Papers by Keyword: Atom Probe Tomography

Abstract: We studied three series of Z-phase strengthened steels using scanning electron microscopy, transmission electron microscopy, and atom probe tomography to reveal the detailed microstructure of these steels. In particular, the phase transformation from M(C,N) to Z-phase (CrMN) was studied. Carbon content in the steels is the governing factor in this transformation. The impact toughness of some test alloys was rather low. This is attributed to the formation of a continuous W-rich film along prior austenite grain boundaries. Cu and C addition to the test alloys changed Laves phase morphology to discrete precipitates and improved toughness dramatically. BN particles were found in some steels. Formation of BN is directly linked to the B concentration in the steels.

Abstract: Two examples of precipitation studies (in Al-Li-Cu and Al-Li-Mg alloys) are shown to demonstrate the complementarity of atom probe tomography, small-angle-scattering and differential scanning calorimetry for precipitation studies. It will be used to unravel an unexpected two-step precipitation behavior of T₁ in Al-Li-Cu and to ascertain precipitates size in Al-Li-Mg. through a model free comparison between atom probe and SAXS.

Abstract: The relationship between the cluster morphology formed during natural or artificial aging and the paint-bake hardening response in an Al-0.62Mg-0.93Si (mass%) alloy have been investigated using atom probe tomography (APT). Increasing the subsequent aging time at 170 °C causes a gradual increase in hardness in the artificially aged materials, while the retardation period of the hardness increase appears in the naturally aged materials at the early stage of aging. The statistically-proved records in the APT analysis have shown that the artificially aged materials have some large clusters. It is revealed that the hardening at the early stage of the subsequent aging at 170 °C is not promoted in the long-time naturally aged material although the number density of small clusters increases approximately 1.3 times by prolonged natural aging.Hence, we believe that the small clusters are hard to transform continuously into the β'' phase during aging at 170 °C. As for the naturally aged materials, the long-time aging leads to a significant drop in hardness at the early stage of aging at 170 °C. It is speculated that the Mg-Si mixed clusters formed after long-time natural aging can be reversed during the subsequent heat treatment.

Abstract: Cooling of age-hardening Al-alloys after solution annealing is a critical step with respect to distortion and residual stresses. In order to predict their extent by simulation models, the mechanical behaviour must be known in a wide range of conditions and compositions. Therefore, experimental data is needed both for calibration and validation of the mechanical model. It is known for Al-Mg-Si alloys that supersaturation of the solid solution leads to a significant increase of strength during cooling. In order to understand the influence of single alloying elements on the strengthening effect, the mechanical properties of different binary alloys are investigated experimentally. The precipitation behaviour during cooling was investigated by Differential Scanning Calorimetry in a wide cooling rate range. A methodology to determine the degree of supersaturation of the solid solution based on the calorimetric results is presented. This approach is compared to atom probe tomography data. The mechanical behaviour of the alloys after various heat treatments was analysed by mechanical tests performed in a quenching and deformation dilatometer. Flow curves with high resolution at small strains (< 3 %) were measured at different temperatures. The results of the different experimental techniques are discussed in comparison and with respect to their testing limitations.

Abstract: We have investigated the strain-hardening mechanisms across the relevant scales in a Fe-22Mn-0.6C (wt.%) twinning induced plasticity steel by multi-scale microstructure characterization. The approach makes use of electron microscopy techniques such as electron channeling contrast imaging (ECCI) to characterize microstructure features at the micro/nanoscale, and atomic-scale investigations of partitioning behavior across interfaces and solid solution/clustering effects by atom probe tomography (APT). The contribution of most relevant microstructure features to strain hardening is analyzed.

Abstract: Deviations from the Fickian-laws of diffusion in the case of concentration dependent diffusion coefficients and high composition gradients gain more and more acceptance nowadays. The cause of this phenomenon is the finite permeability of the atomic layers, or in other words “interface control”. The consequences are wide-spreading e.g. linear diffusion kinetics, deviations in the nucleation behavior of reaction products and kinetically determined interface shape in miscible alloys. Furthermore, if the original chemical interface is broader than the optimum width, even a sharpening of the interface by diffusion can be observed. Previous experiments proving these effects used more or less ideal specimens (e.g. single crystalline or amorphous samples with very flat interfaces) and some doubts can be raised whether these effects can be observed in a realistic specimen with a more complex grain structure. In this talk we will present the results of atom probe measurements on sputter deposited Ni/Cu multilayers (containing surface roughness, lattice defects, etc.). Samples with sharp and smeared Ni/Cu interfaces were produced and later annealed. We found an asymmetry on the interface width in the as-prepared specimens depending on the stacking order. After annealing this asymmetry vanished and remarkably the Cu/Ni interface sharpened by diffusion. After short diffusion time, the interface width became independent on the sample origin (sharp or smeared interface) proving the kinetic control of the interface. Atom probe tomography also allows the direct, local investigation of the grain boundary diffusion in any single grain boundaries. Surprisingly the best description of the shortcut transport can be achieved by assuming a concentration-independent grain boundary diffusion coefficient.

