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At least 361 records · Page 20

NSUF Report EBSD analyses on metallic fuel samples: Tips and improvements in sample preparation

EBSD (Electron Backscatter Diffraction) is an analytic technique used to evaluate the microstructure of a specimen. It can be used to evaluate interesting crystallographic data ranging from grains size to grain orientation, from grain boundaries to stresses. Moreover, in the field of nuclear materials EBSD can aid in estimating properties important for reactor performance, such as dislocation and residual strain [1]. EBSD patterns are generated by focusing a stationary electron gun on the specimen and detecting the backscatter electrons that satisfy Bragg conditions, and thus are diffracted by the crystal planes forming the so called Kikuchi bands. These bands correspond to each of the lattice diffracting crystal planes and are detected on a phosphor screen via a low-light CCD camera [2]. The patterns are generated within a small interaction volume located at a depth of less than 50-100 nm. Because of this, the data quality is extremely sensitive to the integrity of the crystallographic lattice order at the surface of the sample and thus to sample preparation and to oxidation [3]. While conventional sample preparation methods are widely used in materials science, they often do not lead to quality electron backscatter patterns needed for the characterization of nuclear materials [4]. This has been related by many authors to the challenges associated with handling radiological specimens, their rapid oxidation, and artifacts in such samples (e.g. high number of defects, precipitates and/or porosities) [4-8]. EBSD, however, can be an invaluable technique to evaluate microstructural evolution during fabrication and after irradiation at the required mesoscale for model and simulation. It also provides important information on grain structure necessary to understand irradiation effect, such as grain subdivision. Thus, it is of paramount importance to further the application of this technique to nuclear materials and especially irradiated fuels.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Perovskite/Perovskite Tandem Photoelectrodes for Low-Cost Unassisted Photoelectrochemical Water Splitting

In this project, we aim to address the challenges of achieving efficient and cost-effective unassisted photoelectrochemical water splitting using perovskite/perovskite tandem photoelectrodes. We utilized the following unique approaches to advance our innovation. (1) We developed stable and efficient low-E g (1.2 – 1.4 eV) perovskites as the bottom electrodes. We demonstrated approaches to improve the photovoltaic performance and photothermal stability of low-E g Sn-Pb iodide perovskite solar cells. (2) We developed a low-temperature synthesis route to fabricate wide-E g (>1.8 eV) perovskite top electrodes. By combining theoretical and experimental investigation, we found methods to reduce the formation of defects and dislocations in the wide-E g mixed halide perovskites and suppress halide segregation. (3) We developed a robust metal oxide-based interconnecting layer to integrate two perovskite layers into tandem photoelectrodes. Our monolithically integrated tandem devices feature a high V OC of more than 2 V and a high J SC of more than 15 mA/cm 2 . We showed the new design of the tandem photoelectrodes that is critical to the stable operation of tandem photoelectrodes for unassisted PV/PEC water splitting. (4) We demonstrated a water-impermeable barrier of carbon paste/epoxy/metal foil composite, which can prevent photocorrosion and water ingress of perovskite active layers. This surface protection enabled the operation of perovskite photoelectrodes in water and significantly enhanced the long-term stability of our tandem devices. (5) We conducted standardized PEC characterization in collaboration with NREL and reported accurate determination of solar-to-hydrogen conversion efficiencies of perovskite/perovskite tandem photoelectrodes. At the end of the project, we demonstrated perovskite/perovskite tandem photoelectrodes with STH efficiencies of up to 18% and less than 20% efficiency loss after continuous operation for more than 500 hours in water. Our results demonstrate the potential to develop a low-cost, durable, and efficient water-splitting system that meets the DOE 2026 and 2031 cost targets for hydrogen production.

08 HYDROGEN↗

Experiment 1: Orbital Processing of High-Quality Zn-Alloyed CdTe Compound Semiconductors

