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Wu, Yaqiao

Publications and source records attributed to Wu, Yaqiao.

At least 55 records · Page 3

UNIRRADIATED

This is the mechanical testing data archive from a neutron irradiation campaign of nuclear structural alloys fabricated by powder metallurgy with hot isostatic pressing (PM-HIP). Data in this archive include uniaxial tensile testing data, fractography of selected tensile bars, and nanoindentation. The irradiation campaign was designed to facilitate a direct comparison of PM-HIP to conventional casting or forging. Five common nuclear structural alloys were included in the campaign: 316L stainless steel, SA508 pressure vessel steel, Grade 91 ferritic steel, and Ni-base alloys 625 and 690. Irradiations were carried out in the Advanced Test Reactor (ATR) at Idaho National Laboratory (INL) to target doses of 1 and 3 displacements per atom (dpa) at target temperatures of 300ºC and 400ºC through the DOE Office of Nuclear Energy, Nuclear Science User Facilities (NSUF) project 15-8242.

Wharry, Janelle↗

TEM Characterization of Neutron Irradiated HfAl3-Al Composite Specimens

Particles comprised of a thermal neutron absorbing material (HfAl3) are dispersed in a metal matrix material with high thermal conductivity (aluminum) to conduct the heat generated by neutron capture away from the fuel and materials. This metal matrix composite is very promising for use as a conduction-cooled neutron absorber and has the potential to be useful as a shroud or heat sink for testing advanced fast reactor fuels and materials in an existing thermal reactor. To design and optimize the absorber block system for advanced reactor designs, fundamental understanding of the irradiation effect on material properties is necessary. This dataset contains TEM characterization results of neutron irradiated HfAl3-Al composite specimens. It is focused on the irradiation induced defects (dislocation lines and loops) characterization using the on-zone axis bright field STEM technique. This data was collected using a FEI Tecnai G2 F30 S/TEM at the Microscopy and Characterization Suite (MaCS), Center for Advanced Energy Studies (CAES).

Guillen, Donna↗

TEM Characterization of Neutron Irradiated HfAl3-Al Composite Specimens

Particles comprised of a thermal neutron absorbing material (HfAl3) are dispersed in a metal matrix material with high thermal conductivity (aluminum) to conduct the heat generated by neutron capture away from the fuel and materials. This metal matrix composite is very promising for use as a conduction-cooled neutron absorber and has the potential to be useful as a shroud or heat sink for testing advanced fast reactor fuels and materials in an existing thermal reactor. To design and optimize the absorber block system for advanced reactor designs, fundamental understanding of the irradiation effect on material properties is necessary. This dataset contains TEM characterization results of neutron irradiated HfAl3-Al composite specimens. It is focused on the irradiation induced defects (dislocation lines and loops) characterization using the on-zone axis bright field STEM technique. This data was collected using a FEI Tecnai G2 F30 S/TEM at the Microscopy and Characterization Suite (MaCS), Center for Advanced Energy Studies (CAES).

Guillen, Donna↗

Transmission electron microscopy of ion irradiated ODS MA956 samples

Oxide dispersion strengthened (ODS) alloys are promising candidate materials for the next generation advanced nuclear reactors due to their superior irradiation resistance and mechanical properties. To better understand the effect of irradiation on MA956, it is essential to study higher dose (50-100 dpa) samples, so that the general trend of microstructural evolution and the resulting radiation-hardening can be deduced. Currently, ion irradiations are considered the only way to achieve doses beyond ~50 dpa in a practical time frame relevant to alloy and welding development programs. This dataset contains TEM characterization results of ODS MA956 samples that were ion irradiated under different conditions: Sample #5 (1.25 dpa at 190℃); Sample #9 (50 dpa at 190℃); Sample #15 (1.25dpa under 320℃); and Sample 17 (25 dpa at 320℃). TEM characterization focused on the irradiation induced defects (dislocation lines and loops) using the on-zone axis bright field STEM technique. These data were collected using a FEI Tecnai G2 F30 S/TEM at Microscopy and Characterization Suite (MaCS) at Center for Advanced Energy Studies (CAES), Idaho Falls, ID. This project (ion irradiation and TEM studies) was supported by the U.S. Department of Energy, Office of Nuclear Energy under DOE Idaho Operations Office Contract DE-AC07-05ID14517 as part of Nuclear Science User Facilities award #18-14784 (PI: Ramprashad Prabhakaran, PNNL).

