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 (εB=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.
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.
Clouds of impurity atoms near line defects are believed to affect the plastic deformation of alloys. Three-dimensional atom probe techniques were used to image these so-called Cottrell atmospheres directly. Ordered iron-aluminum alloys (40 atomic percent aluminum) doped with boron (400 atomic parts per million) were investigated on an atomic scale along the <001> direction. A boron enrichment was observed in the vicinity of an <001> edge dislocation. The enriched region appeared as a three-dimensional pipe 5 nanometers in diameter, tangent to the dislocation line. The dislocation was found to be boron-enriched by a factor of 50 (2 atomic percent) relative to the bulk. The local boron enrichment is accompanied by a strong aluminum depletion of 20 atomic percent.
The early stage of the chromium precipitation in copper was analyzed at the atomic scale by Atom Probe Tomography (APT). Quantitative data about the precipitate size, 3D shape, density, composition and volume fraction were obtained in a Cu-1Cr-0.1Zr (wt.%) commercial alloy aged at 713K. Surprisingly, nanoscaled precipitates exhibit various shapes (spherical, plates and ellipsoid) and contain a large amount of Cu (up to 50%), in contradiction with the equilibrium Cu-Cr phase diagram. APT data also show that some impurities (Fe) may segregate along Cu/Cr interfaces. The concomitant evolution of the precipitate shape and composition as a function of the aging time is discussed. A special emphasis is given on the competition between interfacial and elastic energy and on the role of Fe segregation.
The physical architecture and the performance of a quantitative three-dimensional atom probe recently constructed are described. The development of such an instrument relies on the design of a multi-impact position sensitive detector. The multidetection system that we have developed is based on the use of a 10×10 anode array placed behind a two microchannel plate assembly in a chevron arrangement. The spread of charge between the microchannel plate and the multianode is used to derive the position of ion striking the detector. Spatial coordinates can be calculated for multiple and simultaneous time-of-flight events. The procedure used for the derivation of ion positions from charge measurements is given. Specific experiments were carried out in order to determine the intrinsic spatial resolution of the multidetector. Three-dimensional reconstruction of two-phase materials are provided and illustrate the performance of this new apparatus. The reconstructed images demonstrate that atoms are positioned with a precision of a few tenths of a nanometer. The mass resolution M/ΔM (FWHM) of the apparatus is close to 200.
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