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Laser surface remelting can be used to manipulate the microstructure of cast material. Here, we present a detailed analysis of the microstructure of Fe$_2$VAl following laser surface remelting. Within the melt pool, elongated grains grow nearly epitaxially from the heat-affected zone. These grains are separated by low-angle grain boundaries with 1{\deg}-5{\deg} misorientations. Segregation of vanadium, carbon, and nitrogen at grain boundaries and dislocations is observed using atom probe tomography. The local electrical resistivity was measured by an in-situ four-point-probe technique. A smaller increase in electrical resistivity is observed at these low-angle grain boundaries compared to high-angle grain boundaries in a cast sample. This indicates that grain boundary engineering could potentially be used to manipulate thermoelectric properties.

Atom probe tomography has been raising in prominence as a microscopy and microanalysis technique to gain sub-nanoscale information from technologically-relevant materials. However, the analysis of some functional ceramics, particularly perovskites, has remained challenging with extremely low yield and success rate. This seems particularly problematic for materials with high piezoelectric activity, which may be difficult to express at the low temperatures necessary for satisfactory atom probe analysis. Here, we demonstrate the analysis of commercial BaTiO3 particles embedded in a metallic matrix. Density-functional theory shows that a metallic coating prevents charge penetration of the electrostatic field, and thereby suppresses the associated volume associated change linked to the piezoelectric effect.

In this work, the nanometer-scale mass flow coupled to dislocation processes near the γ/γ′-interface during high temperature and low stress creep of a model Ni-base single crystal superalloy is investigated. In the early creep stages, the dislocation networks in the γ-phase at γ/γ′-interfaces attract γ-stabilizing elements like Cr, Co and in particular Re, resulting in compositional gradients close to the interface. At larger strains, where dislocations frequently cut into the γ′-phase, this local interfacial enrichment in these elements is no longer observed. The cutting dislocations take part of the segregated atoms away, whilst the remaining atoms are released and diffuse back into the γ-channels.

High-strength Al-Zn-Mg-Cu alloys are highly susceptible to stress corrosion cracking (SCC) which severely limits their lifetime. Reversion and re-aging (RRA) temper provides a higher SCC resistance at no loss in strength, yet the microstructural origins of these enhanced properties remain elusive. In an Al-Zn-Mg-Cu alloy, we show that the fine precipitate dispersion in the grain interiors is similar in the peak aged and RRA tempers. However, upon RRA, precipitates inside the grains are enriched in Cu, lowering the Cu matrix content, and reducing the relative difference in the Cu precipitate composition between bulk and grain boundaries. This study enriches the current understanding on the critical role of Cu related to SCC resistance in Al-Zn-Mg-Cu alloys.

We have studied the large-scale plasticity assisted topological inversion in a Ni-based superalloy after creep at 850 °C. Multi-scale characterization from the micro- to the near-atomic scale was used to unravel the processes governing topological inversion of a Ni-based single crystal superalloy and reconstruct the resulting three-dimensional microstructure. A plasticity assisted redistribution of interacting solutes mechanism, where shearing dislocations mass-transport solutes, is proposed to explain the transition from a rafted to intricately interconnected (inverted) structure. The interplay between microstructural evolution and mechanical behavior is discussed in terms of applied stress and microstructural features, relating atomic-scale processes to macro-scale behavior.

It is critical to control the electrical resistivity of alloys used for wires in harsh environment, e.g. for implanter bio-devices. As-drawn and aged MP35N wires were investigated, exhibiting increasing resistivity with aging time and temperature, in contrast to precipitate-forming alloys. We reveal Cr segregation to deformation twin boundaries upon aging, which effectively facilitates electron scattering and increases the resistivity. Since the diffusion of Cr atoms to these fault planes is rather fast, the larger increment of resistivity occurs very quickly, especially at elevated temperatures. This mechanism is likely active in a wide range of non-dilute alloys that form extended fault planes.

Industrial scale single crystal (SX) Ni-base superalloys contain numerous low angle grain boundaries inherited from the solidification process. Here, we demonstrate that low angle grain boundaries in a fully heat-treated SX model Ni-base superalloy are strongly segregated with up to 12 at% Re. Some Re-rich dislocations forming this grain boundary are found located inside γ, others close to a γ/γ′ interface. Although these segregated Re atoms lose their solid-solution strengthening effect, they may enhance the creep resistance by pinning the low angle grain boundaries and slowing down dislocation reactions.

