Point excess solute: A new metric for quantifying solute segregation in atom probe tomography datasets including application to naturally aged solute clusters in Al-Mg-Si-(Cu) alloys

Accurate, repeatable and quantitative analysis of nanoscale solute clustering in atom probe tomography (APT) datasets is a complex challenge which is made more difficult by the positional uncertainty and lack of absolute resolution inherent to the technique. In this work a new method, the point excess solute, is introduced for quantifying solute segregation in datasets with limited spatial resolution. This new method is based on measuring the matrix concentration using a dataset sampling method. We show the new method can accurately reproduce the values expected from synthetic datasets a priori and when the dataset spatial resolution and or phase contrast is too low for accurate quantification this is observable. The method is then applied to naturally aged solute clusters in the Al-Mg-Si-Cu system. Datasets were collected with a range of natural ageing times from 8 min to 76 weeks. The formation of the solute clusters is shown to be unaffected by the Cu content of the alloy

Effect of microsegregation and heat treatment on localised γ and γ’ compositions in single crystal Ni-based superalloys

The present work investigates the impact of residual segregation on the underlying microstructure of a 3rd generation single crystal, nickel-based superalloy to understand potential variation in mechanical behaviour between dendrite cores and interdendritic regions. Despite the applied heat-treatments, chemical variation between dendrite cores and interdendritic regions persisted particularly for elements Re, Nb and Ta. Atom probe tomography (APT) was utilized for its nanoscale capability to map site-specific chemical changes in the γ matrix, γ’ precipitates and across the γ/γ’ interface. Greater interfacial segregation of Re, matched by a corresponding depletion of Ni were observed within dendrite cores, with the extent found to increase following heat treatment. Differences in lattice parameters between dendrite cores and interdendritic regions were identified, with larger lattice misfits associated with interdendritic regions

Precipitation of the ordered α2 phase in a near-α titanium alloy

Precipitate evolution in a near-α alloy was studied using transmission electron microscopy (TEM) and correlative atom probe tomography (APT) after ageing at 550-700 for times up to 28 days. It is found that precipitation occurs much faster and is more prolific in samples heat treated at higher temperatures. Particles were spherical after ageing at 550 °C, while after ageing at 700 °C they become ellipsoids with the major axis lying close to the [0001] direction. At longer ageing times, the α2 precipitates were found to contain greater amounts of Sn + Si, indicating that Sn and Si are stronger Ti3(Al,Sn,Si) formers than Al

Point excess solute: A new metric for quantifying solute segregation in atom probe tomography datasets including application to naturally aged solute clusters in Al-Mg-Si-(Cu) alloys

Data availability: The raw and processed data required to reproduce these findings cannot be shared at this time due to legal reasons.Supplementary data are available online at: https://www.sciencedirect.com/science/article/pii/S1044580323007611#s0060 .Copyright © 2023 The Authors. Accurate, repeatable and quantitative analysis of nanoscale solute clustering in atom probe tomography (APT) datasets is a complex challenge which is made more difficult by the positional uncertainty and lack of absolute resolution inherent to the technique. In this work a new method, the point excess solute, is introduced for quantifying solute segregation in datasets with limited spatial resolution. This new method is based on measuring the matrix concentration using a dataset sampling method. We show the new method can accurately reproduce the values expected from synthetic datasets a priori and when the dataset spatial resolution and or phase contrast is too low for accurate quantification this is observable. The method is then applied to naturally aged solute clusters in the Al-Mg-Si-Cu system. Datasets were collected with a range of natural ageing times from 8 min to 76 weeks. The formation of the solute clusters is shown to be unaffected by the Cu content of the alloy.The authors would like to thank Constellium for providing the materials and financially supporting this research alongside the Engineering and Physical Science Research Council (EPSRC) through studentship 1922133. The authors are grateful to EPSRC for funding of the LEAP 5000XR for the UK National Atom Probe Facility through grant EP/M022803/1

The effect of phase chemistry on the extent of strengthening mechanisms in model Ni-Cr-Al-Ti-Mo based superalloys

The exceptional mechanical properties of polycrystalline nickel-based superalloys arise through various concurrent strengthening mechanisms. Whilst these mechanisms are generally understood, consensus has yet to be established on the precise contribution of each to the overall alloy strength. Furthermore, changes in alloy chemistry influence several different mechanisms, making the assessment of individual alloying elements complex. In this study, a series of model quinary Ni-based superalloys has been investigated to systematically study the effect of varying Mo content on the contributing strengthening mechanisms. Using microstructural data, the yield strength was modelled by summing the individual effects of solid solution in both the γ and γ ' phases, coherency, grain boundary and precipitation strengthening. The total predicted yield stress increased with Mo content despite the diminishing contribution of precipitation strengthening. It is shown that solid solution strengthening of the ordered γ' precipitate phase is a key contributor to the overall strength, and that variations in composition between the tertiary and secondary γ ' lead to significant changes in mechanical properties that should be accounted for in models of alloy strength.Funding was provided by the EPSRC/Rolls-Royce Strategic Partnership under EP/M005607/1 and EP/H022309/1. The Oxford Atom Probe facility was funded by the EPSRC under EP/M022803/1. E. I. Galindo-Nava would like to acknowledge the Royal Academy of Engineering for his fellowship funding. Neutron diffraction beam time was supported through the Canadian Neutron Beam Centre under Experiment number 1258