Prabhakaran, Ramprashad↗

Atom probe tomography of segregation at grain boundaries and gas bubbles in neutron irradiated U-10 wt% Mo fuel

During neutron irradiation to fission densities > 5.2 × 10 21 fiss/cm 3 , Xe agglomerates forming gas bubbles of varying size within the U-Mo fuel matrix. Herein, segregation of fission products to Xe bubbles and grain boundaries (GB) were studied using atom probe tomography (APT). Segregation behavior was found to vary among GBs, small bubbles (<10 nm), and larger bubbles (>10 nm). Solid fission products were enriched at GBs and larger bubbles, but not at small bubbles. Finally, a denuded zone was identified adjacent to a > 10 nm Xe gas bubble and a GB.

36 MATERIALS SCIENCE↗

Thermomechanical Properties of Neutron Irradiated Al 3 Hf-Al Thermal Neutron Absorber Materials

A thermal neutron absorber material composed of Al 3 Hf particles in an aluminum matrix is under development for the Advanced Test Reactor. This metal matrix composite was fabricated via hot pressing of high-purity aluminum and micrometer-size Al 3 Hf powders at volume fractions of 20.0, 28.4, and 36.5%. Room temperature tensile and hardness testing of unirradiated specimens revealed a linear relationship between volume fraction and strength, while the tensile data showed a strong decrease in elongation between the 20 and 36.5% volume fraction materials. Tensile tests conducted at 200 °C on unirradiated material revealed similar trends. Evaluations were then conducted on specimens irradiated at 66 to 75 °C to four dose levels ranging from approximately 1 to 4 dpa. Tensile properties exhibited the typical increase in strength and decrease in ductility with dose that are common for metallic materials irradiated at ≤0.4T m . Hardness also increased with neutron dose. The difference in strength between the three different volume fraction materials was roughly constant as the dose increased. Nanoindentation measurements of Al 3 Hf particles in the 28.4 vol% material showed the expected trend of increased hardness with irradiation dose. Transmission electron microscopy revealed oxygen at the interface between the Al 3 Hf particles and aluminum matrix in the irradiated material. Scanning electron microscopy of the exterior surface of tensile tested specimens revealed that deformation of the material occurs via plastic deformation of the Al matrix, cracking of the Al 3 Hf particles, and to a lesser extent, tearing of the matrix away from the particles. The fracture surface of an irradiated 28.4 vol% specimen showed failure by brittle fracture in the particles and ductile tearing of the aluminum matrix with no loss of cohesion between the particles and matrix. The coefficient of thermal expansion decreased upon irradiation, with a maximum change of –6.3% for the annealed irradiated 36.5 vol% specimen.

36 MATERIALS SCIENCE↗

Microstructural Characterization of Ion Irradiated ODS MA956 Alloy

Oxide Dispersion Strengthened (ODS) alloys are considered as promising nuclear materials for the next generation advanced nuclear reactors due to their improved elevated temperature mechanical properties and radiation damage resistance. MA956 is a commercial ODS alloy with superior oxidation resistance and creep strength at elevated temperatures. The improved properties for ODS alloys can be attributed to the presence of dispersed nanosized oxide particles. These oxide particles can act as barriers to dislocation motion and provide additional sinks and sites for point defect recombination. Hence, their stability can greatly affect the properties of the irradiated ODS alloys. Besides, irradiation will induce defects into the ODS alloys, and these defects can develop further as irradiation dose increases. Furthermore, the defects propagation can significantly undermine the mechanical properties of the bulk materials, resulting in irradiation hardening and lower ductility. Therefore, it is necessary to have a good understanding of the defect’s evolution with irradiation. Hence, efforts are ongoing to understand the effect of ion irradiation on ODS MA956 with emphasis on oxide particles and evolution of defects as a function of dose (2.5, 50 and 100 dpa).

