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DOE OSTI2020

Ni5Ga3 Catalysts for CO2 Reduction to Methanol: Exploring the Role of Ga Surface Oxidation/reductions on Catalytic Activity

Ad-Ni5Ga3/SiO2 catalyst, which is highly active and stable for thermal CO2 hydrogenation to methanol, was investigated to understand its surface dynamics during reaction conditions. The catalyst was prepared, tested and characterized using a multitude of techniques, including ex-situ XRD, TEM, H2-TPR, CO chemisorption and in-situ ETEM and APXPS. The formation of Ga2O3 upon air exposure was observed and the consequences on catalytic activity were investigated. Results revealed that upon air exposure Ga migrates from the subsurface region to the surface of the nanoparticles forming a Ga-oxide shell surrounding a metallic core. The oxide shell can be reduced completely at high temperatures and the temperature of the reduction activation treatment plays a crucial role on the catalytic activity. This air exposure-reduction procedure results in a redistribution of the Ga species in the surface/subsurface region, promoted by a higher Ga affinity for oxygen. XRD analysis of the post-reaction samples provide evidence for the partial transformation of a Ni5Ga3 intermetallic phase into a Ni-rich Ni3Ga phase. APXPS data indicate that the Ni-rich phase forms in the subsurface region. A Ga-rich phase exists on the surface, where the Ni/Ga ratio reaches 2/3 upon activation in hydrogen. At low reduction temperatures an amorphous Ga2O3 shell remains, indicating a promotion effect on methanol synthesis activity.

Ni-Ga, intermetallic, methanol synthesis, in-situ ↗

DOE OSTI2014

Synthesis, characterization, and hydrogen uptake studies of magnesium nanoparticles by solution reduction method

Graphical abstract: X-ray diffraction (XRD) pattern of magnesium nanoparticles synthesized by solution reduction method with and without TOPO. - Highlights: • Simple and convenient method of preparing Mg nanoparticles. • Characterized by XRD, SEM, FESEM and TEM. • Trioctylphosphine oxide offers a greater control over the size of the particles. • Hydrogen uptake of samples at different temperatures and pressure of 4.5 MPa. - Abstract: Facile and simple, surfactant-mediated solution reduction method was used to synthesize monodisperse magnesium nanoparticles. Little amount of magnesium oxide nanoparticles were also formed due to the presence of TOPO and easy oxidation of magnesium, eventhough, all precautions were taken to avoid oxidation of the sample. Precise size control of particles was achieved by carefully varying the concentration ratio of two different types of surfactants, – trioctylphosphine oxide and hexadecylamine. Recrystallized magnesium nanoparticle samples with and without TOPO were analyzed by X-ray diffraction, scanning electron microscope, field emission scanning electron microscope, and transmission electron microscope. The peak diameters of particles were estimated from size distribution analysis of the morphological data. The particles synthesized in the presence and absence of TOPO found to have diameters 46.5 and 34.8 nm, respectively. This observed dependence of particle size on the presence of TOPO offers a convenient method to control the particle size by simply using appropriate surfactant concentrations. Exceptional enhancement in hydrogen uptake and kinetics in synthesized magnesium nanoparticles as compared to commercial magnesium sample was due to the smaller particle size and improved morphology. Overall hydrogen uptake not affected by the little variation in particle size with and without TOPO.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Investigating the use of in situ liquid cell scanning transmission electron microscopy