Zinc-alloyed cadmium telluride (Zn:CdTe) crystals were grown in unit gravity and in microgravity for comparative analysis. Two crystals were grown on USML-1/STS-50 in 1992, and two additional crystals were grown on USML-2/STS-73 in 1995. The Crystal Growth Furnace (CGF) in the seeded Bridgman-Stockbarger crystal growth geometry was utilized on both missions. Crystals grown on USML-1/STS-50 were found to have solidified with partial wall contact due to the near-absence of the hydrostatic pressure in microgravity, a residual g-vector that was not axial, and the nonwetting sample/ampoule wetting conditions. Crystals grown on USML-2/STS-73 included: a sample/ampoule identical to the USML-1/STS-73 sample/ampoule, with the addition of a restraining spring to simulate hydrostatic pressure internally, and a tapered ampoule which accomplished 2.2 cm of crystal growth without wall contact. Infrared transmission of all ground and flight samples was found to be 63-66 percent, very close to the theoretical 66 percent, suggesting good stoichiometric control. Infrared microscopy confirmed that the primary precipitates were Te and their size (1-10 microns) and density suggested that the flight- and ground-base samples experienced similar thermal histories. Longitudinal macrosegregation, calculated using scaling analysis, was predicted to be low. Nearly diffusion controlled growth was achieved even in unit gravity and macrosegregation data could be fit with a diffusion controlled model. Radial segregation was monitored and was found to vary with fraction solidified, particularly through the shoulder region, where the sample cross section was varying significantly. It was also disturbed in the flight samples in regions where asymmetric wall contact was noted. In regions where a steady state was established, the radial segregation was invariant within our experimental measurement error. Flight samples were found to be much higher in structural perfection than samples processed in unit gravity under identical growth conditions. In regions where solidification had occurred without wall contact, the free surfaces evidenced virtually no twinning, although twins appeared in the flight samples in regions of wall contact and were pervasive in the ground samples. These results were confirmed using optical microscopy and synchrotron x-ray white beam topography. Full-width half-maximum rocking curve widths (FWHM), recorded in arc-seconds, were significantly reduced from 20 a-s (1 g) to 9 a-s (micro-g) for the best regions of the crystals. The 9 a-s (FWHM) rocking curve value in the unconfined flight samples equals the best value reported terrestrially for this material. The ground samples exhibited a fully developed (111)[110] dislocation mosaic structure, whereas dislocations within the flight samples were discrete and no mosaic structure was evident. The defect density was quantitatively reduced from 75,000 (1 g) to 800 (micro-g) +/-50 percent. Dislocation etch pit density results were confirmed using transmission synchrotron white beam and monochromated beam topography. The low defect density is thought to have resulted from the near absence of hydrostatic pressure, which allowed the molten boule to solidify with little or no wall contact. This minimized the transfer of hoop stresses during solidification and post-solidification processing.

Larson, D. J., Jr.↗

In situ observation of the atomic shuffles during the {${{11}}\bar{{{2}}}{{1}}$} twinning in hexagonal close-packed rhenium

Twinning, on par with dislocations, is critically required in plastic deformation of hexagonal close-packed crystals at low temperatures. In contrast to that in cubic-structured crystals, twinning in hexagonal close-packed crystals requires atomic shuffles in addition to shear. Though the twinning shear that is carried by twinning dislocations has been captured for decades, direct experimental observation of the atomic shuffles, especially when the shuffling mode is not unique and does not confine to the plane of shear, remains a formidable challenge to date. Here, by using in-situ transmission electron microscopy, we directly capture the atomic mechanism of the {${{11}}\bar{{{2}}}{{1}}$} twinning in hexagonal close packed rhenium nanocrystals. Results show that the {${{11}}\bar{{{2}}}{{1}}$} twinning is dominated by the ($\textbf{b}$ 1/2 , h 1/2 ) twinning disconnections. In contrast to conventional expectations, the atomic shuffles accompanying the twinning disconnections proceed on alternative basal planes along 1/6 {${{1\bar1}}{{{0}}}{{0}}$} , which may be attributed to the free surface in nanocrystal samples, leading to a lack of mirror symmetry across the {${{11}}\bar{{{2}}}{{1}}$} twin boundary.

(S)TEM↗

Evolution of Pore Structure and Permeability of Rocks Under Hydrothermal Conditions (Final Report)

