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DOE OSTI2016

Experimental studies of Micro- and Nano-grained UO 2 : Grain Growth Behavior, Sufrace Morphology, and Fracture Toughness

This activity is supported by the US Nuclear Energy Advanced Modeling and Simulation (NEAMS) Fuels Product Line (FPL) and aims at providing experimental data for the validation of the mesoscale simulation code MARMOT. MARMOT is a mesoscale multiphysics code that predicts the coevolution of microstructure and properties within reactor fuel during its lifetime in the reactor. It is an important component of the Moose-Bison-Marmot (MBM) code suite that has been developed by Idaho National Laboratory (INL) to enable next generation fuel performance modeling capability as part of the NEAMS Program FPL. In order to ensure the accuracy of the microstructure-based materials models being developed within the MARMOT code, extensive validation efforts must be carried out. In this report, we summarize the experimental efforts in FY16 including the following important experiments: (1) in-situ grain growth measurement of nano-grained UO 2 ; (2) investigation of surface morphology in micrograined UO 2 ; (3) Nano-indentation experiments on nano- and micro-grained UO 2 . The highlight of this year is: we have successfully demonstrated our capability to in-situ measure grain size development while maintaining the stoichiometry of nano-grained UO 2 materials; the experiment is, for the first time, using synchrotron X-ray diffraction to in-situ measure grain growth behavior of UO 2 .

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2017

Report on in-situ studies of flash sintering of uranium dioxide

Flash sintering is a novel type of field assisted sintering that uses an electric field and current to provide densification of materials on very short time scales. The potential for field assisted sintering techniques to be used in producing nuclear fuel is gaining recognition due to the potential economic benefits and improvements in material properties. The flash sintering behavior has so far been linked to applied and material parameters, but the underlying mechanisms active during flash sintering have yet to be identified. This report summarizes the efforts to investigate flash sintering of uranium dioxide using dilatometer studies at Los Alamos National Laboratory and two separate sets of in-situ studies at Brookhaven National Laboratory’s NSLS-II XPD-1 beamline. The purpose of the dilatometer studies was to understand individual parameter (applied and material) effects on the flash behavior and the purpose of the in-situ studies was to better understand the mechanisms active during flash sintering. As far as applied parameters, it was found that stoichiometry, or oxygen-to-metal ratio, has a significant effect on the flash behavior (time to flash and speed of flash). Composite systems were found to have degraded sintering behavior relative to pure UO 2 . The critical field studies are complete for UO 2.00 and will be analyzed against an existing model for comparison. The in-situ studies showed that the strength of the field and current are directly related to the sample temperature, with temperature-driven phase changes occurring at high values. The existence of an ‘incubation time’ has been questioned, due to a continuous change in lattice parameter values from the moment that the field is applied. Some results from the in-situ experiments, which should provide evidence regarding ion migration, are still being analyzed. Some preliminary conclusions can be made from these results with regard to using field assisted sintering to fabricate nuclear fuel. First, the pure UO 2 -based system shows promising behavior with flash sintering, but composite systems are likely to show better sintering behavior with spark plasma sintering. Efforts to develop these methods should therefore be tailored towards the likelihood of success. Additionally, modeling is a rapidly developing aspect of current flash sintering research and should be used in parallel with experiments. Ultimately, ongoing flash sintering studies on various materials, like those summarized in this report, are rapidly contributing to the feasibility of controlling this method for use in the future.

##CAI suggestions##↗
DOE OSTI2022

Charge Compensation by Iodine Covalent Bonding in Lead Iodide Perovskite Materials