Engineering nanoparticles with desired shape-dependent properties is the key to many applications in nanotechnology. Although many synthetic procedures exist to produce anisotropic gold nanoparticles, the dynamics of growth are typically unknown or hypothetical. In the case of seed-mediated growth in the presence of DNA into anisotropic nanoparticles, it is not known exactly how DNA directs growth into specific morphologies. A series of preliminary experiments were carried out to contribute to the investigation of the possible mechanism of DNA-mediated growth of gold nanoprisms into gold nanostars using liquid cell scanning transmission electron microscopy (STEM). Imaging in the liquid phase was achieved through the use of a liquid cell platform and liquid cell holder that allow the sample to be contained within a “chip sandwich” between two electron transparent windows. Ex situ growth experiments were performed using Au-T30 NPrisms (30-base thymine oligonucleotide-coated gold nanoprisms) that are expected to grow into gold nanostars. Growth to form these nanostars were imaged using TEM (transmission electron microscopy) and liquid cell STEM (scanning transmission electron microscopy). An attempt to perform in situ growth experiments with the same Au-T30 nanoprisms revealed challenges in obtaining desired morphology results due to the environmental differences within the liquid cell compared to the ex situ environment. Different parameters in the experimental method were explored including fluid line set up, simultaneous and alternating reagent addition, and the effect of different liquid cell volumes to ensure adequate flow of reagents into the liquid cell. Lastly, the binding affinities were compared for T30 and A30 DNA incubated with gold nanoparticles using zeta potential measurements, absorption spectroscopy, and isothermal titration calorimetry (ITC). It was previously reported thymine bases have a lower binding affinity to gold surfaces than adenine bases. However, the results reported here contradict the previously reported data. Future prospectives on this work are outlined.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Microstructure and fission products in the UCO kernel of an AGR-1 TRISO fuel particle after post irradiation safety testing

Tristructural isotropic (TRISO) coated particle fuel as a key fuel concept for the High Temperature Gas-cooled Reactors (HTGRs) and a candidate accident tolerant fuel (ATF) has been currently investigated under the US-DOE Advanced Gas Reactor (AGR) fuel development and qualification program. Over the past decades, extensive studies have been conducted to evaluate the fission product release, diffusion on Ag, Pd and Cd in the SiC layer and the TRISO coating system, and post-safety-test performance. However, to date, there are limited reported results on the fuel kernels’ response to irradiation with or without post irradiation high temperature annealing. To incrementally fulfill this knowledge gap extensive studies using transmission electron microscopes (TEM) and atom probe tomography (APT) were conducted on a TRISO fuel particle kernel with a 19.74% 235U enrichment, irradiated to 18.63% FIMA and subsequently subjected to post-safety testing at 1600ºC for 300 hours.. Microstructure characterizations, elemental analysis, and phase identification were conducted using conventional TEM and scanning TEM (STEM) imaging, energy-dispersive X-ray spectroscopy (EDS), selected-area electron diffraction (SAED) and atom probe tomography (APT). The following findings were made: (1) significant reconstructions and phase evolutions occurred in the irradiated and post-safety annealed fuel kernel, and its microstructure consists of two primary phases, namely a “high-Z (atomic mass)” UC phase and a “low-Z” UO phase, (2) no fission gas bubbles are identified within the fuel kernel, that can be attributed to the high temperature post safety annealing, (3) fission products Zr, Nb, Mo, Ru, Tc and Rh were found to preferentially segregate into UC phase or to form metallic precipitates, while the lanthanide fission products tend to stay in the solution of UO phase, (4) Pd was detected in the rod-shaped precipitates, (5) APT data reveals segregation of Te, Pd, and Ag at the UO and UC phase boundary, and (6) Pd is detected in both the UO and UC phases but with an enrichment in the former one.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2020

Biomineralization of Cu 2 S Nanoparticles by Geobacter sulfurreducens

Biomineralization of Cu has been shown to control contaminant dynamics and transport in soils. However, very little is known about the role that subsurface microorganisms may play in the biogeochemical cycling of Cu. In this study, we investigate the bioreduction of Cu(II) by the subsurface metal-reducing bacterium Geobacter sulfurreducens. Rapid removal of Cu from solution was observed in cell suspensions of G. sulfurreducens when Cu(II) was supplied, while transmission electron microscopy (TEM) analyses showed the formation of electron-dense nanoparticles associated with the cell surface. Energy-dispersive X-ray spectroscopy (EDX) point analysis and EDX spectrum image maps revealed that the nanoparticles are rich in both Cu and S. This finding was confirmed by X-ray absorption near-edge structure (XANES) and extended X-ray absorption fine structure (EXAFS) analyses, which identified the nanoparticles as Cu 2 S. Biomineralization of Cu x S nanoparticles in soils has been reported to enhance the colloidal transport of a number of contaminants, including Pb, Cd, and Hg. However, formation of these Cu x S nanoparticles has only been observed under sulfate-reducing conditions and could not be repeated using isolates of implicated organisms. As G. sulfurreducens is unable to respire sulfate, and no reducible sulfur was supplied to the cells, these data suggest a novel mechanism for the biomineralization of Cu 2 S under anoxic conditions. The implications of these findings for the biogeochemical cycling of Cu and other metals as well as the green production of Cu catalysts are discussed.

