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At least 199 records · Page 11

Thermal Conductivity Degradation in High Burnup U-Pu-Zr Fuel

Recent advancements in the characterization of irradiated U-Pu-Zr fuels have revealed complexities that challenge existing understanding of constituent redistribution. Traditionally, models have proposed three concentric regions within the fuel, each characterized by distinctive phases and porosity. However, through detailed analysis of high burnup U-Pu-Zr, we discovered the presence of four distinct constituent redistribution regions. Particularly novel is the observation of significant Pu redistribution, a previously unreported phenomenon that necessitates a reevaluation of current models. This work aims to delve deeper into these findings, seeking to correlate mesoscale measurements of thermal diffusivity and respective thermal conductivity with the phases present in each redistribution region. To achieve this objective, we employed mesoscale thermoreflectance methods using the unique, Idaho National Laboratory (INL) developed, Thermal Conductivity Microscope (TCM) at INL’s Irradiated Materials Characterization Laboratory. The TCM employs two tightly focused lasers: one for heating to generate periodic thermal waves in the substrate, and another spatially separated probe laser to detect changes in the optical reflectivity of the gold-coated substrate resulting from thermal wave diffusion. We conducted several thermal diffusivity measurements within each region of constituent redistribution of a U-19Pu-10Zr fuel pin cross section irradiated to 11 at. % burnup. The TCM measurement positions strategically aligned with transmission electron microscopy (TEM) lift-out locations previously collected from the fuel sample. Complementary microstructural analysis techniques such as optical and scanning electron microscopy (OM/SEM), electron probe microanalysis for chemical compositions, and TEM-based selective area electron diffraction (SAED) analysis for crystallographic insights into each phase were also utilized. This comprehensive approach allowed us to correlate local thermal diffusivity data with microstructural characteristics, enabling the computation of local thermal conductivity at each position. The significance of this contribution lies in its pioneering use of the TCM for ternary fuel mesoscale examination, shedding light on the previously overlooked effects of Pu redistribution on local thermal conductivity. By informing current models capturing constituent redistribution and heat transfer, our findings pave the way for more accurate predictions of metallic fuel performance. Moreover, this work sets the stage for future comparisons with similar TCM examinations on U-19Pu-10Zr fuels at ultra-low burnup, facilitating a comprehensive understanding of thermal property changes across different burnup levels. Ultimately, our study not only enriches our understanding of the thermophysical properties of individual redistribution regions within U-Pu-Zr fuel but also offers valuable insights for the design and operational parameters of proposed next-generation fast reactors.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Generalized Analysis of Dynamic Flow Fouling on Heat Transfer Surfaces

Several energy applications involve flow of untreated heat transfer fluids that contain trace amounts of mineral salts, such as calcium carbonate and calcium sulfate, which show reverse solubility with temperature. The gradual accretion of these salts onto the heat transfer surfaces causes fouling that degrades thermal performance over time. While fouling of bare surfaces has been extensively studied, fouling of nonwetting superhydrophobic or liquid-infused surfaces is less understood, especially under dynamic flow conditions. This study presents a systematic experimental analysis to elucidate dynamic flow fouling of calcium carbonate and calcium sulfate on smooth, superhydrophobic and liquid-infused surfaces in a generalized manner. Here, copper tubes with modified inner surface wettability are fabricated and subjected to forced convection at different flow rates and fouling salt concentrations. Fouling characteristics of the two salts on the different surfaces are examined through microstructural analysis, and quantified in terms of asymptotic fouling resistance that measures the total extent of fouling, and a threshold time, which correlates to the onset of significant fouling. Using Taguchi design of experiments, the study reports, for the first time, closed-form analytical relationships for the asymptotic fouling thermal resistance and threshold time on the Reynolds number, dimensionless concentration of fouling agent and dimensionless infused liquid viscosity that represents the different surface types in a unified manner. It is shown that the analytical model accurately predicts the fouling characteristics in up to about 97% of the data, based on which contour maps of optimum surface designs for minimizing fouling resistance are presented. The results provide information on designing surfaces for reduced fouling or for estimating the fouling characteristics for a given surface in applications.