Metal halide perovskite materials (MHPs) are a family of next-generation semiconductors that are enabling low-cost, high-performance solar cells and optoelectronic devices. The most-used halogen in MHPs, iodine, can supplement its octet by covalent bonding resulting in atomic charges intermediate to I− and I0. Here, we examine theoretically stabilized defects of iodine using density functional theory (DFT); defect formation enthalpies and iodine Bader charges which illustrate how MHPs adapt to stoichiometry changes. Experimentally, X-ray photoelectron spectroscopy (XPS) is used to identify perovskite defects and their relative binding energies, and validate the predicted chemical environments of iodine defects. Examining MHP samples with excess iodine compared with near stoichiometric samples, we discern additional spectral intensity in the I 3d5/2 XPS data arising from defects, and support the presence of iodine trimers. I 3d5/2 defect peak areas reveal a ratio of 2:1, matching the number of atoms at the ends and middle of the trimer, whereas their binding energies agree with calculated Bader charges. Results suggest the iodine trimer is the preferred structural motif for incorporation of excess iodine into the perovskite lattice. Understanding these easily formed photoactive defects and how to identify their presence is essential for stabilizing MHPs against photodecomposition.

36 MATERIALS SCIENCE↗
DOE OSTI2016

ION IRRADIATION OF ETHANE AND WATER MIXTURE ICE AT 15 K: IMPLICATIONS FOR THE SOLAR SYSTEM AND THE ISM

Solid water has been observed on the surface of many different astronomical objects and is the dominant ice present in the universe, from the solar system (detected on the surface of some asteroids, planets and their satellites, trans-Neptunian objects [TNOs], comets, etc.) to dense cold interstellar clouds (where interstellar dust grains are covered with water-rich ices). Ethane has been detected across the solar system, from the atmosphere of the giant planets and the surface of Saturn’s satellite Titan to various comets and TNOs. To date, there were no experiments focused on icy mixtures of C{sub 2}H{sub 6} and H{sub 2}O exposed to ion irradiation simulating cosmic rays, a case study for many astronomical environments in which C{sub 2}H{sub 6} has been detected. In this work, the radiolysis of a C{sub 2}H{sub 6}:H{sub 2}O (2:3) ice mixture bombarded by a 40 MeV{sup 58}Ni{sup 11+} ion beam is studied. The chemical evolution of the molecular species existing in the sample is monitored by a Fourier transform infrared spectrometer. The analysis of ethane, water, and molecular products in solid phase was performed. Induced chemical reactions in C{sub 2}H{sub 6}:H{sub 2}O ice produce 13 daughter molecular species. Their formation and dissociation cross sections are determined. Furthermore, atomic carbon, oxygen, and hydrogen budgets are determined and used to verify the stoichiometry of the most abundantly formed molecular species. The results are discussed in the view of solar system and interstellar medium chemistry. The study presented here should be regarded as a first step in laboratory works dedicated to simulate the effect of cosmic radiation on multicomponent mixtures involving C{sub 2}H{sub 6} and H{sub 2}O.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2016

SOFT X-RAY IRRADIATION OF SILICATES: IMPLICATIONS FOR DUST EVOLUTION IN PROTOPLANETARY DISKS

The processing of energetic photons on bare silicate grains was simulated experimentally on silicate films submitted to soft X-rays of energies up to 1.25 keV. The silicate material was prepared by means of a microwave assisted sol–gel technique. Its chemical composition reflects the Mg{sub 2}SiO{sub 4} stoichiometry with residual impurities due to the synthesis method. The experiments were performed using the spherical grating monochromator beamline at the National Synchrotron Radiation Research Center in Taiwan. We found that soft X-ray irradiation induces structural changes that can be interpreted as an amorphization of the processed silicate material. The present results may have relevant implications in the evolution of silicate materials in X-ray-irradiated protoplanetary disks.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2010