59 BASIC BIOLOGICAL SCIENCES↗

NASA NTRS2020

Inverse Compton Cooling in the Coronae of Simulated Black Hole Accretion Flows

We present a formulation for a local cooling function to be employed in the diffuse, hot corona region of 3D GRMHD simulations of accreting black holes. This new cooling function calculates the cooling rate due to inverse Compton scattering by considering the relevant microphysics in each cell in the corona and approximating the radiation energy density and Compton temperature there by integrating over the thermal seed photon flux from the disk surface. The method either assumes ion and electron tem- peratures are equal (1T), or calculates them separately (2T) using an instantaneous equilibrium approach predicated on the actual relevant rate equations (Coulomb and Compton). The method is shown to be consistent with a more detailed ray-tracing calculation where the bulk of the cooling occurs, but is substantially less costly to per- form. As an example, we apply these methods to a harm3d simulation of a 10M⊙, non-spinning black hole, accreting at nominally 1% the Eddington value. Both 1T and 2T approaches lead to increased radiative efficiency and a larger fraction of total cooling in the corona as compared to the original target-temperature cooling function used by harm3d, especially in the 1T case. Time-averaged post-processing reveals that the continuum spectral observations predicted from these simulations are qualitatively similar to actual X-ray binary data, especially so for the 1T approach which yields a harder power-law component (Γ = 2.25) compared to the 2T version (Γ = 2.53).

Brooks E. Kinch↗

NASA NTRSDate not supplied

Error Sources and Mitigation Strategies for Thermocouples Integrated in Flexible Thermal Protection System Materials