The physical and transport properties of porous rocks can be altered by a variety of diagenetic, metamorphic, and tectonic processes, and the changes that result are of critical importance to such industrial applications as resource recovery, carbon dioxide sequestration, and waste isolation in geologic formations. The associated interrelationships between rocks, pore fluids and deformation are also key to understanding many natural processes, including dynamic metamorphism, fault mechanics, fault stability and pressure solution creep. In this project, we investigated the changes of permeability and pore geometry owing to inelastic deformation by solution-transfer, brittle fracturing and dislocation creep. In particular, we studied the coupling between pore fluids and deformation in fluid-filled quartz, calcite, mudstones and ultramafic rocks and examine the effects of coupled mechanical and chemical processes on the evolution of porosity and permeability under hydrothermal conditions. The investigations used a combination of techniques, that included triaxial laboratory experiments; uniaxial compressive loading with in situ observations of microstructure; permeability under hydrostatic compression; observations of microstructure using optical and electron microscopes, and micro-CT imaging; and numerical calculations. Laboratory experiments were designed to provide mechanical and transport data under conditions that isolate the particular mechanisms responsible for the changes. The data obtained were used to quantify changes in surface roughness, porosity, pore dimensions and their spatial fluctuations. The results of the experiments and data from image analyses were compared to the results of network, finite-difference and other numerical models to verify the validity of experimentally established relations between permeability and other rock properties. A bibliography for the period from 2015-2019 is appended below. New results obtained in the final year and the unfunded extension period are detailed below.

58 GEOSCIENCES↗

In-situ observation of nano-oxide and defect evolution in 14YWT alloys

Nanostructured ferritic alloys (NFAs) are considered as candidates for structural components in advanced nuclear reactors due to their excellent radiation resistance as a result of a high density of nano-oxides (NOs) in the microstructure. Therefore, gaining an understanding on the stability of NOs under irradiation is crucial. In this study, we have investigated the evolution of defects and NOs in 14YWT NFAs under in-situ Kr ion irradiation at room temperature (RT) and 450°C up to 10 dpa. It has been found that irradiations at 450°C do not create any changes in the NOs, similar to the bulk irradiations. On the other hand, elemental mapping indicates that NOs dissolve mostly after 10 dpa irradiations at RT. Thus, while defects are both annihilated and pinned by NOs at low doses (before the dissolution of NOs), glissile loops start to escape to the foil surface at high doses (after the dissolution of NOs), justifying the significantly low fraction of (111) loops compared to the literature values. Furthermore, high resolution transmission electron microscopy analysis has shown that the NOs are mostly coherent Y 2 Ti 2 O 7 particles with pyrochlore crystal structure after both RT and 450°C irradiations, similar to those observed before irradiation.

36 MATERIALS SCIENCE↗

Hypervelocity Dust Impact in Olivine: Fib/Tem Characterization and Comparison of Experimental and Natural Microcraters

The flux of objects impacting the surfaces of solar system airless bodies is dominated by micrometeoroids less than 1 mm diameter whose impact effects play a major role in the space weathering of airless body surfaces. To obtain better understanding of how small scale impact effects vary as a function of impact speed in an important lunar and asteroidal mineral, we produced artificial microcraters in San Carlos olivine using Fe metal dust particles 0.10 to 5 µm in diameter electrostatically accelerated to speeds between 0.35 to 25 km s-1. The crater morphologies, size distrrubiton and microstruc-tures were characterized by field-emission SEM (FE-SEM) and also by FIB cross sectioning of selected craters for field-emission scanning transmission electron microscopy (FE-STEM). These same techniques were also applied to study a natural 20 µm-diameter microcrater in a olivine grain on the surface of lunar rock 12075. Measured microcrater diameters in the experimental sample range between 0.20 to 5 µm with larger craters having more irregular outlines dominated by spallation fractures. FE-SEM and FE-STEM imaging docu-ment the formation of shock melt in the size population of experimental craters below approximately 1 µm in diameter, corresponding to particle impact speeds in the 10-25 km s-1 range. The natural olivine crater exhibits similar shock melt features along the perimeter of its cavity, but the shock melt also contains nanophase Fe metal particles, something not observed in the experimental samples. FE-STEM imaging of the experimental craters reveals complex shock-generated dislocation and nanofracture microstructures in zones extend-ing 1-2 µm into the olivine from the crater cavity. The natural microcrater shows a lower density of shock-generated disloca-tions that extends a factor of 2 deeper into the the olivine than in the experimental samples.

Roy Gray Christoffersen↗

Behavior of Particle Depots in Molten Silicon During Float-Zone Growth in Strong Static Magnetic Fields