DEVELOPMENT OF CERAMIC WASTE FORMS FOR AN ADVANCED NUCLEAR FUEL CYCLE

A series of ceramic waste forms were developed and characterized for the immobilization of a Cesium/Lanthanide (CS/LN) waste stream anticipated to result from nuclear fuel reprocessing. Simple raw materials, including Al{sub 2}O{sub 3} and TiO{sub 2} were combined with simulated waste components to produce multiphase ceramics containing hollandite-type phases, perovskites (particularly BaTiO{sub 3}), pyrochlores and other minor metal titanate phases. Three fabrication methodologies were used, including melting and crystallizing, pressing and sintering, and Spark Plasma Sintering (SPS), with the intent of studying phase evolution under various sintering conditions. X-Ray Diffraction (XRD) and Scanning Electron Microscopy coupled with Energy Dispersive Spectroscopy (SEM/EDS) results showed that the partitioning of the waste elements in the sintered materials was very similar, despite varying stoichiometry of the phases formed. Identification of excess Al{sub 2}O{sub 3} via XRD and SEM/EDS in the first series of compositions led to a Phase II study, with significantly reduced Al{sub 2}O{sub 3} concentrations and increased waste loadings. The Phase II compositions generally contained a reduced amount of unreacted Al{sub 2}O{sub 3} as identified by XRD. Chemical composition measurements showed no significant issues with meeting the target compositions. However, volatilization of Cs and Mo was identified, particularly during melting, since sintering of the pressed pellets and SPS were performed at lower temperatures. Partitioning of some of the waste components was difficult to determine via XRD. SEM/EDS mapping showed that those elements, which were generally present in small concentrations, were well distributed throughout the waste forms.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2010

Direct Comparison of the X-Ray Emission and Absorption of Cerium Oxide

Bremstrahlung Isochromat Spectroscopy (BIS). The XES spectra were collected using a Specs electron gun for the excitation and the XES 350 grating monochromator and channel plate system from Scienta as the photon detection. Spectra were collected in 'normal mode,' where the electron gun kinetic energy (KE) and the energy position of the center of the channel plate were both fixed and the energy distribution in the photon (hv) spectrum was derived from the intensities distributed across the channel plate detector in the energy dispersal direction. The polycrystalline Ce sample was oxidized by exposure to air at ambient pressures. After introduction to the ultra-high vacuum system, the oxidized sample was bombarded with Ar, to clean the topmost surface region and stabilize the surface and near surface regions. Although CeO{sub 2} would be the thermodynamically preferred composition in an oxygen rich environment, the combination of a vacuum environment and ion etching may have driven the near surface region into a Ce{sub 2}O{sub 3} stoichiometry. XES data collection occurred with the sample at or near room temperature. The base pressure of the system was 3 x 10{sup -10} torr, but the pressure changed depending the energy and current of the electron gun. For example, with the XES measurements at KE = 3KeV, the pressure was approximately 8 to 9 x 10{sup -10} torr and the excitation current to the sample was typically 0.01 mA. More detail of the sample preparation and analysis can be found in Reference 1. The XAS experiments were performed at Beamline 8 of the Advance Light Source, as part of a larger collaboration. The ex situ sample used at the ALS was prepared in a fashion similar to that described above. X-ray Emission Spectroscopy (XES) and X-ray Absorption Spectroscopy (XAS), have been used to investigate the photon emission and absorption associated with the Ce3d{sub 5/2} and Ce3d{sub 3/2} core-levels in CeOxide. A comparison of the two processes and their spectra will be made. Recently, we reported the observation of a very strong resonant effect in the Resonant Inverse Photoelectron Spectroscopy of CeOxide. It has now become apparent that there is a utility in a direct comparison of the X-ray Emission Spectroscopy (XES) and X-ray Absorption Spectroscopy (XAS) of similarly prepared CeOxide samples. That comparison is made in this Brief Report/Comment.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Nanoscale Measurements of the Surface Photovoltage in Cu(In,Ga)Se2, Cu2ZnSn4, and Cu2ZnSnSe4 Thin Films: The Role of the Surface Electronics on the Efficiency of Solar Cells: Preprint

We report on recent advances in the development of nanoscale measurements of the surface photovoltage (SPV) based on scanning tunneling microscopy (STM) and its application to the kesterites Cu2ZnSnS4 (CZTS) and Cu2ZnSnSe4 (CZTSe). One critical aspect of the electronic structure of Cu(In,Ga)Se2 (CIGS) that has yet to be determined in their related kesterite compounds is the character of the surface electronics. In CIGS, spontaneous deviations in the stoichiometry of the surface cause a depletion (or even a type inversion) region that reinforces the CIGS homojunction. First-principle calculations predict that this inversion region will be more difficult to form in CZTS. In this contribution, the characteristics of the surface space charge region for both CIGS and CZTS(e) are investigated by STM. The implications of the results of these measurements on the future development of CZTS solar cells will be discussed.