Abstract: Two steels, ferritic, high strength with interphase precipitation and nanobainitic, were used to show the advances in and application of atom probe. The coexistence of the nanoscale, interphase Nb-Mo-C clusters and stoichiometric MC nanoparticles was found in the high strength steel after thermomechanical processing. Moreover, the segregation of carbon at different heterogeneous sites such as grain boundary that reduces the solute element available for fine precipitation was observed. The APT study of the solutes redistribution between the retained austenite and bainitic ferrite in the nanobainitic steel revealed: (i) the presence of two types of the retained austenite with higher and lower carbon content and (ii) segregation of carbon at the local defects such as dislocations in the bainitic ferrite during the isothermal hold.

Abstract: Post-irradiation annealing (PIA) behavior of irradiation-induced microstructural changes and hardening of two kind of A533B (first generation (1^stGENS: 0.16 wt.% Cu) and second generation (2^ndGENS: 0.04 wt.% Cu)) steels after neutron-irradiation of 3.9 × 10¹⁹ n cm^–2 at 290 °C has been studied by positron annihilation spectroscopy, atom probe tomography and Vickers microhardness measurements. In the 1^stGENS, clear two recovery stages are observed: (i) as-irradiated state to 450 °C and (ii) 450 to 600 °C. The first stage is due to annealing out of the most of irradiation-induced vacancy-related defects (VRDs), and the second stage corresponds to dissolving irradiation-induced Cu-rich solute nano-clusters (CRSCs). The experimental hardening is almost twice of the hardening due to the CRSCs estimated by Russell-Brown model below 350 °C, but almost the same as the estimation from 400 to 550 °C. In the 2^ndGENS, the VRDs and non-Cu-rich solute nano-clusters (NCRSCs) recover at 450 °C. No CRSC has been formed even in all the annealing process. The experimental hardening is almost twice of the hardening estimated due to the NCRSCs by Russell-Brown model below 400 °C.

Abstract: Nanoscale systems show a wide variety of physical properties that cannot be observed in the bulk. Using atom probe tomography, it is possible to study nanostructured materials with almost atomic resolution in all three dimensions. In this article, we will present a short review of the latest atom-probe measurements carried out at University of Münster with particular focus on diffusion and segregation measurements in triple junctions and interface analysis.

Abstract: With the development of nanotechnologies, the number of industrial processes dealing with the production of nanostructures or nanoobjects is in constant progress (microelectronics, metallurgy). Thus, knowledge of atom mobility and the understanding of atom redistribution in nanoobjects and during their fabrication have become subjects of increasing importance, since they are key parameters to control nanofabrication. Especially, todays materials can be both composed of nanoobjects as clusters or decorated defects, and contain a large number of interfaces as in nanometer-thick film stacking and buried nanowires or nanoislands. Atom redistribution in this type of materials is quite complex due to the combination of different effects, such as composition and stress, and is still not very well known due to experimental issues. For example, it has been shown that atomic transport in nanocrystalline layers can be several orders of magnitude faster than in microcrystalline layers, though the reason for this mobility increase is still under debate. Effective diffusion in nanocrystalline layers is expected to be highly dependent on interface and grain boundary (GB) diffusion, as well as triple junction diffusion. However, experimental measurements of diffusion coefficients in nanograins, nanograin boundaries, triple junctions, and interfaces, as well as investigations concerning diffusion mechanisms, and defect formation and mobility in these different diffusion paths are today still needed, in order to give a complete picture of nanodiffusion and nanosize effects upon atom transport. In this paper, we present recent studies dealing with diffusion in nanocrystalline materials using original simulations combined with usual 1D composition profile measurements, or using the particular abilities of atom probe tomography (APT) to experimentally characterize interfaces. We present techniques allowing for the simultaneous measurement of grain and GB diffusion coefficients in polycrystals, as well as the measurement of nanograin lattice diffusion and triple junction diffusion. We also show that laser-assisted APT microscopy is the ideal tool to study interface diffusion and nanodiffusion in nanostructures, since it allows the determination of 1D, 2D and 3D atomic distributions that can be analyzed using diffusion analytical solutions or numerical simulation.