In the photovoltaics industry, the largest market share is represented by solar cells made from multicrystalline silicon, which is grown by directional solidification. During the growth process, the silicon melt is in contact with the silicon nitride coated crucible walls and the furnace atmosphere which contains carbon monoxide. The dissolution of the crucible coating, the carbon bearing gas, and the carbon already present in the feedstock, lead to the precipitation of silicon carbide, and silicon nitride, at later stages of the growth process. The precipitation of Si3N4 and SiC particles of up to several hundred micrometers in diameter leads to severe problems during the wire sawing process for wafering the ingots. Furthermore the growth of the silicon grains can be negatively influenced by the presence of particles, which act as nucleation sources and lead to a grit structure of small grains and are sources for dislocations. If doped with Nitrogen from the dissolved crucible coating, SiC is a semi conductive material, and can act as a shunt, short circuiting parts of the solar cell. For these reasons, the incorporation of such particles needs to be avoided. In this contribution we performed model experiments in which the transport of intentionally added SiC particles and their interaction with the solid-liquid interface during float zone growth of silicon in strong steady magnetic fields was investigated. SiC particles of 7μm and 60μm size are placed in single crystal silicon [100] and [111] rods of 8mm diameter. This is achieved by drilling a hole of 2mm diameter, filling in the particles and closing the hole by melting the surface of the rod until a film of silicon covers the hole. The samples are processed under a vacuum of 1x10(exp -5) mbar or better, to prevent gas inclusions. An oxide layer to suppress Marangoni convection is applied by wet oxidation. Experiments without and with static magnetic field are carried out to investigate the influence of melt convection on the distribution of particles and their incorporation into the crystal. The field strengths applied by a superconducting magnet are 1T, 3T, 4.5T, and 5T. The increase in field strength dampens the melt flow, and so this study provides comparative data to the crystal growth experiment to be carried out onboard the sounding rocket mission TEXUS 51, where purely diffusive growth condition will be achieved under microgravity conditions.

Jauss, T.↗

Effects of Mars Atmosphere on Arc Welds: Phase 2

Gas tungsten arc welding (GTAW) is a vital fusion welding process widely used throughout the aerospace industry. Its use may be critical for the repair or manufacture of systems, rockets, or facilities on the Martian surface. Aluminum alloy AA2219-T87 and titanium alloy Ti-6Al-4V butt welds have been investigated for weldability and weld properties in a simulated Martian gas environment. The resulting simulated Martian welds were compared to welds made in a terrestrial atmosphere, all of which used argon shielding gas. It was found that GTAW is a process that may be used in a Martian gas environment, not accounting for pressure and gravitational effects, as long as adequate argon shielding gas is used to protect the weld metal. Simulated Martian welds exhibited higher hardness in all cases and higher tensile strength in the case of AA2219-T87. This has been attributed to the absorption of carbon into the fusion zone, causing carbide precipitates to form. These precipitates may act to pin dislocations upon tensile testing of AA2219-T87. Dissolved carbon may have also led to carburization, which may have caused the increase in hardness within the fusion zone of the welds. Based on the results of this experiment and other similar experiments, GTAW appears to be a promising process for welding in a Martian gas environment. Additional funding and experimentation is necessary to determine the effects of the low pressure and low gravity environment found on Mars on GTAW.

Courtright, Z. S.↗

Interface effect of Fe and Fe 2 O 3 on the distributions of ion induced defects

The stability of structural materials in extreme nuclear reactor environments—with high temperature, high radiation, and corrosive media—directly affects the lifespan of the reactor. In such extreme environments, an oxide layer on the metal surface acts as a passive layer protecting the metal underneath from corrosion. To predict the irradiation effect on the metal layer in these metal/oxide bilayers, nondestructive depth-resolved positron annihilation lifetime spectroscopy (PALS) and complementary transmission electron microscopy (TEM) were used to investigate small-scale defects created by ion irradiation in an epitaxially grown (100) Fe film capped with a 50 nm Fe 2 O 3 oxide layer. In this study, the evolution of induced vacancies was monitored, from individual vacancy formation at low doses—10 –5 dpa—to larger vacancy cluster formation at increasing doses, showing the sensitivity of positron annihilation spectroscopy technique. Furthermore, PALS measurements reveal how the presence of a metal–oxide interface modifies the distribution of point defects induced by irradiation. TEM measurements show that irradiation induced dislocations at the interface is the mechanism behind the redistribution of point defects causing their accumulation close to the interface. Finally, this work demonstrates that the passive oxide layers formed during corrosion impact the distribution and accumulation of radiation induced defects in the metal underneath and emphasizes that the synergistic impact of radiation and corrosion will differ from their individual impacts.

