32 research outputs found
An Atom Probe Tomography study of site preference and partitioning in a nickel-based superalloy
A SANS and APT study of precipitate evolution and strengthening in a maraging steel
In this work a combination of the characterisation techniques small angle neutron scattering (SANS) and atom probe tomography (APT) are used to study the precipitation in a maraging steel. Three similar maraging steel alloys were aged at different temperatures and ageing times, and then characterised using SANS, APT and microhardness. The alloys consist of two types of precipitates, namely Laves phase and β-NiAl, the precipitates have different composition and hence precipitate ageing, which makes it complicated to model. The SANS experimental set-up was relatively simple and allowed the precipitate size and fraction of a large number of samples to be measured in a single experiment. The APT results were used for constraining the SANS modelling, particularly the composition, shape and distribution of phases. The characterisation led to the following description of precipitation: NiAl phase reaches coarsening at early stages of ageing and shifts its strength mechanisms from shearing to Orowan looping, which cause the characteristic peak strength; the Laves phase is in growth throughout and its strength contribution increases with ageing time. These observations were shown to be consistent with precipitate evolution and strengthening models, and the work of others. Although, there are some issues with the combination of SANS and APT approach, which are discussed, the methodology provides a valuable tool to understand complex precipitation behaviours
Chromium-based bcc-superalloys strengthened by iron supplements
Chromium alloys are being considered for next-generation concentrated solar power applications operating > 800 °C. Cr offers advantages in melting point, cost, and oxidation resistance. However, improvements in mechanical performance are needed. Here, Cr-based body-centred-cubic (bcc) alloys of the type Cr(Fe)-NiAl are investigated, leading to ‘bcc-superalloys’ comprising a bcc-Cr(Fe) matrix (β) strengthened by ordered-bcc NiAl intermetallic precipitates (β’), with iron additions to tailor the precipitate volume fraction and mechanical properties at high temperatures. Computational design using CALculation of PHAse Diagram (CALPHAD) predicts that Fe increases the solubility of Ni and Al, increasing precipitate volume fraction, which is validated experimentally. Nano-scale, highly-coherent B2-NiAl precipitates with lattice misfit ∼ 0.1% are formed in the Cr(Fe) matrix. The Cr(Fe)-NiAl A2-B2 alloys show remarkably low coarsening rate (∼102 nm3/h at 1000 °C), outperforming ferritic-superalloys, cobalt- and nickel-based superalloys. Low interfacial energies of ∼ 40/20 mJ/m2 at 1000/1200 °C are determined based on the coarsening kinetics. The low coarsening rates are principally attributed to the low solubility of Ni and Al in the Cr matrix. The alloys show high compressive yield strength of ∼320 MPa at 1000 °C. The Fe-modified alloy exhibits resistance to age softening, related to the low coarsening rate as well as the relatively stable Orowan strengthening as a function of precipitate radius. Microstructure tailoring with Fe additions offers a new design route to improve the balance of properties in “Cr-superalloys”, accelerating their development as a new class of high-temperature materials
Microstructural evolution and transmutation in tungsten under ion and neutron irradiation
This study aims to compare the effects of neutron and self-ion irradiation on the mechanical properties and microstructural evolution in W. Neutron irradiation at the HFR reactor to 1.67 dpa at 800 °C resulted in the formation of large Re and Os rich clusters and voids. The post-irradiation composition was measured using APT and verfified against FISPACT modelling. The measured Re and Os concentration was used to create alloys with equivalent concentrations of Re and Os. These alloys were exposed to self-ion irradiation to a peak dose of 1.7 dpa at 800 °C. APT showed that self-ion irradiation leads to the formation of small Os clusters, wheras under neutron irradiation large Re/Os clusters form. Voids are formed by both ion and neutron irradiation, but the voids formed by neutron irradiation are larger. By comparing the behaviour of W-1.4Re and W-1.4Re-0.1Os, suppression of Re cluster formation was observed. Irradiation hardening was measured using nanoindentation and was found to be 2.7 GPa, after neutron irradiation and 1.6 GPa and 0.6 GPa for the self-ion irradiated W-1.4Re and W-1.4Re-0.1Os. The higher hardening is attributed to the barrier strength of large voids and Re/Os clusters that are observed after neutron irradiation
Amorphous-crystalline nanostructured Nd-Fe-B permanent magnets using laser powder bed fusion: Metallurgy and magnetic properties
Laser powder-bed fusion (PBF-LB), a class of additive manufacturing (AM), has attracted wide interest in the production of Nd-Fe-B permanent magnets, benefiting from the minimisation of waste of rare-earth elements and the post-processing requirements. Most research on PBF-LB Nd-Fe-B has focused on reducing defects in printed parts alongside the improvement of the resultant magnetic properties. Detailed analysis of the microstructure that results in permanent magnetic properties is yet to be published. In this research, a combination of high-resolution microstructural investigations was conducted for this purpose. For the first time, an in-depth analysis of the grain structure in terms of morphology, size distribution, and texture is presented and correlated to the permanent magnetic performance. Melt pools showed a hierarchical grain size distribution of primary Nd2Fe14B phase grains with a polygonal morphology and random crystalline alignment, in addition to a small amount of Nd-rich and Nd-lean precipitates in the matrix of the Ti-rich amorphous grain boundaries. The permanent magnetic properties of this material are mainly determined by the nanostructured Nd2Fe14B grains and the amorphous Ti-rich iron-based intergranular phase but could be weakened by precipitates that act as magnetic pores. Remelting during PBF-LB led to the transformation of the coarse grains of the previously solidified layer to fine ones, favourable for the permanent magnetic properties. The mechanisms of these complex phase formations and transformations during processing and the development of the nanocrystalline microstructure are elucidated in this paper as a basis for informing the optimisation process for microstructural development
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
Understanding irradiation-induced nanoprecipitation in zirconium alloys using parallel TEM and APT
We investigate nano-scale irradiation-induced precipitation in a ZrSnFeCrNi-alloy (Zircaloy-2) by combining atom probe tomography (APT) for chemical detail with scanning transmission electron microscopy (STEM) and high resolution energy dispersive X-ray (EDX) spectroscopy for wider context and complimentary and correlative TEM diffraction techniques for crystallographic relationships. We find that Fe and Cr-rich nano-rods precipitate in Zircaloy-2 following proton irradiation at 350 °C to a low dose of ∼2 dpa. The long-axis of the nano-rods are aligned in a direction 12–15° from the Zr matrix , align in the basal plane and are of width 1.5–5 nm. Smaller rods are of APT-determined composition Zr4(Fe0.67Cr0.33), tending towards Zr3(Fe0.69Cr0.31) as the rod volume increases to > ∼400 nm3, in agreement with STEM-EDX determination of composition resembling that of Zr3Fe with Cr replacing some of the Fe. The Fe/Cr ratio has been shown to increase with distance from the nearest partially-dissolved Zr(Fe,Cr)2 phase particle. The nucleation of nano rods has implications for macroscopic irradiation-induced deformation phenomena, irradiation-induced hardening and the evolution of dislocation loops and other defects
Advances in Atom Probe Tomography Instrumentation: Implications for Materials Research
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