07 ISOTOPE AND RADIATION SOURCES↗

Catalyzed oxidation of IG-110 nuclear graphite by simulated fission products Ag and Pd nanoparticles

To evaluate the stability of nuclear materials in high temperature gas reactors under air ingress conditions, catalytic oxidation of IG-110 graphite by two simulated fission products, metallic Pd and Ag, was studied in oxidative atmosphere and at temperatures up to 1000°C using an integrated furnace, mass spectroscopy and infrared spectroscopy system. Transmission electron microscopy and X-ray diffraction studies show that Pd and Ag nanoparticles were successfully introduced onto powdery IG-110 graphite through an impregnation and subsequent heat-treatment process. The combined mass spectroscopy and infrared spectroscopy methods allow simultaneous analysis of two gaseous products, CO and CO 2 , and separate measurements of activation energy for their formation reactions. It was found that the introduction of Pd or Ag to IG-110 graphite substantially catalyzed the oxidation of graphite, characteristic of decreased onset temperatures for the oxidation of graphite. Moreover, the catalytic effects by Pd and Ag are considerably different based on measured concentration ratios of CO 2 to CO as a function of oxidation temperatures. Ag makes the graphite oxidation commence at approximately 400°C with CO 2 being the dominant product. In contrast, Pd significantly increases the concentration ratio of CO 2 to CO at temperatures higher than approximately 690°C, although it decreases the onset temperature for the oxidation reaction to around 525°C. To understand the catalytic difference, the mechanism of the graphite oxidation was discussed based on the changes of surface oxygen species on Ag and Pd.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Novel effects of grain size and ion implantation on grain boundary segregation in ion irradiated austenitic steel

Nuclear reactor environments are extreme in nature due to the combination of exposure to corrosive coolant, mechanical stresses, and neutron irradiation damage. This combination of environments can lead to irradiation induced/assisted precipitation, segregation, and embrittlement coupled with enhanced creep and stress corrosion cracking. While nanostructured materials are of interest in a variety of applications due to their unique properties including high mechanical strength, for nuclear applications nanostructured materials have the added benefit of irradiation resistance due to the high volume density of sinks for irradiation-induced defects. In this study, we show unique radiation-induced segregation (RIS) behavior in nanocrystalline 304 stainless steel (SS304). Typical RIS in austenitic steels includes Ni enrichment and Cr depletion within the grain boundaries. In nanostructured SS304 this RIS is reduced. Furthermore, interestingly, some grain boundaries in the nanocrystalline SS304 in this study were found to be enriched in Cr after Fe 2+ ion irradiation at 500 °C up to 50 displacements per atom (dpa). To understand this unique observation, lattice-based atomic kinetic Monte Carlo simulations were performed to investigate the effects of grain size, thermal segregation, as well as injected interstitials (introduced as Fe self-ions). The results indicate that the Cr enrichment at grain boundaries may be caused by combined effects of grain size, self-ion injection and preferential Cr diffusion via the interstitial mechanism. In conclusion, the findings also suggest a possible difference in RIS between ion and neutron irradiations.