36 MATERIALS SCIENCE↗

Microstructural effects on the rotating bending fatigue behavior of Ti–6Al–4V produced via laser powder bed fusion with novel heat treatments

The rotating bending fatigue (RBF) behavior (fully reversed, R = -1) of additively manufactured (AM) Ti–6Al–4V alloy produced via laser powder bed fusion (PBF-L) was investigated with respect to different microstructures achieved through novel heat treatments. The investigation herein seeks to elucidate the effect of microstructure by controlling variables that can affect fatigue behavior in Ti–6Al–4V, such as chemistry, porosity, and surface roughness. In order to control these variables, different hot isostatic pressing (HIP) treatments at 800 °C, 920 °C, and 1050 °C with a 920 °C temper were applied to three sets of Ti–6Al–4V cylinders that originated from the same PBF-L build, such that there were 30 tests per condition. After HIP treatment, the specimens were machined and tested. The highest runout stress was achieved after sub-β transus HIP at 800 °C for 2 h at 200 MPa of pressure. A significant drop in fatigue strength was attributed to large prior-β grains and grain boundary α resulting from super-β transus HIP treated specimens. In conclusion, for the sub-β transus HIP specimens, differences in fatigue strength were attributed to α lath thickness, relative dislocation density, and dislocation boundary strengthening.

36 MATERIALS SCIENCE↗

Fractional Quantum Hall Effect in Weyl Semimetals

Weyl semimetal may be thought of as a gapless topological phase protected by the chiral anomaly, where the symmetries involved in the anomaly are the U(1) charge conservation and the crystal translational symmetry. The absence of a band gap in a weakly interacting Weyl semimetal is mandated by the electronic structure topology and is guaranteed as long as the symmetries and the anomaly are intact. The nontrivial topology also manifests in the Fermi arc surface states and topological response, in particular taking the form of an anomalous Hall effect in magnetic Weyl semimetals, whose magnitude is only determined by the location of the Weyl nodes in the Brillouin zone. In this work, we consider the situation when the interactions are not weak and ask whether it is possible to open a gap in a magnetic Weyl semimetal while preserving its nontrivial electronic structure topology along with the translational and the charge conservation symmetries. Surprisingly, the answer turns out to be yes. The resulting topologically ordered state provides a nontrivial realization of the fractional quantum Hall effect in three spatial dimensions in the absence of an external magnetic field, which cannot be viewed as a stack of two dimensional states. Our state contains loop excitations with nontrivial braiding statistics when linked with lattice dislocations.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Defect Production and Microstructural Feature Impact for Radiation Damage in Additively Manufactured 316 Stainless Steel

This milestone presents multi-scale modeling research results for additively manufactured 316 stainless steel. A combination of phase field, cluster dynamics, molecular dynamics, and density functional theory with machine learning is used, allowing for predictions of radiation-driven microstructural evolution in additively manufactured 316 stainless steel over a range of temperatures, damage rates, neutron spectra, and microstructures, and supporting the development of combined ion and neutron irradiation for material qualification. Informed by ion irradiation and neutron irradiation results across the Advanced Materials and Manufacturing Technologies program, we investigate the unique aspects of radiation-driven microstructure evolution in additively manufactured 316 stainless steel. In particular, we focus on understanding the impact of carbon concentration (varying, for example, between the 316L and 316H standards) on void formation; radiation-induced segregation at dislocation cells and grain boundaries; and the evolution of dislocation loops and network dislocation populations. We find that the unique characteristics of the additively manufactured microstructures must be accounted for in understanding the evolution of dislocation populations under thermal and irradiation conditions, such as the variation in sink strengths arising due to the variation in dislocation density. We also find that the radiation-induced segregation of Cr and Ni to grain boundaries and cell walls differs due to the differences in their defect sink biases. We also find that increasing the Ni content can slow vacancy diffusion, which may provide a mechanism for the observed reduction in transient swelling rate for austenitic Fe-Cr-Ni alloys with increasing Ni content. In addition, ion irradiations have shown that increasing carbon content in 316 SS results in a larger population of smaller voids, suggesting reduced vacancy diffusion. Our results show that the carbon content of additively manufactured 316 SS has a significant impact on the migration rate of defect clusters. The presence of carbon atoms results in carbon-vacancy trapping, significantly reducing the diffusion rate of vacancies. Carbon atoms may also be trapped near the surface of a void, which may reduce void growth by trapping vacancies that diffuse toward the void.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Nucleation of Grain Boundary Phases

Here, we derive a theory that describes homogeneous nucleation of grain boundary (GB) phases. Our analysis takes account of the energy resulting from the GB phase junction, the line defect separating two different GB structures, which is necessarily a dislocation as well as an elastic line force due to the jump in GB stresses. The theory provides analytic forms for the elastic interactions and the core energy of the GB phase junction that, along with the change in GB energy, determines the nucleation barrier. We apply the resulting nucleation model to simulations of GB phase transformations in tungsten. Our theory explains why under certain conditions GBs cannot spontaneously change their structure even to a lower energy state.

