F. Vurpillot

Trajectory overlaps and local magnification in three-dimensional atom probe

Local magnification effects related to the presence of a second phase in three-dimensional atom probe have been investigated using a simulation of ion trajectories from the analyzed sample surface. Spherical precipitates containing only B atoms embedded in pure A solid solution were considered. The magnification was found to vary drastically from 0.5 to 2.0 times when the evaporation field of B (EB) was varied from 1.15 EA to 0.85 EA. The trajectories were found to overlap over distances close to 1 nm only when the reduced evaporation field (eB=EB/EA) is outside of a gap ranging from 0.9 to 1.1. Simulations indicate that the “measured” composition in the inner core of precipitates is not biased in this gap. This is also the case for particles which have a diameter larger than a critical value of 2 nm.

Design of a femtosecond laser assisted tomographic atom probe

A tomographic atom probe (TAP) in which the atoms are field evaporated by means of femtosecond laser pulses has been designed. It is shown that the field evaporation is assisted by the laser field enhanced by the subwavelength dimensions of the specimen without any significant heating of the specimen. In addition, as compared with the conventional TAP, due to the very short duration of laser pulses, no spread in the energy of emitted ions is observed, leading to a very high mass resolution in a straight TAP in a wide angle configuration. At last, laser pulses can be used to bring the intense electric field required for the field evaporation on poor conductive materials such as intrinsic Si at low temperature. In this article, the performance of the laser TAP is described and illustrated through the investigation of metals, oxides, and silicon materials.

Design of a delay-line position-sensitive detector with improved performance

A delay-line position-sensitive detector with improved performance is presented. In this device, timing is carried out by means of fast digitizer boards. The use of dedicated signal processing procedures leads to a timing accuracy of 70 ps and a dead-time below 1.5 ns. As a result, the spatial resolving power of this detector is close to 1 mm leading to a high multihit capability. A temporary detector has been designed in which the delay-line anode is combined with a phosphor screen allowing additional positioning to be made via a charge-coupled device camera. This additional positioning is used to unambiguously quantify performances in terms of spatial resolution and multihit capabilities. A three-dimensional atom probe analysis of a material containing low evaporation field phases is used to demonstrate the capabilities of this detector.

Structural analyses in three-dimensional atom probe: a Fourier transform approach

The three‐dimensional atom probe (3DAP) technique gives the elemental identities and the position of atoms within the small volume analysed (on the order of 10 × 10 × 100 nm3). The large number of atoms collected (up to two million) and the excellent spatial resolution of this instrument allows the observation of some crystallographic features of phases chemically identified. This paper shows that the application of a discrete Fourier transform algorithm to a 3DAP dataset provides information that is not easily accessible in real space. The derivation of the mean size of particles from Fourier intensities is an example. Using 3D ‘dark‐field’ imaging, single ordered grains were isolated from the disordered matrix of a ternary alloy. Moreover, the intrinsic spatial resolution of the instrument was evaluated by this method for pure metal; the resolution reaches 0.2 nm laterally and 0.06 nm in depth. This excellent resolution is shown to be sufficient to give access to the crystalline lattice. The use of image filtering in the reciprocal space enables for atomic columns to be imaged the first time from 3DAP data.

Modeling Image Distortions in 3DAP

A numerical model has been developed to simulate images obtained from the three-dimensional atom probe. This model was used to simulate the artefacts commonly observed in two-phase materials. This model takes into account the dynamic evolution of the atomic-scale shape of the specimen during field evaporation. This article reviews the model and its applications to some specific cases. Local magnification effects were studied as a function of the size, the shape, and the orientation of precipitated phases embedded in the matrix. Small precipitates produce large aberrations in good agreement with experiments. The magnification from such precipitates, as measured from the simulation, is only found to match the theoretical value for mesoscopic scale precipitates (size similar to the specimen size). Orientation effects are also observed in excellent agreement with experiments. The measured thickness of a grain-boundary-segregated film in the simulation is found to decrease with the angle between the normal to the grain boundary and the tip axis. Depth scaling artefacts caused by variation in the evaporation field of atoms in multilayer structures were successfully simulated and again showed good agreement with effects observed experimentally.

Estimation of the tip field enhancement on a field emitter under laser illumination

We report the experimental evidence of controlled field evaporation of atoms from the surface of a tip-like-shape specimen with subwavelength dimensions by means of subpicosecond laser pulses. It is shown that the evaporation is assisted by the intrinsic laser electric field without any significant thermal activation. The single-atom detection sensitivity of the field ion microscope is used to get an accurate measurement of the electric field enhancement factor at the tip apex as a function of the wave polarization. The absence of thermal diffusion of atoms at the tip surface prior to field evaporation, demonstrates the feasibility of a laser assisted three-dimensional atom probe.

A model accounting for spatial overlaps in 3D atom-probe microscopy

The spatial resolution of three-dimensional atom probe is known to be mainly controlled by the aberrations of ion trajectories near the specimen surface. An analytical model accounting for the spatial overlaps that occur near phase interfaces is described. This model makes it possible to correct the apparent composition of small spherical precipitates in order to determine the true composition. The prediction of the overlap rate as a function of the particle size was found in remarkably good agreement with the simulations of ion trajectories that were made. The thickness of the mixed zone around beta precipitates was found to be of 0.3 nm for a normalised evaporation field of beta phase of 0.8. Using simulations, the overlap rate could be parameterised as a function of the apparent atomic density observed in particles. This model has been applied to copper precipitation in FeCu.

An improved reconstruction procedure for the correction of local magnification effects in three‐dimensional atom‐probe

A new 3DAP reconstruction procedure is proposed that accounts for the evaporation field of a secondary phase. It applies the existing cluster selection software to identify the atoms of the second phase and, subsequently, an iterative algorithm to homogenise the volume laterally. This procedure, easily implementable on existing reconstruction software, has been applied successfully on simulated and real 3DAP analyses.

Thermal response of a field emitter subjected to ultra-fast laser illumination

Using an ultra-fast laser assisted atom probe, the temporal evolution of the temperature of a tungsten field emitter subjected to illumination is studied. The combination of pump probe experiments and evaporation rate measurements is used to estimate the duration of field evaporation, the induced peak temperature and the cooling time. The main conclusion of the measurements is that, despite a significant heating of the tip by the laser pulse, the cooling time is anomalously fast, below 0.5 ns. Hence, thermal effects are considered to play a major role in ion emission in contrast to conclusions of our previous works. It is shown that the really fast anomalous cooling rate can only be related to a confined heating zone at the tip apex smaller than the wavelength of the laser.

Reconstructing atom probe data: A review

Atom probe tomography stands out from other materials characterisation techniques mostly due to its capacity to map individual atoms in three-dimensions with high spatial resolution. The methods used to transform raw detector data into a three-dimensional reconstruction have, comparatively to other aspects of the technique, evolved relatively little since their inception more than 15 years ago. However, due to the importance of the fidelity of the data, this topic is currently attracting a lot of interest within the atom probe community. In this review we cover: (1) the main aspects of the image projection, (2) the methods used to build tomographic reconstructions, (3) the intrinsic limitations of these methods, and (4) future potential directions to improve the integrity of atom probe tomograms.