36 MATERIALS SCIENCE↗

Recrystallization driven softening and heating rate dependencies of FeCrAl nuclear fuel cladding during accident transients

A refined understanding of FeCrAl cladding behavior during rapid transients is critical for its potential deployment in light-water reactors. Current assessments focus on transient burst testing metrics such as balloon geometry, burst temperature, and hoop stress, often used as proxies for simpler conventional tensile properties. However, directly correlating isothermal tensile and creep data with accident transient scenarios remains a challenge, although it is essential for high fidelity model development. Recent modeling based on tensile tests up to 800 °C, conducted with both immediate loading and a 10-minute soak, showed that immediate loading better predicts experimental burst temperatures, indicating a thermal softening effect. Building upon this observation, the current study connects transient performance, microstructural evolution, and high-temperature tensile properties by leveraging results from C26M claddings burst tests performed at heating rates of 1–50 °C/s and hoop stresses from 25 to 100 MPa. At 25 MPa, rupture temperatures varied by only 6 °C, but at 100 MPa, the difference reached 116 °C, with faster heating yielding higher burst temperatures. Microstructural analysis identified recrystallization as the primary cause of heating rate-dependent softening, eliminating prior cold-working. In-situ thermomechanical data linked ballooning onset to localized instabilities, similar to ultimate tensile strength behavior in conventional tensile tests. High heating rates correlated with immediate loading tensile data, while lower rates matched soaked data. Furthermore, by linking burst performance to microstructural evolution and tensile properties, this work provides a foundation for more accurate modeling of FeCrAl claddings and potentially other Fe-based materials under accident conditions.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Ion irradiation testing of Improved Accident Tolerant Cladding Materials

This report summarizes the results of ion irradiations conducted on two FeCrAl alloys (named as ORNL A&B) for improving the accident tolerance of LWR nuclear fuel cladding. After irradiation with 1.5 MeV protons to ~0.5 to ~1 dpa and 300°C nanoindentations were performed on the cross-sections along the ion range. An increase in hardness was observed in both alloys. Microstructural analysis shows radiation induced defects.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

Spectral analysis and temperature measurement during flash sintering under AC electric field

In-situ diffraction experiments were used to study the change in peak profiles of 8YSZ during conventional sintering and flash sintering under AC electric field. Using calibration from a conventionally heated standard, the lattice expansion of 8YSZ under flash conditions was correlated to actual specimen temperature, indicating temperature comparable to that required for conventional sintering. At higher current densities, a temperature rise greater than 2000 °C was reached, which resulted in abnormal grain growth and temperature instability. Microstructural analysis demonstrated that finer grain size can be achieved by limiting the current in order to avoid high specimen temperatures. Experiments varying the thickness of the green compact resulted in higher heat loss due to thermal conduction and corresponding reduction in final density. A replacement to the blackbody radiation model was successfully used to fit the data and explain all effects based on Joule heating as well as provide a flash sintering processing map incorporating furnace temperature, power dissipation, and sample geometry.

36 MATERIALS SCIENCE↗

Novel PBX formulations containing thermally-expandable microspheres for on-demand control of explosive behavior

In this work, we present the formulation and analysis of inert Plastic-Bonded eXplosive (PBX)-surrogates loaded with thermally expandable microspheres (TEMs). TEMs consist of a thermoplastic acrylonitrile shell (10-50 µm diameter) encapsulating an inert low boiling hydrocarbon. Upon heating, the TEMs expand as the shell softens while the hydrocarbon gasifies, increasing the internal pressure and expanding the particle by as much as 120 vol%. We hypothesize that TEM expansion within a PBX will introduce tunable changes in local density and porosity, and ultimately the shock sensitivity. This paper focuses on microstructural analysis of surrogate PBX-TEM formulations, both before and after thermally- induced TEM expansion. The formulations were analyzed by scanning electron microscopy (SEM), ultra-small angle neutron scattering (USANS), and X-ray Computed Tomography (x-ray CT) under various thermal conditions. Evidence suggests that TEM expansion within a PBX is a viable method to impart microstructural changes that are predicted to have a measurable, on-demand effect on the initiation sensitivity. Future work includes development of PBX-TEM formulations with HMX and shock initiation experiments.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Origin, parameters, and underlying deformation mechanisms of propagating deformation bands in irradiated 316L stainless steel