36 MATERIALS SCIENCE↗

Collisional Histories of Comets and Trojan Asteroids: Diopside, Magnesite, and Fayalite Impact Studies

Comets and asteroids have weathered dynamic histories, as evidenced by their rough surfaces. The Nice model describes a violent reshuffling of small bodies during the Late Heavy Bombardment, with collisions acting to grind these planetesimals away. This creates an additional source of impact material that can re-work the surfaces of the larger bodies over the lifetime of the solar system. Here, we investigate the possibility that signatures due to impacts (e.g. from micrometeoroids or meteoroids) could be detected in their spectra, and how that can be explained by the physical manifestation of shock in the crystalline structure of minerals. All impact experiments were conducted in the Johnson Space Center Experimental Impact Laboratory using the vertical gun. Impact speeds ranged from approx.2.0 km/s to approx.2.8 km/s. All experiments were conducted at room temperature. Minerals found in comets and asteroids were chosen as targets, including diopside (MgCaSi2O6, monoclinic pyroxene), magnesite (MgCO3, carbonate), and fayalite (FeSiO4, olivine). Impacted samples were analyzed using a Fourier Transform Infrared Spectrometer (FTIR) and a Transmission Electron Microscope (TEM). Absorbance features in the 8-13 m spectral region demonstrate relative amplitude changes as well as wavelength shifts. Corresponding TEM images exhibit planar shock dislocations in the crystalline structure, attributed to deformation at high strain and low temperatures. Elongating or shortening the axes of the crystalline structure of forsterite (Mg2SiO4, olivine) using a discrete dipole approximation model (Lindsay et al., submitted) yields changes in spectral features similar to those observed in our impacted laboratory minerals.

Lederer, S. M.↗

Bayesian calibration of a physics-based crystal plasticity and damage model

In this work, we present a model parameter calibration procedure for a physics-based crystal plasticity model. The calibration process utilizes a powerful statistics-based Bayesian calibration method. Calibration of the crystal plasticity parameters makes use of experimentally-measured data, i.e. compressive stress–strain response, from $\langle$100$\rangle$ and $\langle$123$\rangle$ single crystal copper dynamically loaded via Kolsky bar tests. The calibration of damage parameters is achieved using experimentally-measured free-surface velocity history data from plate impact test on $\langle$100$\rangle$ and $\langle$110$\rangle$ single crystal copper, which generates shock compression followed by dynamic tensile failure. A validation assessment is then carried out by comparing the calibrated model predictions and experimental measurements of the dynamic tensile damage generated in an impacted bicrystal copper plate. Lastly, a model-informed rationale for the experimentally-observed dependence of the spatial distribution of ductile damage (porosity) on crystallography is provided.

42 ENGINEERING↗

Nanoscale serration characteristics of additively manufactured superalloys

Structural elements made of nickel-based superalloys usually operate at high temperatures. Many surface failure mechanisms such as creep, fatigue, fretting fatigue, corrosion, and stress corrosion cracking start from the surface. Thus, studying the surface mechanical properties and deformation behavior of materials is vital in order to draw a correlation between the surface properties and failures. Herein, a nanoindentation technique was implemented to characterize surface properties of a widely used additively manufactured (AM) superalloy, i.e., Inconel 625. The specimens were tested in a range of temperatures in a vacuum chamber. Serrated plastic flow characterized by pop-in events during nanoindentation, known as Portevin-Le Chatelier (PLC) effect, was observed in all three tested elevated temperatures. This phenomenon depicts itself as bursts of plasticity in the loading section of the load-displacement curves. These bursts were studied comprehensively to explore incipient plasticity. Hertzian contact mechanics were implemented to extract the maximum shear stress beneath the indenter from the pop-in loads. The results show that the initial pop-in load increases as the temperature increases. The average initial pop-in load increases by almost four times from 300 °C to 650 °C. This was attributed to the formation of strengthening precipitates. The average size of the serrations and the magnitude of dislocation nucleation increase from 300 °C to 500 °C and decrease from 500 °C to 650 °C. Finally, the serrations are attributed to the dislocation generation and movement as well as their interaction with the solute atoms and precipitates.

36 MATERIALS SCIENCE↗