36 MATERIALS SCIENCE↗

Catalyzed oxidation of nuclear graphite by simulated fission products Sr, Eu, and I

The influence of three fission products Sr, Eu, and I on the oxidation of IG-110 nuclear graphite was studied in the temperature range of 400 to 1000 °C. Sr and Eu were introduced as chlorides, and I was introduced as NaI. The temperature dependence of both CO 2 and CO production during the graphite oxidation measured with mass spectroscopy and infrared spectrometry shows that the introduction of these three compounds to graphite significantly decreases the onset temperature for the oxidation of graphite. Among the three compounds, NaI is the most active towards the oxidation reaction, characterized by a significant decrease of the onset temperature from approximately 650 to 400 °C before and after its introduction to graphite. Separate measurements of CO 2 and CO concentration at varying temperatures enable the calculation of the activation energy for the formation of CO 2 and CO. The activation energies for the oxidation of pure and fission product-impregnated graphite samples decrease in the following order: standard IG-110 graphite, EuCl 3 -impregnated IG-110, SrCl 2 -impregnated IG-110, and NaI-impregnated IG-110. This trend indicates that the three compounds catalyze the oxidation of graphite at temperatures relevant to the operation of high-temperature gas-cooled reactors. Furthermore, it is found that the three compounds can also affect the molar ratio of reaction products CO 2 and CO, and the rates of the graphite oxidation. At temperatures higher than about 850 °C, the impregnated samples exhibit lower CO 2 : CO ratios than the pure graphite. Different from EuCl 3 and NaI, the introduction of SrCl 2 decreases the graphite oxidation rates at temperatures higher than about 770 °C. Their catalytic mechanism can be understood based on a redox cycle of the intermediate active species, promoting the dissociation of molecular oxygen and transfer to the carbon.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Nucleation and growth of molybdenum disulfide grown by thermal atomic layer deposition on metal oxides

To enable greater control over thermal atomic layer deposition (ALD) of molybdenum disulfide (MoS 2 ), here we report studies of the reactions of molybdenum hexafluoride (MoF 6 ) and hydrogen sulfide (H 2 S) with metal oxide substrates from nucleation to few-layer films. In situ quartz crystal microbalance experiments performed at 150, 200, and 250 °C revealed temperature-dependent nucleation behavior of the MoF 6 precursor, which is attributed to variations in surface hydroxyl concentration with temperature. In situ Fourier transform infrared spectroscopy coupled with ex situ x-ray photoelectron spectroscopy (XPS) indicated the presence of molybdenum oxide and molybdenum oxyfluoride species during nucleation. Density functional theory calculations additionally support the formation of these species as well as predicted metal oxide to fluoride conversion. Residual gas analysis revealed reaction by-products, and the combined experimental and computational results provided insights into proposed nucleation surface reactions. With additional ALD cycles, Fourier transform infrared spectroscopy indicated steady film growth after ~13 cycles at 200 °C. XPS revealed that higher deposition temperatures resulted in a higher fraction of MoS 2 within the films. Deposition temperature was found to play an important role in film morphology with amorphous films obtained at 200 °C and below, while layered films with vertical platelets were observed at 250 °C. Finally, these results provide an improved understanding of MoS 2 nucleation, which can guide surface preparation for the deposition of few-layer films and advance MoS 2 toward integration into device manufacturing.

36 MATERIALS SCIENCE↗

Thermoelectric power generation in the core of a nuclear reactor

Thermoelectric energy converters offer a promising solution to generate electrical power using heat in the nuclear reactor core. Despite significant improvements in thermoelectric efficiency of nanostructured materials, the performance of these advanced materials has yet to be demonstrated in the harsh radiation environment of a reactor core. Herein, we demonstrate a thermoelectric generator (TEG) made from nanostructured bulk half-Heusler (HH) materials generating stable electrical power density > 1140 W/m 2 after 30 days in the MIT Nuclear Research Reactor under an unprecedented fast-neutron (>1 MeV) fluence of 1.5 × 10 20 n/cm 2 . Despite an initial degradation due to irradiation damage when operating under relatively low temperatures, our TEG showed a 20-fold increase in power output when operating under high temperature due to in-situ annealing and resulting thermoelectric property recovery. First-principles modeling indicates that a chemically disordered metallic phase was formed under irradiation at lower temperatures, resulting in a drastic degradation in thermoelectric properties, while at sufficiently high temperatures the system returned to the initial chemically ordered HH phase and the thermoelectric properties recovered. Transmission electron microscopy and electron diffraction demonstrated that the chemically disordered phase was formed upon ion irradiation, confirming the prediction from first-principles simulations. Furthermore, the results suggest that with proper control over the TEG operating temperatures, the nanostructured bulk TEGs could produce stable electrical power and operate indefinitely in the core of a nuclear reactor.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

