Search NASA⌕ Search

SEARCH · Search NASA

Results for “Atom Probe Tomography (APT)”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 127 records · Page 7

Manufacturing Oxide Dispersion Strengthened (ODS) steel plate via cold spray and friction stir processing

Oxide dispersion strengthened (ODS) steels, traditionally fabricated by ball milling and conventional powder metallurgy techniques to achieve bulk form, followed by intricate rolling and thermal treatment steps to achieve plate or sheet form. Here, we present a novel processing route that combines cold spray (CS) with friction stir processing (FSP) to manufacture ODS steel plate directly from gas atomization reaction synthesis (GARS)-prepared powder, thus no rolling steps involved. Microstructural and mechanical characterizations were performed to assess the quality and properties of the resulting ODS steel plate. Our findings demonstrate that the slightly porous CS deposited layer was fully consolidated after FSP, yielding a fully dense ODS steel plate that exhibited a favorable tradeoff between strength and ductility upon extraction from the substrate. Furthermore, through microstructural analysis, we revealed the presence of an appreciable density (∼10 22 /m 3 ) of nano-sized oxide particles, with the majority being smaller than 5 nm via the combined CS + FSP fabrication route. This work serves as a first proof-of-concept demonstration of the manufacturing approach described herein, offering a possible alternative route for producing ODS steel plates.

36 MATERIALS SCIENCE↗

Correlative STEM-APT characterization of radiation-induced segregation and precipitation of in-service BWR 304 stainless steel

In this study, radiation induced segregation and precipitation phenomena in an in-service boiling water reactor 304 stainless steel component were investigated using directly correlated 3D-atom probe tomography and scanning transmission electron microscopy. Significant quantitative differences in measured segregation at grain boundaries were found between the atom probe and energy dispersive spectroscopy measurements of the exact same locations. In particular, a much stronger Si segregation (~10 atomic% via atom probe versus ~4 atomic% via electron microscopy) and different Cr profile shapes were detected that are critical to models of radiation induced segregation and stress corrosion cracking behavior. These quantitative differences highlight the need for comparative microscopy and critical evaluation of limitations in each analytical method. Elemental segregation to dislocations and conjoined-clusters were also highlighted by atom probe; confirming and expanding upon what has been observed in test reactor neutron and accelerator-based ion irradiations.

36 MATERIALS SCIENCE↗

Understanding effects of chemical complexity on helium bubble formation in Ni-based concentrated solid solution alloys based on elemental segregation measurements

Here, helium bubble formation and swelling were systematically studied in Ni-based concentrated solid solution alloys containing different numbers and types of elements. Our microscopy analysis showed that although increasing the alloy chemical complexity helps suppress bubble formation in general, there is no monotonic relationship between the bubble growth rate and the number of alloying elements. Certain elements (e.g., Fe and Pd) are more effective in suppressing bubble growth than others (e.g., Cr and Mn). Atom probe tomography was applied to accurately measure elemental segregation around bubbles, revealing unique effects of certain alloying elements on vacancy migration towards bubbles. More specifically, the high vacancy mobility via Cr sites leads to a large vacancy flux and an increased bubble size, while the high degree of atomic size mismatch introduced by Pd helps deflect vacancy flow away from bubbles and decrease the amount of swelling. The effects identified in this study provide new strategies to design concentrated solid solutions with superior resistance to swelling.

36 MATERIALS SCIENCE↗

Precipitation-site competition in duplex stainless steels: Cu clusters vs spinodal decomposition interfaces as nucleation sites during thermal aging

Competing microstructural evolution mechanisms can exist simultaneously when duplex stainless steels are operating for several decades in a high temperature service environment. Such competition between different microstructural evolution pathways can be difficult to ascertain using simple model alloy systems necessitating detailed structural and compositional analysis of phase transformation mechanisms in complex alloys Thus, in this study duplex stainless steels with complex but well understood chemistries were used to investigate the relative importance of different heterogeneous nucleation sites – specifically spinodal decomposition and Cu clustering – on precipitation of Ni-Si-Mn particles during long term thermal aging. Precipitation of Ni-Si-Mn particles in duplex stainless steels and ferritic steels during thermal aging and irradiation is known to have profound effect on mechanical properties. Using duplex stainless steels with custom modified compositions along with atom probe tomography characterization and first-passage kinetic Monte Carlo (FPKMC) simulations it is revealed that while the interface between Cr and Fe formed during spinodal decomposition can be a pathway for diffusion of Ni, Si, Mn, and Cu, it is not a site that encourages precipitation of Ni-Si-Mn rich particles. Instead, the presence of a higher concentration of Cu in these steels leads to formation of small Cu clusters with high energy interfaces that act as nucleation sites for Ni-Si-Mn particles because of its strong interaction particularly with Ni increasing the chemical driving force for precipitation. These results will help inform predictive models for the use of duplex stainless steels and other precipitation-hardened alloys for extended operation at high temperatures.