Brief Presenter Biography:Ruth Miller is an aer-ospace systems engineer in the Entry Systems and Ve-hicle Development Branch at NASA Ames Research Center.Introduction:The flexible thermal protection sys-tem (FTPS) on NASA’s Low-Earth Orbit Flight Test of an Inflatable Decelerator (LOFTID) vehicle will be in-strumented with thermocouples (TCs) to measure the in-depth thermal response during entry into Earth’s atmos-phere[1, 2]. Accurate flight temperature measurements are critical for verifying vehicle performance during the flight test and reducing uncertainties in the thermal models.However,the deployable nature of inflatable decelerator technology presents challengesfor integrat-ing TCs, specifically the TCsneed to be compactableand cannot damage the FTPSnor the inflatable structure(IS).Unlike traditional rigid aeroshells, routing TCsthrough the thickness of the FTPS could cause signifi-cant damage during packing of the deployable aeroshellbecause the different layers may shift small amounts in relation to each other imparting strain on the TCsand FTPS materials. The LOFTID TCleads are routed from the measurement location back to the data acquisition system in the vehicle centerbody within the same FTPS layer that they are monitoring the temperature. This ap-proach eliminates the need to put holes in the FTPS lay-ers,butas a consequence,the insulated TCleads travel for an appreciable distance through a region that will expose them to high temperaturesand large thermal gra-dients.LOFTID’s TCswere baselined to be commercially available Type K TCswith a binder impregnated glass braid insulation. These TCswere chosen because they had been used successfully on IRVE-3 and in ground-based arc jet testing. Additionally, these TCsdid notdamage the FTPS nor IS during packing and deploy-ment testing. However, the glass braid insulation is only rated to a maximum continuous use temperature of 482ºC. For reference, the duration of the heat pulse on the LOFTID vehicle is on the order of minutes and themaximum predicted temperaturebeneaththe outermost FTPS layersis 1350ºC.Ground-based testing in a tube furnace at NASA Ames Research Centerwas conducted to determine if the baseline TCsrouted through FTPS samples would survive and provide accurate temperature measure-mentsat LOFTID flight-relevant temperatures[3].The test results showed large measurement errors occurred beginning at approximately 400°C due to conductive deposits on the TCinsulation electrically shorting the TCleads.The conductive deposits and thus electrical shorting weredetermined to be caused by twoerror sources:1.The organic binder on the TCinsulation carbon-izingin a high temperature, low oxygen envi-ronment2.Decomposition products from the FTPSperme-atingthe braided TC insulationFurther testing in the tube furnace demonstrated that heat cleaning the TCinsulation effectivelyremovedthe organic binder andeliminatedthe first error source.The second error sourcewas shown to be mitigated by the addition of amica wraparound each individual TCleadtoact as an impermeable barrier.To understand the applicability of theground-based tube furnace test results to flight,anarc jet testseriesat Boeing’s Large Core Arc Tunnel (LCAT) facilitywas conducted[4].The error sourcesand mitigation strate-giesidentified in the tube furnace testing were substan-tiatedin the arc jet testing.However, the arc jet testing also revealed three new error sources:1.Glass TCinsulation meltingwhich resultsin electrical shorting of the TCeither through di-rect contact between the two leads or through the electrically conductive FTPS materials2.TCwire meltingwhich results in a noisy and/or open-loop TCresponse3.Type K TCwire green-rotwhich results in large calibration errors Scope of the Presentation:This presentation will include a brief discussion onthe effect of electrical shorting on the output of a TC(i.e. how to identify elec-trical shorting in TCdataand what the associated erroris).The tube furnace and arc jet test resultswill be dis-cussedand the solutions LOFTID is implementing to mitigate the error sourcesidentified in the tube furnace and arc jet testingwill be presented.Additionally, futureresearch and development work to eliminateTCerror sourcesfor future missionswill be recommended.

R A Miller↗

NASA NTRS1987

Morphometrics of cellular damage in mice testis receiving X-ray and high-energy particle irradiation

Murine tests were exposed to single, low doses of either X-ray, helium, or argon radiation. Animals were sacrificed seventy-two hours later. Testes were fixed for transmission electron microscopy (TEM) and sectioned at either 60 nm for TEM observation or at 2 micron for counting using routine light microscope methods. Counts of the total population of surviving spermatogonia, including all type A cells, intermediate, and type B cells, were taken from tubule cross sections identified as Stage 6 and Stage 1 according to spermatogonial configuration. The surviving fraction of spermatogonia as compared to control, S/S sub o, was calculated for each dose. For both ions and X-rays, there was a rapid decline in survival at dose levels of .10 to .15 Gy in Stage 6 tubules. This was followed by a more gradual decrease in population. At higher doses, 0.30 Gy for argon and 0.80 Gy for helium and X-rays, the cell survival rates declined rapidly. Pre-leptotene spermatocytes in Stage 1 tubules exhibited a different survival curve indicating the extreme radio-sensitivity of type B spermatogonia. Data verify that the seminiferous tubules are composed of a heterogeneous population of cells with different radio-sensitivities and that these differences are manifested even at very low doses.