The solute partitioning under dynamic strain-induced austenite reversion in a Fe-11Mn-1Al-0.07C (in wt.%) steel was studied by atom probe tomography. It was found that the concentrations of Mn and Al fluctuate in austenite at the nanoscale during warm deformation at 650 °C, leading to less stable chemical zones. It is proposed that stored energy in ferrite can change the thermodynamic equilibrium, leading to the formation of austenite with lower Mn and higher Al contents. This paper reveals evidence that stored strain can deviate the thermodynamic equilibrium, and hence could be a new path for engineering the nanostructures in austenite.

We demonstrate the formation of a hierarchical microstructure by optimized combination of Mo-doping and thermo-mechanical processing in a NiCoCr medium-entropy-alloy (MEA) that results in a significant improvement in yield-strength (~775 MPa) and ultimate-tensile-strength (~1200 MPa) with an elongation to fracture up to 35%. Addition of Mo slows down the recrystallization kinetics of the cold-rolled alloy at 700 °C. After 4 h annealing, the microstructure comprises soft recrystallized and hard non-recrystallized zones, dispersed σ precipitates, annealing twins and retained stacking faults/nanotwins that are shown to contribute to the overall mechanical behavior.

Partitioning of C during tempering of quenched Fe-9.6Ni-0.5C-0.6Mn-0.6Mo-0.7Cr-0.1V (at.%) steel is determined by atom probe tomography and the resulting microstructure is described. The precipitated austenite size, together with its C and Ni content control its thermal stability and these can vary differently with tempering time and temperature. Thus, both austenite and strong carbide formers compete for the available C early in the process. Due to widely different transport kinetics, C likely plays a dominant role early but is either fully consumed or its role diminishes by dilution, and Ni partitioning eventually takes over as the austenite stability-controlling species.

The successful development of advanced materials such as nanostructured ferritic alloys (NFA) for next generation nuclear reactor concepts and ultra-supercritical steam power plants requires information on long term thermal creep. To support this initiative, this work examines the NFA MA957 (Fe-14Cr-1.0Ti-0.3Mo + 0.3Y2O3 in wt%) crept to 61,251 h at 825 °C and 70 MPa, the longest creep test available to date for this material. Using atom probe tomography and electron microscopy, it is shown that the grain size and nanoprecipitate size/composition are unaffected following this 7 yr creep test, although significant porosity is noted throughout the microstructure attributed to microvoid coalescence and growth.

We report on the full three-dimensional compositional partitioning among the features of a planar imperfection comprising a superlattice intrinsic stacking fault (SISF) with its leading and trailing partials, as well as the antiphase boundary (APB) in the wake of the trailing partial formed in the L12-ordered γ′ phase of a CoNi-based single crystal superalloy. The partial dislocations and the APB are found to be Cr/Co rich relative to the surrounding γ′ and richer in W/Ta/Ti compared to the γ matrix phase. Solute diffusion mechanisms are derived from the compositional gradients in the vicinity of the imperfection.

A face-centered cubic (FCC) phase in electro-polished specimens for transmission electron microscopy of commercially pure titanium has sometimes been reported. Here, a combination of atom-probe tomography, scanning transmission electron microscopy and low-loss electron energy loss spectroscopy is employed to study both the crystal structural and chemical composition of this FCC phase. Our results prove that the FCC phase is actually a TiHx (x ≥ 1) hydride, and not a new allotrope of Ti, in agreement with previous reports. The formation of the hydride is discussed.

We investigated the origin of the deleterious grain boundary α phase formed during the aging of the β-titanium alloy, Ti–5Al–5Mo–5V–3Cr–0.5Fe (wt.%). We probed the composition of low and high-angle grain boundaries from the as-quenched β condition correlating electron microscopy and atom probe tomography. Our analysis reveals strong segregation of some α-stabilizing elements at both types of boundaries, especially oxygen, along with a depletion of β-stabilizing elements. The grain boundary maintains the body-centered-cubic structure despite the presence of this local composition. Our thermodynamic calculations, based on the measured grain boundary compositions, indicate that the segregation significantly increases the chemical driving force for α nucleation upon aging. Our work provides essential insight into the formation of the undesired grain boundary α layers along prior-β grain boundaries in metastable β-Ti alloys and paves the way for microstructural engineering of these alloys with enhanced mechanical properties.