14 SOLAR ENERGY↗
DOE OSTI2011

Lattice-Strain Control of Exceptional Activity in Dealloyed Core-Shell Fuel Cell Catalysts

We present a combined experimental and theoretical approach to demonstrate how lattice strain can be used to continuously tune the catalytic activity of the oxygen reduction reaction (ORR) on bimetallic nanoparticles that have been dealloyed. The sluggish kinetics of the ORR is a key barrier to the adaptation of fuel cells and currently limits their widespread use. Dealloyed Pt-Cu bimetallic nanoparticles, however, have been shown to exhibit uniquely high reactivity for this reaction. We first present evidence for the formation of a core-shell structure during dealloying, which involves removal of Cu from the surface and subsurface of the precursor nanoparticles. We then show that the resulting Pt-rich surface shell exhibits compressive strain that depends on the composition of the precursor alloy. We next demonstrate the existence of a downward shift of the Pt d-band, resulting in weakening of the bond strength of intermediate oxygenated species due to strain. Finally, we combine synthesis, strain, and catalytic reactivity in an experimental/theoretical reactivity-strain relationship which provides guidelines for the rational design of strained oxygen reduction electrocatalysts. The stoichiometry of the precursor, together with the dealloying conditions, provides experimental control over the resulting surface strain and thereby allows continuous tuning of the surface electrocatalytic reactivity - a concept that can be generalized to other catalytic reactions.

30 DIRECT ENERGY CONVERSION↗
DOE OSTI2011

Inducing Mineral Precipitation in Groundwater by Addition of Phosphate

Induced precipitation of phosphate minerals to scavenge trace metals and radionuclides from groundwater is a potential remediation approach for contaminated aquifers. Phosphate minerals can sequester trace elements by primary mineral formation, solid solution formation and/or adsorption, and they are poorly soluble under many environmental conditions, making them attractive for long-term sustainable remediation. The success of such engineered schemes will depend on the particular mineral phases generated, their rates of formation, and their long term stability. The purpose of this study was to examine the precipitation of calcium phosphate minerals under conditions representative of a natural groundwater. Because microorganisms are present in groundwater, and because some proposed schemes for induced phosphate mineral precipitation rely on the stimulation of native groundwater populations, we also tested the effect of bacterial cells (initial densities of 105 and 107 ml-1) within the precipitation medium. We also tested the effect of a trace mixture of propionic, isovaleric, formic and butyric acids (total concentration 0.035 mM). The experiments showed that the general progression of mineral precipitation was similar under all of the conditions, with initial formation of amorphous calcium carbonate, and transformation to poorly crystalline hydroxyapatite (HAP) by the end of the week-long experiments. The presence of the bacterial cells appeared to delay precipitation, although by the end of 7 days the overall extent of precipitation was similar for all of the treatments. The stoichiometry of the final precipitates as well as results of Rietveld refinement of x-ray diffraction data indicated that the treatments including organic acids and bacterial cells resulted in increased distortion of the HAP crystal lattice, with the higher concentration of cells resulting in the greatest distortion. Uptake of Sr into the phosphate minerals was decreased in the treatments with cells and organic acids, compared to the control. The results of the experiments enable a greater understanding of the challenges associated with phosphate-based remediation schemes for contaminated environments.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2011

Magnesium-Dependent Interaction of PKR with Adenovirus VAI

Protein kinase R (PKR) is an interferon-induced kinase that plays a pivotal role in the innate immunity pathway for defense against viral infection. PKR is activated to undergo autophosphorylation upon binding to RNAs that contain duplex regions. Activated PKR phosphorylates the {alpha}-subunit of eukaryotic initiation factor 2, thereby inhibiting protein synthesis in virus-infected cells. Viruses have evolved diverse PKR-inhibitory strategies to evade the antiviral response. Adenovirus encodes virus-associated RNA I (VAI), a highly structured RNA inhibitor that binds PKR but fails to activate. We have characterized the stoichiometry and affinity of PKR binding to define the mechanism of PKR inhibition by VAI. Sedimentation velocity and isothermal titration calorimetry measurements indicate that PKR interactions with VAI are modulated by Mg{sup 2+}. Two PKR monomers bind in the absence of Mg{sup 2+}, but a single monomer binds in the presence of divalent ion. Known RNA activators of PKR are capable of binding multiple PKR monomers to allow the kinase domains to come into close proximity and thus enhance dimerization. We propose that VAI acts as an inhibitor of PKR because it binds and sequesters a single PKR in the presence of divalent cation.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2011