Duplex stainless steel, Thermal aging, Precipitati↗

Extensive nanoprecipitate morphology transformation in a nanostructured ferritic alloy due to extreme thermomechanical processing

Nano-oxide precipitates in a modern nanostructured ferritic alloy were investigated after extreme thermomechanical processing into a thin-walled tube geometry. It was found that the morphology of the precipitates changed from spherical to rod-shaped, with some increasing to aspect ratios of up to 9, despite the precipitate volume fraction (0.3%) and number density (> 10 23 m -3 ) of precipitates remaining unchanged. High-resolution electron microscopy showed that the precipitates likely remained coherent with the Fe-matrix, while atom probe tomography confirmed that the precipitate compositions remained unaffected by the transformation. The morphological change was attributed to the shearable nature of the (Y,Ti,O)-rich precipitates, indicating they should be considered as “soft” obstacles to dislocation motion. The elongation was most pronounced in larger (>5 nm) precipitates, which may be caused by preferential dissolution of the smallest (1–3 nm) precipitates followed by the competition between re-precipitation and solute diffusion to larger precipitates during recovery heat treatments.

36 MATERIALS SCIENCE↗

X-ray diffraction and in situ pressurization of dentine apatite reveals nanocrystal modulus stiffening upon carbonate removal

Bone-like materials comprise carbonated-hydroxyapatite nanocrystals (c-Ap) embedding a fibrillar collagen matrix. The mineral particles stiffen the nanocomposite by tight attachment to the protein fibrils creating a high strength and toughness material. The nanometer dimensions of c-Ap crystals make it very challenging to measure their mechanical properties. Mineral in bony tissues such as dentine contains 2~6 wt.% carbonate with possibly different elastic properties as compared with crystalline hydroxyapatite. Here we determine strain in biogenic apatite nanocrystals by directly measuring atomic deformation in pig dentine before and after removing carbonate. Transmission electron microscopy revealed the platy 3D morphology while atom probe tomography revealed carbon inside the calcium rich domains. High-energy X-ray diffraction in combination with in situ hydrostatic pressurization quantified reversible c-Ap deformations. Additionally, crystal strains differed between annealed and ashed (decarbonated) samples, following 1 or 10 h heating at 250 °C or 550 °C respectively. Measured bulk moduli (K) and a-/c-lattice deformation ratios (η) were used to generate synthetic K syn and ηsyn identifying the most likely elastic constants C 33 and C 13 for c-Ap. These were then used to calculate the nanoparticle elastic moduli. For ashed samples, we find an average E 11 =107 GPa and E 33 =128 GPa corresponding to ~5% and ~17% stiffening of the a-/c-axes of the nanocrystals as compared with the biogenic nanocrystals in annealed samples. Ashed samples exhibit ~10% lower Poisson's ratios as compared with the 0.25~0.36 range of carbonated apatite. Carbonate in c-Ap may therefore serve for tuning local deformability within bony tissues.

36 MATERIALS SCIENCE↗

An Atom Probe Tomography Study of the Through Wall Attenuation Effect on Cu-rich Precipitate Formation in a Reactor Pressure Vessel Steel

In this study, high-Cu weld material harvested from an ex service reactor pressure vessel (RPV) steel from Unit 1 of the decommissioned Zion Nuclear Generating Station has been characterized using atom probe tomography. Samples taken from 4 different positions through the thicknesses of the pressure vessel wall from the water-side to the air-side were characterized, along with an unirradiated baseline material. In the baseline material, no precipitates were found and the Cu was observed to be fully in solid solution; however, scanning transmission electron microscopy combined with energy dispersive spectroscopy (STEM-EDS) revealed the presence of ϵ -Cu that form during processing of the material and results in the concomitant decrease of matrix Cu. Following irradiation, a high number density of nano-scale Cu-rich precipitates (CRPs) were observed, uniformly distributed throughout the matrix. The Cu content within the CRPs was found to be ~30-35 at.% regardless of location in the wall. No statistically significant variation in the compositions, mean radius, number density, or volume fraction as a function of location within the wall was observed. The measured matrix Cu level excluding CRPs contribution was found to be ~90 appm higher than the solubility limit suggesting that further nucleation and growth of the CRPs under continued operations would have occurred. These results clearly demonstrate that the neutron energy attenuation has no significant effect on the precipitation kinetics of CRPs regardless of location in the wall in high-Cu RPV steels under irradiation.