Lüders-type propagating deformation bands were observed in specimens of irradiated 316L stainless steel samples removed from Spallation Neutron Source target vessels after service. Mechanical testing with digital image correlation (DIC) and in-situ tensile testing with scanning electron microscopy electron backscatter diffraction showed that the observed Lüders-type behavior was not related to the known transformation-induced plasticity or twinning-induced plasticity behavior. Instead, the phenomenon occurs at small local strain values before a significant amount of martensite or deformation twins appear in the microstructure. Microstructural analysis and in-situ mechanical test results suggest Lüders-type band formation and propagation were related to the appearance and evolution of defect-free channels—analogous to slip bands. A modified Swift equation with a Ludwigson-like component was offered to rationalize the phenomenon and model the strain-softening processes at small strain values. Finally, the results indicate complex microstructural processes and deformation mechanisms were active at small strain values and underline the benefits of advanced mechanical test approaches such as DIC.

36 MATERIALS SCIENCE↗

Phase equilibria in the quasi-ternary system Ag{sub 2}Se–Ga{sub 2}Se{sub 3}–In{sub 2}Se{sub 3} and physical properties of (Ga{sub 0.6}In{sub 0.4}){sub 2}Se{sub 3}, (Ga{sub 0.594}In{sub 0.396}Er{sub 0.01}){sub 2}Se{sub 3} single crystals

The quasi-ternary system Ag{sub 2}Se–Ga{sub 2}Se{sub 3}–In{sub 2}Se{sub 3} was investigated by differential thermal, X-ray phase, X-ray structure, microstructure analysis and microhardness measurements. Five quasi-binary phase diagrams, six polythermal sections, isothermal section at 820 K and the liquidus surface projection were constructed. The character and temperature of the invariant processes were determined. The specific resistance of the single crystals (Ga{sub 0.6}In{sub 0.4}){sub 2}Se{sub 3}, (Ga{sub 0.594}In{sub 0.396}Er{sub 0.01}){sub 2}Se{sub 3} was measured, 7.5×10{sup 5} and 3.15×10{sup 5} Ω m, respectively, optical absorption spectra in the 600–1050 nm range were recorded at room temperature, and the band gap energy was estimated which is 1.95±0. 01 eV for both samples. - Graphical abstract: The article reports for the first time the investigated liquidus surface projection of the Ag{sub 2}Se–Ga{sub 2}Se{sub 3}–In{sub 2}Se{sub 3} system and isothermal section at 820 K of the system. Five phase diagrams, six polythermal sections, isothermal section at 820 K and the liquidus surface projection were built at the first time. The existence of the large region of the solid solutions based on AgIn{sub 5}Se{sub 8}, Ga{sub 2}Se{sub 3} and AgGa{sub 1−x}In{sub x}Se{sub 2} was investigated. The existence of two ternary phases was established in the Ga{sub 2}Se{sub 3}–In{sub 2}Se{sub 3} system. Two single crystals (Ga{sub 0.6}In{sub 0.4}){sub 2}Se{sub 3}, (Ga{sub 0.594}In{sub 0.396}Er{sub 0.01}){sub 2}Se{sub 3} were grown and some of optical properties of them were studied at first time. Display Omitted - Highlights: • Liquidus surface projection was built for Ag{sub 2}Se–Ga{sub 2}Se{sub 3}–In{sub 2}Se{sub 3} system. • Solid solution ranges of AgIn{sub 5}Se{sub 8}, Ga{sub 2}Se{sub 3} and AgGa{sub 1−x}In{sub x}Se{sub 2} were investigated. • Two single crystals (Ga{sub 0.6}In{sub 0.4}){sub 2}Se{sub 3}, (Ga{sub 0.594}In{sub 0.396}Er{sub 0.01}){sub 2}Se{sub 3} were grown. • Some optical properties of these single crystals were studied.