Structure of a Eurkaryotic CLC Transporter Defines an Intermediate State in the Transport Cycle

CLC proteins transport chloride (Cl{sup -}) ions across cell membranes to control the electrical potential of muscle cells, transfer electrolytes across epithelia, and control the pH and electrolyte composition of intracellular organelles. Some members of this protein family are Cl{sup -} ion channels, whereas others are secondary active transporters that exchange Cl{sup -} ions and protons (H{sup +}) with a 2:1 stoichiometry. We have determined the structure of a eukaryotic CLC transporter at 3.5 angstrom resolution. Cytoplasmic cystathionine beta-synthase (CBS) domains are strategically positioned to regulate the ion-transport pathway, and many disease-causing mutations in human CLCs reside on the CBS-transmembrane interface. Comparison with prokaryotic CLC shows that a gating glutamate residue changes conformation and suggests a basis for 2:1 Cl{sup -}/H{sup +} exchange and a simple mechanistic connection between CLC channels and transporters.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2011

Spin-Glass Behavior of Semiconducting KxFe2-yS2

We report the discovery of K{sub x}Fe{sub 2-y}S{sub 2} single crystals, isostructural to K{sub x}Fe{sub 2-y}S{sub 2} superconductors. The sulfide compound is a small gap semiconductor and shows spin-glass behavior below 32 K. Our results indicate that stoichiometry, defects, and the local environment of FeCh (Ch = S,Se) tetrahedra have important effects on the physical properties of isostructural and isoelectronic K{sub x}Fe{sub 2-y}S{sub 2} compounds.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2011

Menzerite-(Y) a New Species {(Y REE)(Ca Fe2plus)2}[(Mg Fe2plus)(Fe3plus Al)](Si3)O12 from a Felsic Granulite Parry Sound Ontario and a New Garnet End-member (Y2Ca)Mg2(SiO4)3

Menzerite-(Y), a new mineral species, forms reddish brown cores, n = 1.844 (20), up to 70 {micro}m across, rimmed successively by euhedral almandine containing up to 2.7 wt% Y{sub 2}O{sub 3} and by K-feldspar in a felsic granulite on Bonnet Island in the interior Parry Sound domain, Grenville Orogenic Province, Canada. It is named after Georg Menzer (1897-1989), the German crystallographer who solved the crystal structure of garnet. Single-crystal X-ray-diffraction results yielded space group Ia3d, a = 11.9947(6) {angstrom}. An electron-microprobe analysis of the grain richest in Y (16.93 wt% Y{sub 2}O{sub 3}) gave the following formula, normalized to eight cations and 12 oxygen atoms: {l_brace}Y{sub 0.83}Gd{sub 0.01}Dy{sub 0.05}Ho{sub 0.02}Er{sub 0.07}Tm{sub 0.01}Yb{sub 0.06}Lu{sub 0.02}Ca{sub 1.37}Fe{sub 0.49}{sup 2+}Mn{sub 0.07}{r_brace} [Mg{sub 0.55}Fe{sub 0.42}{sup 2+}Fe{sub 0.58}{sup 3+}Al{sub 0.35} V{sub 0.01}Sc{sub 0.01}Ti{sub 0.08}](Si{sub 2.82}Al{sub 0.18})O{sub 12}, or {l_brace}(Y,REE)(Ca,Fe{sup 2+}){sub 2}{r_brace}[(Mg,Fe{sup 2+})(Fe{sup 3+},Al)](Si{sub 3})O{sub 12}. Synchrotron micro-XANES data gave Fe{sup 3+}/{Sigma}Fe = 0.56(10) versus 0.39(2) calculated from stoichiometry. The scattering power refined at the octahedral Y site, 17.68 epfu, indicates that a relatively light element contributes to its occupancy. Magnesium, as determined by electron-microprobe analyses, would be a proper candidate. In addition, considering the complex occupancy of this site, the average Y-O bond length of 2.0244(16) {angstrom} is in accord with a partial occupancy by Mg. The dominance of divalent cations with Mg > Fe{sup 2+} and the absence of Si at the octahedral Y site (in square brackets) are the primary criteria for distinguishing menzerite-(Y) from other silicate garnet species; the menzerite-(Y) end-member is {l_brace}Y{sub 2}Ca{r_brace}[Mg{sub 2}](Si{sub 3})O{sub 12}. The contacts of menzerite-(Y) with almandine are generally sharp and, in places, cuspate. It is interpreted to have equilibrated with ferrosilite, augite, quartz, oligoclase, allanite-(Ce), magnetite, ilmenite and fluorapatite, in the absence of almandine, on the prograde path at 7-8.5 kbar and T {approx} 700-800 C, and subsequently dissolved incongruently in an anatectic melt to form almandine, most likely, at P {approx} 8.5-9.5 kbar and T {approx} 800-850 C.