Sapp, Walter J.↗

DOE OSTI2019

Multi-axial and multi-energy channeling study of disorder evolution in ion-irradiated nickel

In this study, to better understand defect structure and the evolution of irradiation-induced damage in single crystal Ni, in situ Rutherford backscattering spectroscopy in channeling geometry (RBS/C) is performed along the <100>, <110>, and <211> axes with different probing beam energies. The RBS/C data reveal that damage evolution occurs in three steps. The first step at low doses (up to 0.2 dpa), characterized by a linear increase with dose, is related to the formation of point defects and small clusters. The second step in the intermediate dose range (0.2–1.0 dpa) shows a sublinear increase in disorder to saturation. This sublinear increase is due to the growth of defect clusters resulting from the interaction of irradiation-induced defects with already existing damage from previous ion impacts. The third step at high doses (1.0–32.4 dpa) exhibits a surprising decrease in the disorder level, which may be attributed to defect evolution from black spot defects to large dislocation loops that leads to strain relaxation. In addition, the damage extends much deeper than the predicted depths and is attributed to long-range defect migration effects confirmed by transmission electron microscopy (TEM) observations. Although similar damage evolution trends have been observed along all channeling directions, the disorder accumulation is largest along the <100> and <211> axes than observed along <110> axis. This “preferential” disordering process along <100> and <211> suggests that more defects are shielded by the <110> atomic rows than the two other axes. Finally, the co-existence of both uncorrelated displaced lattice atoms and dislocation loops in Ni irradiated at 1 ion/nm 2 is revealed by the energy-dependent RBS/C studies along all three axes. In contrast, dislocation loops and stacking fault tetrahedral are simultaneously present in the crystal structure of Ni irradiated at 100 ions/nm 2 that is consistent with previous molecular dynamics simulations and TEM observations.

36 MATERIALS SCIENCE↗

DOE OSTI2016

How Do Radionuclides Accumulate in Marine Organisms? A Case Study of Europium with Aplysina cavernicola

In the ocean, complex interactions between natural and anthropogenic radionuclides, seawater, and diverse marine biota provide a unique window through which to examine ecosystem and trophic transfer mechanisms in cases of accidental dissemination. The nature of interaction between radionuclides, the marine environment, and marine species is therefore essential for better understanding transfer mechanisms from the hydrosphere to the biosphere. Although data pertaining to the rate of global transfer are often available, little is known regarding the mechanism of environmental transport and uptake of heavy radionuclides by marine species. Among marine species, sponges are immobile active filter feeders and have been identified as hyperaccumulators of several heavy metals. We have selected the Mediterranean sponge Aplysina cavernicola as a model species for this study. Actinide elements are not the only source of radioactive release in cases of civilian nuclear events; however, their physicochemical transfer mechanisms to marine species remain largely unknown. We have targeted europium(III) as a representative of the trivalent actinides such as americium or curium. To unravel biological uptake mechanisms of europium in A. cavernicola, we have combined radiometric (γ) measurements with spectroscopic (time-resolved laser-induced fluorescence spectroscopy, TRLIFS, and X-ray absorption near-edge structure, XANES) and imaging (transmission electron microscopy, TEM, and scanning transmission X-ray microscopy, STXM) techniques. Here, we have observed that the colloids of NaEu(CO 3 ) 2 ·nH 2 O formed in seawater are taken up by A. cavernicola with no evidence that lethal dose has been reached in our working conditions. Spectroscopic results suggest that there is no change of speciation during uptake. Finally, TEM and STXM images recorded at different locations across a sponge cross section, together with differential cell separation, indicate the presence of europium particles (around 200 nm) mainly located in the skeleton and toward the outer surface of the sponge.

63 RADIATION, THERMAL, AND OTHER ENVIRON. POLLUTAN↗

NASA NTRS2010

Thermal Infrared Emission Spectroscopy of Synthetic Allophane and its Potential Formation on Mars

