A. Cerezo

Atom probe tomography today

This review aims to describe and illustrate the advances in the application of atom probe tomography that have been made possible by recent developments, particularly in specimen preparation techniques (using dual-beam focused-ion beam instruments) but also of the more routine use of laser pulsing. The combination of these two developments now permits atomic-scale investigation of site-specific regions within engineering alloys (e.g. at grain boundaries and in the vicinity of cracks) and also the atomic-level characterization of interfaces in multilayers, oxide films, and semiconductor materials and devices.

A study on the early-stage decomposition in the Al–Mg–Si–Cu alloy AA6111 by electrical resistivity and three-dimensional atom probe

Electrical resistivity measurements and three-dimensional atom probe (3DAP) analysis were employed to investigate early-stage decomposition of the Al alloy AA6111 in the temperature range 60–180°C where electrical resistivity initially increased with ageing time. 3DAP measurements provided information on the shape, number density and solute content of the precipitates, as well as the solute concentration of the matrix, for the ageing conditions corresponding to the resistivity maxima. Using the 3DAP results, the precipitate size distributions for these ageing conditions were determined in terms of the measured number of solute atoms per precipitate. The number density and the Cu content of the precipitates decreased with increasing temperature, whereas the Mg/Si ratio increased. The size distribution of precipitates at the higher ageing temperatures showed the addition of larger size precipitates to the precipitate population. A modification to Matthiessens law was employed to describe the anomalous resistivity increase by considering the effect of solutes and precipitates on the resistivity evolution. Using the 3DAP results in analysing the resistivity anomaly, it was found that the decrease in the resistivity maxima with increasing temperature was associated with the decrease in the number density of precipitates and not the scattering power of precipitates. The 3DAP results were further used to provide information on the mechanisms of early-stage decomposition and the temperature dependence of the nucleation rate. From this, the nucleation rate appeared to be controlled by the migration of solute atoms, which was assisted by quenched-in vacancies.

Overview: Recent progress in three-dimensional atom probe instruments and applications

Over the last few years there have been significant developments in the field of three-dimensional atom probe (3DAP) analysis. This article reviews some of the technical compromises that have led to different instrument designs and the recent improvements in performance. An instrument has now been developed, based around a novel reflectron configuration combining both energy compensation and focusing elements, that yields a large field of view and very high mass resolution. The use of laser pulsing in the 3DAP, together with developments in specimen preparation methods using a focused ion-beam instrument, have led to a significant widening in the range of materials science problems that can be addressed with the 3DAP. Recent studies of semiconductor materials and devices are described.

High resolution structural characterization of giant magnetoresistance structures containing a nano-oxide layer

The microstructure and chemistry of a current-perpendicular-to-plane giant magnetoresistance structure containing a nano-oxide layer (NOL) have been studied using a combination of high resolution transmission electron microscopy and three-dimensional atom probe analysis. It was found that the morphology of the NOL changes from a planar layer to discrete particles on annealing, indicating the dominance of surface energy on the morphology evolution. Direct evidence was obtained for significant Mn diffusion from the IrMn antiferromagnetic layer and partitioning to the oxide region during annealing.

Partitioning and segregation of trace element Sn in a low-alloy steel

The partitioning of the trace element Sn into Cu-rich precipitates in a low-alloy pressure-vessel steel has been characterized using the three-dimensional atom probe (3DAP) technique. This investigation has revealed for the first time that the trace element Sn, present at only 0.007 at.% in the steel, partitions strongly to both small spherical precipitates (<4 nm in diameter) and to large non-spherical precipitates (largest dimension 10–50 nm) during thermal ageing. Sn was also seen to segregate strongly to the precipitate/matrix interface of a large Cu precipitate and particularly in the region where a dislocation appears to intersect the precipitate. The strong attraction of large solute atoms to special sites probably drives the interfacial segregation of Sn. This is consistent with the observation of stronger segregation of Sn to the interface of large precipitates than to the coherent interface of smaller precipitates.

3DAP Study of Alloy Element Effects on the Tempering of Steel

Tempering of the engineering steel AISI/SAE 4340 in the temperature range 250-600degC for 1 hour and 10 hours was studied. 3D atom probe techniques were used to map the redistribution of all major alloying elements (Si, Cr, Mn, Ni and Mo) between ferrite and carbide phases as a function of temperature and time. Field emission ion microscopy image shows dislocation spiral and grain boundary in the samples studied