The association of hydrogen with nanometre bubbles of helium implanted into zirconium

Electron energy-loss spectroscopy (EELS) is used to investigate the association of hydrogen with helium bubbles in zirconium. Conventional EELS data yield a signal at 13.5 eV (similar to the hydrogen K-edge, 13 eV), which is spatially distributed around the peripheries of bubbles and may correlate with the concentration of hydrogen/deuterium in the material. Ultra-high energy resolution EELS yields a signal at 148.6 meV (comparable to a range of ZrH bonds, 130–156 meV) from a region containing bubbles and no visible hydrides. These signals are interpreted in the context of either bubble surface chemisorption or bubble stress field trapping mechanisms

Quantitative methods for the APT analysis of thermally aged RPV steels.

Atom Probe Tomography (APT) is extensively used for the analysis of RPV steels. However, many different analysis methods and cluster search parameters are used, making comparisons between different datasets difficult. Suitable d(max) and N(min) parameters for the maximum separation method are investigated. In a randomised distribution of solute there is a finite probability that a group of more than N(min) solute ions exists within the d(max) distance. The same is true for experimental datasets from samples which have been thermally aged or irradiated, however these background clusters are not the result of ageing, they are purely statistically random co-incidences. A method is presented for identifying such "background" statistical clusters in real APT data sets, based upon their size and composition, which allows for improved sensitivity to small clusters

Observation of Mn-Ni-Si-rich features in thermally-aged model reactor pressure vessel steels

Atom probe tomography was used to characterise two low-Cu (< 0.04 at. %) model steels after exposure to long-term thermal ageing. Mn-Ni-Si-rich features were observed to form after as little as 20,731 h (∼ 2.4 years) of ageing. The composition of these features were compared to those predicted by thermodynamic models and the similarities and differences are discussed

Improving the quantification of deuterium in zirconium alloy atom probe tomography data using existing analysis methods

Zirconium alloys are common fuel claddings in nuclear fission reactors and are susceptible to the effects of hydrogen embrittlement. There is a need to be able to detect and image hydrogen at the atomic scale to gain the experimental evidence necessary to fully understand hydrogen embrittlement. Through the use of deuterium tracers, atom probe tomography (APT) is able to detect and spatially locate hydrogen at the atomic scale. Previous works have highlighted issues with quantifying deuterium concentrations using APT due to complex peak overlaps in the mass-to-charge-state ratio spectrum between molecular hydrogen and deuterium (H2 and D). In this work, we use new methods to analyze historic and simulated atom probe data, by applying currently available data analysis tools, to optimize solving peak overlaps to improve the quantification of deuterium. This method has been applied to literature data to quantify the deuterium concentrations in a concentration line profile across an α-Zr/deuteride interface

Comparing the consistency of atom probe tomography measurements of small-scale segregation and clustering between the LEAP 3000 and LEAP 5000 instruments.

The local electrode atom probe (LEAP) has become the primary instrument used for atom probe tomography measurements. Recent advances in detector and laser design, together with updated hit detection algorithms, have been incorporated into the latest LEAP 5000 instrument, but the implications of these changes on measurements, particularly the size and chemistry of small clusters and elemental segregations, have not been explored. In this study, we compare data sets from a variety of materials with small-scale chemical heterogeneity using both a LEAP 3000 instrument with 37% detector efficiency and a 532-nm green laser and a new LEAP 5000 instrument with a manufacturer estimated increase to 52% detector efficiency, and a 355-nm ultraviolet laser. In general, it was found that the number of atoms within small clusters or surface segregation increased in the LEAP 5000, as would be expected by the reported increase in detector efficiency from the LEAP 3000 architecture, but subtle differences in chemistry were observed which are attributed to changes in the way multiple hit detection is calculated using the LEAP 5000

On the Use of Density-Based Algorithms for the Analysis of Solute Clustering in Atom Probe Tomography Data

International audienc

On the use of density-based algorithms for the analysis of solute clustering in atom probe tomography data

Because atom probe tomography (APT) provides three-dimensional reconstructions of small volumes by resolving atomic chemical identities and positions, it is uniquely suited to analyze solute clustering phenomena in materials. A number of approaches have been developed to extract clustering information from the 3D reconstructed dataset, and numerous reports can be found applying these methods to a wide variety of materials questions. However, results from clustering analyses can differ significantly from one report to another, even when performed on similar microstructures, raising questions about the reliability of APT to quantitatively describe solute clustering. In addition, analysis details are often not provided, preventing independent confirmation of the results. With the number of APT research groups growing quickly, the APT community recognizes the need for educating new users about common methods and artefacts, and for developing analysis and data reporting protocols that address issues of reproducibility, errors, and variability. To this end, a round robin experiment was organized among ten different international institutions. The goal is to provide a consistent framework for the analysis of irradiated stainless steels using APT. Through the development of more reliable and reproducible data analysis and through communication, this project also aims to advance the understanding between irradiated microstructure and materials performance by providing more complete quantitative microstructural input for modeling. The results, methods, and findings of this round robin will also apply to other clustering phenomena studied using APT, beyond the theme of radiation damage