Allophane is a poorly-crystalline, hydrous aluminosilicate with variable Si/Al ratios approx.0.5-1 and a metastable precursor of clay minerals. On Earth, it forms rapidly by aqueous alteration of volcanic glass under neutral to slightly acidic conditions [1]. Based on in situ chemical measurements and the identification of alteration phases [2-4], the Martian surface is interpreted to have been chemically weathered on local to regional scales. Chemical models of altered surfaces detected by the Mars Exploration Rover Spirit in Gusev crater suggest the presence of an allophane-like alteration product [3]. Thermal infrared (TIR) spectroscopy and spectral deconvolution models are primary tools for determining the mineralogy of the Martian surface [5]. Spectral models of data from the Thermal Emission Spectrometer (TES) indicate a global compositional dichotomy, where high latitudes tend to be enriched in a high-silica material [6,7], interpreted as high-silica, K-rich volcanic glass [6,8]. However, later interpretations proposed that the high-silica material may be an alteration product (such as amorphous silica, clay minerals, or allophane) and that high latitude surfaces are chemically weathered [9-11]. A TIR spectral library of pure minerals is available for the public [12], but it does not contain allophane spectra. The identification of allophane on the Martian surface would indicate high water activity at the time of its formation and would help constrain the aqueous alteration environment [13,14]. The addition of allophane to the spectral library is necessary to address the global compositional dichotomy. In this study, we characterize a synthetic allophane by IR spectroscopy, X-ray diffraction (XRD), and transmission electron microscopy (TEM) to create an IR emission spectrum of pure allophane for the Mars science community to use in Martian spectral models.

Rampe, E. B.↗

NASA NTRS2014

Chemical Zoning of Feldspars in Lunar Granitoids: Implications for the Origins of Lunar Silicic Magmas

Fine-scale chemical and textural measurements of alkali and plagioclase feldspars in the Apollo granitoids (ex. Fig. 1) can be used to address their petrologic origin(s). Recent findings suggest that these granitoids may hold clues of global importance, rather than of only local significance for small-scale fractionation. Observations of morphological features that resemble silicic domes on the unsampled portion of the Moon suggest that local, sizable net-works of high-silica melt (>65 wt % SiO2) were present during crust-formation. Remote sensing data from these regions suggest high concentrations of Si and heat-producing elements (K, U, and Th). To help under-stand the role of high-silica melts in the chemical differentiation of the Moon, three questions must be answered: (1) when were these magmas generated?, (2) what was the source material?, and (3) were these magmas produced from internal differentiation. or impact melting and crystallization? Here we focus on #3. It is difficult to produce high-silica melts solely by fractional crystallization. Partial melting of preexisting crust may therefore also have been important and pos-sibly the primary mechanism that produced the silicic magmas on the Moon. Experimental studies demonstrate that partial melting of gabbroic rock under mildly hydrated conditions can produce high-silica compositions and it has been suggested by that partial melting by basaltic underplating is the mechanism by which high-silica melts were produced on the Moon. TEM and SIMS analyses, coordinated with isotopic dating and tracer studies, can help test whether the minerals in the Apollo granitoids formed in a plutonic setting or were the result of impact-induced partial melting. We analyzed granitoid clasts from 3 Apollo samples: polymict breccia 12013,141, crystalline-matrix breccia 14303,353, and breccia 15405,78

Mills, R. D↗

DOE OSTI2017

DE-NE0000724 - Research Performance Final Report - Investigation of Thermal Aging Effects on the Evolution of Microstructure and Mechanical Properties of Cast Duplex Stainless Steels