36 MATERIALS SCIENCE↗

Evolution of the role of molybdenum in duplex stainless steels during thermal aging: From enhancing spinodal decomposition to forming heterogeneous precipitates

Thermal aging of ferrite in duplex stainless steels leads to a complex microstructural evolution that can give way to large deleterious changes in mechanical properties. The microstructural evolution mechanisms that happen concurrently are strongly linked to minor changes in composition. By characterizing duplex stainless steels with various compositions over a range of aging conditions, it was revealed that adding a modest amount of Mo to cast austenitic stainless steel (such as changing from grade CF3 to grade CF3M) not only increases the kinetics of spinodal decomposition and Ni-Si-Mn-rich G-phase precipitation, but it also forms a separate Mo-rich phase. At shorter equivalent aging times, Mo segregates from Fe and towards Cr accelerating spinodal decomposition. At longer aging times, Mo enriches in the Ni-Si-Mn clusters before phase separating into an adjoined Mo-rich cluster. We found that these phase changes and precipitation events result in a rather steep drop in fracture and impact toughness. These results will inform the design of similar alloys for use at high temperatures.

36 MATERIALS SCIENCE↗

On the high-temperature stability of the Al 8 Cu 3 Ce intermetallic in an additively manufactured Al-Cu-Ce-Zr alloy

High-temperature resistant eutectic Al alloys are crucial materials for lightweight and energy efficient design in the automotive and aviation industries. Additive manufacturing offers a pathway to refine eutectic microstructures and develop novel alloys with superior high-temperature strength. High-volume fraction intermetallic Al-Cu-Ce alloys have been developed to deliver high-temperature strength in combination with reduced hot-tearing susceptibility. Zr is added to provide additional strengthening via nanoscale Al 3 Zr precipitation, and to stabilize and avoid coarsening of the Al 8 Cu 3 Ce phase. However, the detailed interaction between Zr and Al 8 Cu 3 Ce remains unexplored. In this work, we show with synchrotron X-ray diffraction that laser powder bed fusion fabricated Al-Cu-Ce and Al-Cu-Ce-Zr alloys contain predominantly the Al 8 Cu 3 Ce intermetallic in the as-fabricated condition. Heat treatment of the Al-Cu-Ce alloy results in the Al 8 Cu 3 Ce → Al 8 Cu 4 Ce phase transformation. In the Al-Cu-Ce-Zr alloy, minor fractions of (Al,Cu,Si) 4 Ce and Al 2 Cu-θ are found in the as-fabricated condition, while Al 8 Cu 3 Ce remains stable during heat treatment. Atom probe microscopy quantifies intermetallic stoichiometries and reveals how Zr is enriched at the Al-matrix/Al 8 Cu 3 Ce interface acting as a diffusion barrier against solute exchange. Calibrated thermodynamic modeling underpins this as a kinetic effect. Here, a qualitative microstructural model summarizes, how Zr stabilizes Al 8 Cu 3 Ce against phase transformations and coarsening.

36 MATERIALS SCIENCE↗

New frontiers in atom probe tomography: a review of research enabled by cryo and/or vacuum transfer systems

There has been a recent surge in the use of cryo and/or vacuum specimen preparation and transfer systems that are broadening the scope of research enabled by the microscopy technique of atom probe tomography. This is driven by the fact that, like for many microscopes, the application of atom probe to air and temperature sensitive materials or wet biological specimens has previously been limited by through-air-transfer and through-vacuum-transfer at room temperature. Here we provide an overview of the critical areas of research that require these new transfer and analysis protocols, as well as a review of current advances in transfer devices, environmental cells and glove boxes for controlled sample manipulation. This includes the study of catalysis and corrosion, the application of atom probe to biological samples, the study of liquid-solid interfaces, natural ageing investigations and the analysis of hydrogen in metals.