36 MATERIALS SCIENCE↗

Correlation between microstructure and temperature dependent electrical behavior of annealed Ti/Al/Ni/Au Ohmic contacts to AlGaN/GaN heterostructures

This letter reports on the temperature behavior of the structural and electrical properties of Ti/Al/Ni/Au contacts to AlGaN/GaN heterostructures. While Ohmic contacts formed at 750 °C showed a decreasing temperature behavior of the specific contact resistance ρ{sub C}, which was explained by a thermionic field emission mechanism, an increasing trend is observed in the contacts formed at 850 °C. In this case, ρ{sub C} exhibits a “metal-like” behavior, i.e., describable by a T{sup 1.8} dependence. The microstructural analysis of the interfacial region allowed to explain the results with the formation of metallic intrusions contacting directly the two dimensional electron gas.

36 MATERIALS SCIENCE↗

ZrN coating as diffusion barrier in U(Mo) dispersion fuel systems

The control of the interaction between the U(Mo) fuel phase and the Al matrix is one of the challenges of dispersion fuel plate development for research reactors. Given the specific properties of this interaction layer, larger amounts of it in the meat could lead to a reduction of the plate mechanical integrity and thermal conductivity, eventually leading to pillowing. The SELENIUM project showed that by depositing a ZrN coating on the surface of the U(Mo) fuel particles, the amount of formed U(Mo)-Al interaction layer is limited but still present. Microstructural analysis performed on the as fabricated coating and fresh fuel plates containing ZrN coated U(Mo) dispersed in an Al matrix, revealed that the coating gets damaged during plate production. The post irradiation examinations (PIE) of the ZrN coated U(Mo) fuel plates, from the SELENIUM and SEMPER FIDELIS experiments, show how the U(Mo)-Al interaction layer is formed -only at those locations where the coating is missing or damaged -and the evolution of coating microstructure during irradiation. Finally, as a remedy, to further reduce the amount of interaction layer formed, the use of an Al-Si matrix was proposed based on the higher affinity of Si for U compared to the affinity of Al for U. PIE of a fuel plate consisting of ZrN coated U(Mo) dispersed in an Al-Si matrix irradiated in the SEMPER FIDELIS experiment, clearly demonstrates the benefit of adding Si to the matrix.

36 MATERIALS SCIENCE↗

Plastic flow and microstructural instabilities during high-pressure torsion of Cu/ZnO composites

Highlights: • Hybrid bulk metal - ceramic nanoparticle material was processed by HPT. • ZnO nanoparticles exhibited significant plasticity of up to 86%. • Hydrodynamic instability determined the flow mode of ZnO particle clusters. • Microstructural stability of Cu decreased due to the co-deformation with ZnO. - Abstract: We conducted high-pressure torsion (HPT) of hybrid materials composed of two copper disks with a layer of ZnO ceramic nanoparticles sandwiched in-between. A detailed microstructural analysis of the processed samples revealed a surprisingly high level of plastic deformation introduced in individual ZnO particles, even though they possess a much high hardness than the surrounding Cu. Moreover, we demonstrated that by tailoring the initial geometry of the system (i.e. introducing holes in the cladding Cu disks), we can effectively change the flow mode of ZnO particle clusters from laminar to turbulent one and facilitate their deagglomeration process. Finally, the presence of ZnO particles decreased the microstructural stability of the Cu matrix. We discussed the obtained results in terms of hydrodynamic and microstructural instabilities during plastic deformation. This work expands our understandings of the cooperative severe plastic deformation of two dissimilar materials and sheds new light on the design of hybrid materials.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Frictional properties of Opalinus Clay: influence of humidity, normal stress and grain size on frictional stability