This report details the research activities carried out under DOE-NEUP award number DE-NE0000724 concerning the evolution of structural and mechanical properties during thermal aging of CF–3 and CF–8 cast duplex stainless steels (CDSS). The overall objective of this project was to use state-of-the-art characterization techniques to elucidate trends and phenomena in the mechanical and structural evolution of cast duplex stainless steels (CDSS) during thermal aging. These steels are commonly used as structural materials in commercial light water nuclear power plants, undergoing aging for decades in operation as cooling water pipes, pump casings, valve bodies, etc. During extended exposure to these conditions, CDSS are known to undergo a change in mechanical properties resulting in a loss of ductility, i.e. embrittlement. While it is generally accepted that structural changes within the ferrite phase, such as decomposition into iron (Fe)-rich and chromium (Cr)-rich domains, lead to the bulk embrittlement of the steels, many questions remain as to the mechanisms of embrittlement at multiple length scales. This work is intended to shed insight into the atomic level composition changes, associated kinetic mechanisms, and effects of changing phase structure on micro- and nano-scale deformation that lead to loss of impact toughness and tensile ductility in these steels. In general, this project provides a route to answer some of these major questions using techniques such as 3-dimensional (3-D) atom probe tomography (APT) and real-microstructure finite element method (FEM) modeling, which were not readily available when these steels were originally selected for service in light water reactors. Mechanical properties evaluated by Charpy V-notch impact testing (CVN), tensile testing, and microhardness and nanohardness measurements were obtained for each condition and compared with the initial baseline properties to view trends in deformation behavior during aging. Concurrent analysis of the microstructure and nanostructure by atom probe tomography (APT) and transmission electron microscopy (TEM) provide mechanistic insight into the kinetic and mechanical behavior occurring on the nano-scale. The presence and morphology of the ferrite, austenite, and carbide phases have been characterized, and formation of new phases during aging, including spinodal decomposition products (α- and α'-ferrite) and G-phase, have been observed. The mechanical and structural characterization have been used to create accurate FEM models based on the real micro- and nano-structures of the systems. These models provide new insight into the local deformation behavior of these steels and the effects of each individual phase (including ferrite, austenite, carbides, and spinodal decomposition products) on the evolving bulk mechanical behavior of the system. The project was divided into three major tasks: 1. Initial Microstructure and Mechanical Property Survey and Initiate Heat Treatment; 2. Microstructural Characterization and Mechanical Property Testing During Aging; and 3. Microstructure-based Finite Element Modeling. Each of these tasks was successfully executed, resulting in reliable data and analysis that add to the overall body of work on the CDSS materials. Baseline properties and aging trends in mechanical data confirm prior observations and add new insights into the mechanical behavior of the steels. Structural characterization on multiple length scales provides new information on phase changes occurring during aging and sheds light on the kinetic processes occurring at the atomic scale. Furthermore, a combination of mechanical testing and microstructural characterization techniques was utilized to design FEM models of local deformation behavior of the ferrite and austenite phases, providing valuable new information regarding the effects of each of the microstructural components on the hardening and embrittlement processes. The data and analysis presented in this report and the publication associated with this project (§V) increase the understanding of aging and deformation in CF–3 and CF–8 steels. These results provide valuable information that can be utilized to aid in making informed decisions regarding the ongoing use of these steels in commercial nuclear infrastructure.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2015

Investigations of element spatial correlation in Mn-promoted Co-based Fischer–Tropsch synthesis catalysts

Making connections between performance and structure in bimetallic catalysts requires knowledge of how the two elements are spatially associated. Elemental maps obtained by analytical TEM methods are an invaluable tool for identifying the location of different elements, but for many samples, visual inspection of elemental maps is insufficient for assessing the degree of element spatial correlation. This is particularly true for beam-sensitive materials where short mapping acquisition times lead to images with high noise and low color depth. In these situations, statistical analysis of elemental maps can be used to identify spatial correlations among the elements in a sample. In this work, the relationship between catalyst performance and bimetallic spatial association was explored using Mn-promoted Co-based Fischer-Tropsch synthesis catalysts prepared by different pretreatment methods. Mn was used as a catalyst additive to suppress methane formation. Catalysts that underwent calcination before reduction produced more methane and fewer long-chain hydrocarbons than catalysts that were directly reduced. The extent to which Co and Mn were spatially associated was assessed using correlation metrics, colocation plots, and histograms generated using data from STEM-EDS maps. Although both catalysts yielded visually similar elemental maps, the results of statistical analysis suggested that the calcined catalyst exhibited greater spatial segregation between the Co and Mn. These findings support the hypothesis that having Mn in close proximity to the Co is essential for the manifestation of Mn promotion effects in Co-based FTS catalysts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2019

Mechanical properties of single-crystal tungsten irradiated in a mixed spectrum fission reactor