36 MATERIALS SCIENCE↗

Radiation-Enhanced Anion Transport in Hematite

The influence of radiation-induced (1 MeV energy H+ to ~0.1 dpa at 450°C), non-equilibrium point defect populations on mass transport is studied with an integrated campaign of experimental and theoretical methods. Using epitaxial thin films of hematite with embedded 18O tracer layers and nanoscale atom probe tomography measurements, it is shown that anion self-diffusion is enhanced by at least 2 orders of magnitude under irradiation compared to thermal diffusion alone. Complementary scanning transmission electron microscopy of vacuum annealed specimens, reveals associated microstructural changes in the oxide films, including local phase transformation to Fe3O4 and the development of nanoscale voids from vacancy coalescence. Point defect formation and migration energies were computed from density functional theory and applied within the context of chemical rate theory to analyze contributions from both interstitial and vacancy mechanisms to self-diffusion in thermal and irradiation conditions. Comparisons are made between calculated, literature and newly measured self-diffusion values, revealing good agreement on the magnitude of radiation-enhanced anion diffusion. Further, the model suggests a transition from vacancy to interstitialcy mechanisms at low temperatures and high oxygen activity, consistent with the varied activation energies reported from prior studies.

iron oxides, isotopic tracers, atom probe tomograp↗

Rapid assessment of structural and compositional changes during early stages of zirconium alloy oxidation

A multimodal chemical imaging approach has been developed and applied to detail the dynamic, atomic-scale changes associated with oxidation of a zirconium alloy (Zircaloy-4). Scanning transmission electron microscopy, a gas-phase reactor chamber attached to an atom probe tomography instrument, and synchrotron-based X-ray absorption near-edge spectroscopy were employed to reveal morphology, composition, crystal, and electronic structure changes that occur during initial stages of oxidation at 300 °C. Oxidation was carried out in 10 mbar O 2 gas for short exposure times of 1 and 5 min. A multilayered oxide film with a cubic ZrO adjacent to the oxide/metal interface, a nanoscopic transition region with a graded composition of ZrO 2-x (where 0 < x < 1), and tetragonal ZrO 2 in the outermost oxide were formed. Partitioning of the major alloying element (tin) to the oxide/metal interface and heterogeneously within the oxide accompanied the development of the layered oxide. Our work provides a rapid, high-throughput approach for detailed characterisation of initial stages of zirconium alloy oxidation at an accelerated time scale, with implications for several other alloy systems.

36 MATERIALS SCIENCE↗

Origins of high ductility exhibited by an extruded magnesium alloy Mg-1.8Zn-0.2Ca: Experiments and crystal plasticity modeling

Low ductility and strength are major bottlenecks against Mg alloys' wide applications. In this work, we systematically design the composition and fabrication process for a low-alloyed Mg-Zn-Ca alloy, showing that it can be extruded at low temperatures (~ 250 degrees C) and high speeds (~2 mm/s). After the extrusion, this alloy exhibits a substantially weakened basal texture, relatively small grain size, very high tensile elongation (~ 30%), and good strength. The origin of the considerably improved ductility was studied using a combination of three-dimensional atom probe tomography (3D-APT), transmission electron microscopy (TEM), electron backscattered diffraction (EBSD) in conjunction with surface slip trace analysis, in-situ synchrotron X-ray diffraction, and elasto-plastic self-consistent (EPSC) modeling. Co-segregation of Zn and Ca atoms at a grain boundary is observed and associated with texture weakening and grain boundary mediated plasticity, both improving the ductility. While basal slip and prismatic slip are identified as the dominant deformation systems in the alloy, the ratio between their slip resistances is substantially reduced relative to pure Mg and most other Mg alloys, significantly contributing to the improved ductility of the alloy. This Mg-Zn-Ca alloy exhibiting excellent mechanical properties and low fabrication cost is a promising candidate for industrial productions.

36 MATERIALS SCIENCE↗

Methods for stabilizing biological and soft materials for atom probe tomography

Techniques are disclosed for stabilizing soft specimen traditionally considered too fragile for APT instruments. These specimens include biological samples, polymers and other fragile materials. For this purpose, a protective structure is disclosed that surrounds the sides of the specimen by supporting walls while only exposing the very end or terminus of the specimen to the electrostatic field of the APT instrument. The protective structure may take the form of a nanoscale conical grinder which continually machines the specimen to regenerate the terminus of the specimen in-situ. Alternately, the protective structure may take the form of a nanopipette in which the specimen is first frozen before undergoing field evaporation together with the tip of the nanopipette. Heretofore only routinely possible for rigid and hard materials, the design thus extends APT analysis to produce three-dimensional atomic-scale maps of soft specimens.

36 MATERIALS SCIENCE↗