SUMMARY The Opalinus Clay (OPA) is a clay-rich formation considered as a potential host rock for radioactive waste repositories and as a caprock for carbon storage in Switzerland. Its very low permeability (10−19 to 10−21 m2) makes it a potential sealing horizon, however the presence of faults that may be activated during the lifetime of a repository project can compromise the long-term hydrological confinement, and lead to mechanical instability. Here, we have performed laboratory experiments to test the effect of relative humidity (RH), grain size (g.s.) and normal stress on rate-and-state frictional properties and stability of fault laboratory analogues corresponding to powders of OPA shaly facies. The sifted host rock powders at different grain size fractions (<63 μm and 63 < g.s. < 125 μm), at room (∼25 per cent) and 100 per cent humidity, were slid in double-direct shear configuration, under different normal stresses (5–70 MPa). We observe that peak friction, μpeak and steady-state friction, μss, depend on water vapour content and applied normal stress. Increasing relative humidity from ∼25 per cent RH (room humidity) to 100 per cent RH causes a decrease of frictional coefficient from 0.41 to 0.35. The analysis of velocity-steps in the light of rate-and-state friction framework shows that the stability parameter (a–b) is always positive (velocity-strengthening), and it increases with increasing sliding velocity and humidity. The dependence of (a–b) on slip rate is lost as normal stress increases, for each humidity condition. By monitoring the variations of the layer thickness during the velocity steps, we observe that dilation (Δh) is directly proportional to the sliding velocity, decreases with normal stress and is unaffected by humidity. Microstructural analysis shows that most of the deformation is accommodated within B-shear zones, and the increase of normal stress (σn) promotes the transition from strain localization and grain size reduction to distributed deformation on a well-developed phyllosilicate network. These results suggest that: (1) the progressive loss of velocity dependence of frictional stability parameter (a–b) at σn > 35 MPa is dictated by a transition from localized to distributed deformation and (2) water vapour content does not affect the deformation mechanisms and dilation, whereas it decreases steady-state friction (μss), and enhances fault stability.

58 GEOSCIENCES↗

Effect of formation temperature on properties of graphite/stannum composite for bipolar plate

Bipolar plates are key components in Proton Exchange Membrane (PEM) fuel cells. They carry current away from the cell and withstand the clamping force of the stack assembly. Therefore, PEM fuel cell bipolar plates must have high electrical conductivity and adequate mechanical strength, in addition to being light weight and low cost in terms of both applicable materials and production methods. In this research, the raw materials used to fabricate the high performance bipolar plate are Graphite (Gr), Stannum (Sn) and Polypropylene (PP). All materials used was in powder form and Gr and Sn act as fillers and the PP acts as binder. The ratio of fillers (Gr/Sn) and binder (PP) was fixed at 80:20. For the multi-conductive filler, small amount of Sn, which is 10 up to 20wt% (from the total weight of fillers 80%) have been added into Gr/Sn/PP composite. The fillers were mixed by using the ball mill machine. The second stage of mixing process between the mixer of fillers and binder is also carried out by using ball mill machine before the compaction process by the hot press machine. The effect of formation temperatures (160°C-170°C) on the properties of Gr/Sn/PP composite had been studied in detail, especially the electrical conductivity, bulk density, hardness and microstructure analysis of Gr/Sn/PP composite. The result shows that there are significant improvement in the electrical conductivity and bulk density, which are exceeding the US-DoE target with the maximum value of 265.35 S/cm and 1.682g/cm{sup 3} respectively.

36 MATERIALS SCIENCE↗

Tensile Behavior of Inconel X750 Sheets: Effect of Heat Treatment

X-750 is a nickel-chromium based super alloy of usefulness in a wide variety of applications. Its excellent relaxation resistance is useful for high-temperature springs and bolts; it is utilized in gas turbines, rocket engines, nuclear reactors, pressure vessels, tooling, and aircraft structures. Its performance is similar to that of Inconel alloy 600 but it is made precipitation-hardenable by additions of aluminum and titanium. It has good resistance to corrosion and oxidation along with high tensile and creep-rupture properties at temperatures up to 700 deg. C. In this study, the tensile flow behavior of the alloy was studied by performing uniaxial tensile tests under a range of temperatures and at different strain rates. To assess the microstructure-mechanical property relationships in the alloy, microstructure analysis (through the use of electron microscopy and XRD analysis) was utilized post-experiment. This paper will however focus on reporting the tensile properties and temperature and strain rate effects on the as-received alloy vs. the heat-treated alloy. (authors)

36 MATERIALS SCIENCE↗

A Novel Duplex Treatment of C20 Steel Combining Low-Pressure Carburizing and Laser Quenching

This research paper focuses on a novel duplex treatment combining low-pressure carburizing and laser quenching to reach high surface hardness and hardening depth, improving wear resistance and mechanical properties. Results of microstructural analysis, micro- and nanohardness, wear and x-ray diffraction tests, carried out on laser-treated, carburized and duplex-treated C20 low-alloy steel, demonstrate that the novel duplex treatment developed greatly enhances wear resistance of the material.

36 MATERIALS SCIENCE↗