To collect data for fusion applications and understand the basic properties of tungsten, single-crystal tungsten was neutron irradiated in the mixed-spectrum High Flux Isotope Reactor at the Oak Ridge National Laboratory at temperatures of 90–830 °C to fast fluences of 0.01–9 × 10 25 n/m 2 (E > 0.1 MeV). For tensile tests at room temperature of the irradiated material in both orientations, <110> and <100> tensile orientation, initially there was strengthening that peaked at 0.02 dpa and was followed by progressive modulus of toughness reduction, approaching zero at higher doses. For all irradiation temperatures, in elevated temperature tensile tests there was a distinct transition from ductile-to-brittle behavior between 0.1 and 0.4 dpa, accompanied by an increase in indentation hardness. The ductile-to-brittle transition with increasing dose was particularly critical because it presented as a total loss in elongation and modulus of toughness. The critical transition dose was well below the dose (~1 dpa) where irradiation-induced precipitates are visible in the TEM. The extent of Vickers microhardness increase was significant at higher doses and did not depend on irradiation temperature or crystal orientation, reaching 12.9 GPa after 2.8 dpa. Furthermore, the significant mechanical property degradation above 0.1 dpa is believed to have been caused by the accumulation of irradiation-induced clusters and eventually precipitates of the transmutation elements Re and Os.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Atomic electron tomography in three and four dimensions

Atomic electron tomography (AET) has become a powerful tool for atomic-scale structural characterization in three and four dimensions. It provides the ability to correlate structures and properties of materials at the single-atom level. With recent advances in data acquisition methods, iterative three-dimensional (3D) reconstruction algorithms, and post-processing methods, AET can now determine 3D atomic coordinates and chemical species with sub-Angstrom precision, and reveal their atomic-scale time evolution during dynamical processes. In this work, we review the recent experimental and algorithmic developments of AET and highlight several groundbreaking experiments, which include pinpointing the 3D atom positions and chemical order/disorder in technologically relevant materials and capturing how atoms rearrange during early nucleation at four-dimensional atomic resolution.

30 DIRECT ENERGY CONVERSION↗

NASA NTRSDate not supplied

Performance of a Regenerative Fuel Cell System for the Lunar Surface

Regenerative fuel cells (RFCs) are an attractive energy storage solution for lunar missions as a technology capable of providing a higher specific energy (i.e., W∙h/kg) than state-of-the-art packaged Li-ion battery systems. An RFC consists of the (1 & 2) electrochemical stacks (chemical to electrical energy conversion to supply electricity to an external load, i.e. the fuel cell reaction, and electrical to chemical energy conversion of supplied electrical power to dissociate water into hydrogen and oxygen gases, i.e. water electrolysis), (3) fluidic conditioning, (4) reactant storage, (5) avionics, (6) power management and distribution (PMAD), and (7) thermal management. NASA’s Glenn Research Center has designed, assembled, and tested a breadboard RFC sys-tem capable of operating autonomously for multiple simulated lunar day/night cycles in a laboratory environment. The system is comprised of a non-flow through proton exchange membrane (PEM) fuel cell stack and a liquid-anode feed PEM electrolyzer (EZ) stack designed to electrochemically compress the reactants at balanced pressures up to 12.4 MPa (1800 psia). The fluidic conditioning, avionics, PMAD, and thermal management sub-systems are largely comprised of commercial-off-the-shelf components for this system-level development effort. The hardware is controlled by a CubeSat space processor running an operational program based on core flight architecture that can control the RFC hardware autonomously through a state machine with fault monitoring. The testing results highlighted here were completed with the system in an open-loop configuration such that reactants generated through water electrolysis were vented while gas cylinders supplied fuel cell operation. The breadboard operated autonomously, but there were five unplanned transitions to a safe state that required a manual restart after reviewing the data, determining a root cause, and implementing a solution. Four of the transitions were caused by the thermal management subsystem and the fifth was caused by a water management control issue in the EZ sub-system. The RFC system operated for over 550 hours with the final cycle being slightly abbreviated due to reasons unrelated to system performance.

Kerrigan Cain↗

NASA NTRSDate not supplied

Performance of a Regenerative Fuel Cell System for the Lunar Surface

Kerrigan Cain↗