In situ ion irradiation of amorphous TiO 2 nanotubes

Understanding of structural and morphological evolution in nanomaterials is critical in tailoring their functionality for applications such as energy conversion and storage. Here, we examine irradiation effects on the morphology and structure of amorphous TiO 2 nanotubes in comparison with their crystalline counterpart, anatase TiO 2 nanotubes, using high-resolution transmission electron microscopy (TEM), in situ ion irradiation TEM, and molecular dynamics (MD) simulations. Anatase TiO 2 nanotubes exhibit morphological and structural stability under irradiation due to their high concentration of grain boundaries and surfaces as defect sinks. On the other hand, amorphous TiO 2 nanotubes undergo irradiation-induced crystallization, with some tubes remaining only partially crystallized. The partially crystalline tubes bend due to internal stresses associated with densification during crystallization as suggested by MD calculations. Furthermore, these results present a novel irradiation-based pathway for potentially tuning structure and morphology of energy storage materials.

36 MATERIALS SCIENCE↗

Additive Manufacturing of Miniaturized Peak Temperature Monitors for In-Pile Applications

Passive monitoring techniques have been used for peak temperature measurements during irradiation tests by exploiting the melting point of well-characterized materials. Recent efforts to expand the capabilities of such peak temperature detection instrumentation include the development and testing of additively manufactured (AM) melt wires. In an effort to demonstrate and benchmark the performance and reliability of AM melt wires, we conducted a study to compare prototypical standard melt wires to an AM melt wire capsule, composed of printed aluminum, zinc, and tin melt wires. The lowest melting-point material used was Sn, with a melting point of approximately 230 °C, Zn melts at approximately 420 °C, and the high melting-point material was aluminum, with an approximate melting point of 660 °C. Through differential scanning calorimetry and furnace testing we show that the performance of our AM melt wire capsule was consistent with that of the standard melt-wire capsule, highlighting a path towards miniaturized peak-temperature sensors for in-pile sensor applications.

36 MATERIALS SCIENCE↗

Microstructural and chemical characterization of a purple pigment from a Faiyum mummy portrait

Results are presented from analyses that were conducted to explain the presence of chromium, detected noninvasively using energy dispersive X-ray fluorescence (XRF), in the unusually large (2-3mm diameter) rough gem-like purple pigment particles in the paint used for a Faiyum mummy portrait. An approximately 50 µm diameter particle of the chromium-containing purple pigment was extracted from the Portrait of a Bearded Man, dated to Roman Imperial Egypt in the second century, circa 170-180 CE, accession #32.6 in the Walters Art Museum collection. The particle was characterized using energy dispersive X-ray fluorescence analysis, electron microscopy, diffraction, and atom probe tomography. It is demonstrated that the purple pigment particle is a heterogeneous organic pigment, specifically, a lake pigment likely derived from either plant or insect matter, which contains minor percentages of both transition metals and alkali / alkali earth metals, with nanometer-scale crystallites of lead carbonates and sulfates. The analyses revealed for the first time the nanoscale microstructure and stratigraphy in an ancient lake pigment. Results suggest that similarities with respect to time-period and place of production may be developed among unprovenienced Faiyum mummy portraits to help localize workshops or artists, using analyses focused on lake pigments to characterize specifically metal-based mordants.

36 MATERIALS SCIENCE↗