58 GEOSCIENCES↗
DOE OSTI2012

Irradiation Environment of the Materials Test Station

Conceptual design of the proposed Materials Test Station (MTS) at the Los Alamos Neutron Science Center (LANSCE) is now complete. The principal mission is the irradiation testing of advanced fuels and materials for fast-spectrum nuclear reactor applications. The neutron spectrum in the fuel irradiation region of MTS is sufficiently close to that of fast reactor that MTS can match the fast reactor fuel centerline temperature and temperature profile across a fuel pellet. This is an important characteristic since temperature and temperature gradients drive many phenomena related to fuel performance, such as phase stability, stoichiometry, and fission product transport. The MTS irradiation environment is also suitable in many respects for fusion materials testing. In particular, the rate of helium production relative to atomic displacements at the peak flux position in MTS matches well that of fusion reactor first wall. Nuclear transmutation of the elemental composition of the fusion alloy EUROFER97 in MTS is similar to that expected in the first wall of a fusion reactor.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2012

Density Functional Theory Calculations of Mass Transport in UO2

In this talk we present results of density functional theory (DFT) calculations of U, O and fission gas diffusion in UO{sub 2}. These processes all impact nuclear fuel performance. For example, the formation and retention of fission gas bubbles induce fuel swelling, which leads to mechanical interaction with the clad thereby increasing the probability for clad breach. Alternatively, fission gas can be released from the fuel to the plenum, which increases the pressure on the clad walls and decreases the gap thermal conductivity. The evolution of fuel microstructure features is strongly coupled to diffusion of U vacancies. Since both U and fission gas transport rates vary strongly with the O stoichiometry, it is also important to understand O diffusion. In order to better understand bulk Xe behavior in UO{sub 2{+-}x} we first calculate the relevant activation energies using DFT techniques. By analyzing a combination of Xe solution thermodynamics, migration barriers and the interaction of dissolved Xe atoms with U, we demonstrate that Xe diffusion predominantly occurs via a vacancy-mediated mechanism. Since Xe transport is closely related to diffusion of U vacancies, we have also studied the activation energy for this process. In order to explain the low value of 2.4 eV found for U migration from independent damage experiments (not thermal equilibrium) the presence of vacancy clusters must be included in the analysis. Next we investigate species transport on the (111) UO{sub 2} surface, which is motivated by the formation of small voids partially filled with fission gas atoms (bubbles) in UO{sub 2} under irradiation. Surface diffusion could be the rate-limiting step for diffusion of such bubbles, which is an alternative mechanism for mass transport in these materials. As expected, the activation energy for surface diffusion is significantly lower than for bulk transport. These results are further discussed in terms of engineering-scale fission gas release models. Finally, oxidation of UO{sub 2} and the importance of cluster formation for understanding thermodynamic and kinetic properties of UO{sub 2+x} are investigated.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