Indium clustering in a -plane InGaN quantum wells as evidenced by atom probe tomography

Atom probe tomography (APT) has been used to characterize the distribution of In atoms within non-polar a-plane InGaN quantum wells (QWs) grown on a GaN pseudo-substrate produced using epitaxial lateral overgrowth. Application of the focused ion beam microscope enabled APT needles to be prepared from the low defect density regions of the grown sample. A complementary analysis was also undertaken on QWs having comparable In contents grown on polar c-plane sample pseudo-substrates. Both frequency distribution and modified nearest neighbor analyses indicate a statistically non-randomized In distribution in the a-plane QWs, but a random distribution in the c-plane QWs. This work not only provides insights into the structure of non-polar a-plane QWs but also shows that APT is capable of detecting as-grown nanoscale clustering in InGaN and thus validates the reliability of earlier APT analyses of the In distribution in c-plane InGaN QWs which show no such clustering.The European Research Council has provided financial support under the European Community’s Seventh Framework Programme (FP7/2007-2013)/ERC Grant Agreement No. 279361 (MACONS). This work was also funded in part by the EPSRC (Grant Nos. EP/H047816/1, EP/H0495331 and EP/J003603/1).This is the author accepted manuscript. The final version is available via AIP at http://scitation.aip.org/content/aip/journal/apl/106/7/10.1063/1.4909514

An Atom Probe Tomography study of site preference and partitioning in a nickel-based superalloy

Atom Probe Tomography (APT) has been utilised for an in-depth examination of the commercial polycrystalline Ni-based superalloy RR1000, assessing compositions of the primary, secondary and tertiary γ′ phases. Clear differences in the phase chemistries are noted, particularly for the tertiary γ′ to which much of the alloy strength is attributed. Trace amounts of Hf are found to segregate strongly to the primary and secondary γ′ phases, but also exhibit an extended diffusion profile across the γ-γ′ interface up to 80 nm wide. Ti, Al and Mo demonstrate similar, yet not as pronounced diffusion profiles, indicating assumed phase chemistries may not be representative of those regions adjacent to the γ-γ′ interface. Within γ′, unique element site-occupancy preferences for this alloy were identified. Finally, the grain boundary chemistry across a γ-γ interface and that of an intragranular boride were analysed, identifying the latter as a mixed M5B3 boride rich in Mo and Cr. These demonstrate further the depth of information on Ni-alloys accessible by APT, while the overall implications of results in comparison with other in-service/model alloys are also discussed

Partitioning of Ti and Kinetic Growth Predictions on the Thermally Grown Chromia Scale of a Polycrystalline Nickel-Based Superalloy

Titanium is commonly added to nickel superalloys but has a well-documented detrimental effect on oxidation resistance. The present work constitutes the first atomistic-scale quantitative measurements of grain boundary and bulk compositions in the oxide scale of a current generation polycrystalline nickel superalloy performed through atom probe tomography. Titanium was found to be particularly detrimental to oxide scale growth through grain boundary diffusion.The authors would like to thank Rolls-Royce plc for the materials provision. The Oxford Atom Probe facility is funded by EPSRC (EP/M022803/1). This work was sponsored by the Rolls-Royce—EPSRC strategic partnership grant EP/M005607/1. Dr Galindo-Nava thanks the RAEng for their support by means of a research fellowship

On the microtwinning mechanism in a single crystal superalloy

© 2017 Acta Materialia Inc. The contribution of a microtwinning mechanism to the creep deformation behaviour of single crystal superalloy MD2 is studied. Microtwinning is prevalent for uniaxial loading along 〈011〉 at 800°C for the stress range 625 to 675 MPa and 825°C for 625 MPa. Using quantitative stereology, the twin fraction and twin thickness are estimated; this allows the accumulated creep strain to be recovered, in turn supporting the role of the microtwinning mode in conferring deformation. Atom probe tomography confirms the segregation of Cr and Co at the twin/parent interface, consistent with the lowering of the stacking fault energy needed to support twin lengthening and thickening. A model for diffusion-controlled growth of twins is proposed and it is used to recover the measured creep strain rate. The work provides the basis for a thermo-mechanical constitutive model of deformation consistent with the microtwinning mechanism