping about 30% of the total Er3+ amount. These Er-rich clusters had a mean radius of about 1.5 nm and demonstrated preferable formation in the vicinity of Si nanocrystallites.

Structural analysis of a (Pt/Co)3/IrMn multilayer: Investigation of sub-nanometric layers by tomographic atom probe

The structure of a Ta3 nm/[(Pt2 nm/Co0.4 nm)3/IrMn7 nm]7/Pt10 nm multilayer exhibiting perpendicular exchange bias has been investigated by x-ray reflectometry and laser-assisted tomographic atom probe (LATAP). A strong intermixing at the Co/IrMn interface is pointed out by x-ray reflectometry, this interface being more diffuse than the IrMn/Pt interface. A direct observation of this intermixing at the atomic scale is obtained thanks to the LATAP in real space. The three-dimensional reconstructions reveal the atomic planes in the Pt layers and the Pt–Co intermixing in the (Pt/Co)3 multilayer. The analysis of the concentration profiles allows to determine the chemical composition of the Co subnanometric layers; thus providing for the first time an accurate structural characterization of such layers leading to an estimation of their thickness, roughness, atomic concentration and width of their interfaces.