Electron microscopy and atom probe tomography were combined to investigate the crystallography and chemistry of a single twin boundary (TB) in a rare-earth-free ferromagnetic MnAl Heusler alloy. The results establish a significant segregation of Mn along the twin boundaries. An enrichment of approx. ~8 at.% Mn was measured along the twin boundary with a confined depletion outside the twin boundary, suggesting short range solute diffusion occurring during massive transformation.

We report on the sub-nanometer scale characterization of Co-12Ti-4Mo and Co-12Ti-4Cr (at.%) model alloys. Atom probe tomography reveals that Co and Cr partition to γ, whereas Ti and Mo to γ′. Additions of Mo and Cr to the reference Co-12Ti system lead to strong increases in γ′ volume fraction by about 25% and 12%, respectively. Element-specific spatial distribution maps along the [001] direction of the L12-ordered γ′ phase reveal that both Mo and Cr preferentially replace Ti on its sublattice. The remaining excess Ti is available for formation of additional γ′, resulting in enhanced γ′ volume fractions.

We have studied here the distribution of carbon and alloying elements in the martensite-austenite (M-A) constituent in intercritically reheated coarse-grained heat-affected zone (ICCGHAZ) of a high-strength pipeline steel using atom probe tomography (APT). Notable enrichment of C (0.49 wt%) and Mn (2.32 wt%) was observed within the M-A constituent, which induced the formation of lath martensite and deteriorated the toughness. Elemental segregation in the interfacial region between M-A constituent and matrix may contribute to the debonding mechanism of M-A constituent and assist nucleation of cleavage cracks. Distribution of solute Nb indicated no apparent difference between the matrix and M-A constituent.

We investigated the nucleation and growth of α precipitates in the presence of nano-scale, titanium-rich, ordered-orthorhombic O″ precipitates formed during heating at 5 °C/min to 400 °C in a metastable β-Ti alloy, Ti-5Al-5Mo-5V-3Cr. The Oʺ precipitates are found to assist α nucleation by serving as preferential nucleation sites. In the very initial stages of its precipitation, the α phase is found to have formed via a coupled diffusional-displacive mode as titanium-rich plates. At this stage, aluminum partitions equally between the β matrix and the growing α precipitates, but slowly diffuses up-hill into the α phase during isothermal aging at 400 °C for 15 h. The interplay between such pre-formed metastable phases and α can be exploited to tailor the microstructure, by refining the α distribution, and consequently improve the mechanical properties of β-Ti alloys. Our work paves the way for exploiting this cascade of metastable phases for further microstructural engineering of β-Ti alloys.

Segregation of Ni was observed by atom probe tomography at the edges of a pseudo-hexagonal dislocation loop within As + -implanted (0 0 1) Si wafers, after Ni deposition but before heat treatment. Thanks to crystallographic information retained within the atom probe tomography data, the orientation of the loop was determined to be within the {1 1 1} plane and elongated along the 1 1 ¯ 0 > direction. The presence of pseudo-hexagonal dislocation loops was confirmed by transmission electron microscopy. Concentrations of more than 10 at.% in Ni were measured at the edges of the loop.

The microstructures of nanostructured Ti–Si–N hard coatings were investigated by transmission electron microscopy and pulsed laser atom probe. C and O impurities were detected. No evidence of increased Si levels at the grain boundaries was found, suggesting that Si is either in the form of a layer too thin to be detected using the techniques employed or in the form of a solid solution of SiN clusters.

The corrosion potential of commercially pure titanium in NaCl solutions is dramatically affected by trace Fe additions, which cause the appearance of submicron pockets of β phase at grain boundary triple points. Furthermore, the low solubility of hydrogen in hexagonal close-packed α-Ti makes titanium alloys prone to subsequent hydride-associated failures due to stress corrosion cracking. We analyzed α-α and α-β sections of the abutting grain boundary of a β pocket in a Grade 2 CP-Ti, and the α-β phase boundary. Fe and H partition to β and segregate at the grain boundary, but no segregation is seen at the α-β phase boundary. In contrast, a significant Ni (>1 at%) accumulation is observed at the α-β phase boundary. We propose that the β-pockets act as hydrogen traps and facilitate the nucleation and growth of hydrides along grain boundaries in CP-Ti.