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At least 1,261 records · Page 70

Insights into elevated temperature tensile deformation mechanisms and kink banding in additively manufactured tungsten

Additive manufacturing (AM) potentially enables fabrication and repair of plasma facing components (PFCs) of tungsten. However, deformation mechanisms in AM-fabricated tungsten under service-relevant thermomechanical conditions remain unknown majorly due to challenges in achieving crack-free W. This study reveals the deformation mechanisms operative under tension at 800 °C and 1200 °C in the electron beam melting powder bed fusion (EBM-PBF) fabricated W. Textured columnar grains with mixed <001 >/<111 >|| build-direction were observed. Strong anisotropy in tensile properties persisted across test temperatures, and all specimens exhibited extensive deformation-induced banding phenomena. Grain boundary character analysis of the deformed specimens indicated that these deformation bands were kink bands with tilt grain boundaries prominently present at the band-matrix interface. Interestingly, the material within the kink bands rotated toward higher resolved shear stress, providing insights into the origins of kink band formation in body-centered cubic refractory metals. Intragranular misorientation axis analysis revealed that plasticity was dominated by {110} <111 > slip at 800 °C, whereas additional (213)[11⁢̄1] and (112)[11⁢̄1] slip systems activated at 1200 °C. A dense low-angle boundary networks observed near fractured surface indicated the onset of dynamic recrystallization. Results reveal plasticity governing mechanisms in AM-fabricated W under power plant-relevant conditions, and provide insights into kink band attributes in refractory metals.

Mayes, Riley [ORNL] (ORCID:000900089307010X)↗

Methane foam performance evaluation in water-wet unconsolidated porous media: A systematic experimental investigation at elevated pressure and temperature conditions

In the petroleum industry, enhanced oil recovery (EOR) techniques employ foam extensively to establish conformance control in heterogeneous and fractured reservoirs in order to increase the sweep efficiency. In such applications, foam performance evaluation under complex subsurface conditions is pivotal for the effective and optimized deployment of foam treatment. However, there is a scarcity of hydrocarbon gas foam generation and evaluation studies that examine the relationships between foam performance and the critical foam parameters at high-pressure and high-temperature conditions. Here, this study aims at methodically investigating the effects of several foam parameters on methane foam performance in water-wet proppant packs under harsh operating conditions. This is in relation to the technical needs of hydrocarbon foam injection into hydraulically-induced, propped fractures in unconventional oil reservoirs. To this end, a state-of-the-art experimental foam generation apparatus was designed, fabricated, and commissioned. We performed a large number of foam flow experiments on proppant packs using methane gas and different foaming agents at 3500 psi and 115°C. Anionic and amphoteric surfactants were employed to probe the effect of their ionic nature on foam performance. Foam performance sensitivities to various foam generation parameters and operating conditions, such as surfactant concentration, gas fraction, total injection rate, operating pressure, salinity, and proppant pack length were investigated. To this end, steady-state pressure drops across the proppant packs during foam generation and foam's apparent viscosity were measured to quantify the foam performance of surfactants. The results were then analyzed to determine optimum values of the foam parameters and the interplay between these parameters are discussed here. The systematic results achieved from this work are in agreement with the trends available in the literature and provide new insights into complexities of in situ foam generation in water-wet, unconsolidated porous media at extreme reservoir conditions.

03 NATURAL GAS↗

Elevated temperature tensile tests on DU–10Mo rolled foils

We report that studies were completed to obtain tensile mechanical properties for uranium-10wt.% molybdenum (U-10Mo) foils which were subjected to four different thermomechanical processing conditions. U-Mo alloy foils are being investigated to support fuel conversion of high power research reactors from their current high enriched fuel form to a low enriched fuel form. Mechanical properties of the fuel foil have an effect on irradiation performance and fuel fabrication and therefore are required to support modeling and qualification of new low-enriched uranium monolithic fuel plate designs. The data contained in this document contributes to fuel qualification by fulfilling the requirement that physical properties related to fuel meat be established. It is expected that depleted uranium-10wt% Mo (DU–10Mo) mechanical behavior is representative of the low-enriched U10-Mo to be used in actual fuel plates; therefore DU–10Mo was studied to simplify material processing, handling, and testing requirements. In this report, the different thermomechanical treatments included variations of wrought hot and cold rolling reduction and post rolling annealing. Each of the four foils was hot rolled. After hot rolling reduction, three of the four foils were further reduced by cold rolling. One of the three was reduced a further 20% by cold rolling, and the remaining two were reduced 50% by cold rolling. Following cold rolling reduction, one of the two foils which had been reduced 50% by cold rolling was annealed at 650?°C. Performing this analysis allows assessment of the impact of foil fabrication history on the resultant tensile properties DU–10Mo fuel foils. Tensile properties of DU–10Mo at room temperature through approximately 400 °C determined from the tests conducted herein suggest the material is stronger and has lower ductility than what has been reported previously in the literature. The explanation for these differences has yet to be determined, but is likely related to differences in grain size and/or impurity content, and variation in fabrication history. At the highest temperatures tested (550 °C) better agreement between the values reported here and available literature was found. As expected, yield and ultimate tensile strength decreased with increasing test temperature. Generally, the yield stress for all foil processing conditions was found to be in the range of 1100 MPa for room temperature tests, and in the range of 200 MPa for tests conducted at 550 °C. Ultimate tensile stress was in the range of 1175 MPa at room temperature, decreasing to approximately 225 MPa at 550 °C. Lastly, elongation increased significantly, from 0 to 2% at room temperature to 50% or more for the tests at 550 °C.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Elevated temperature microcantilever testing of fresh U-10Mo fuel

Proliferation concerns are the driving force to reduce the enrichment of research reactor fuel from highly enriched fuel to lower levels of enriched fuel. One promising fuel alloy that would enable a reduction in enrichment without greatly diminishing fuel performance is Uranium with 10 wt. % Molybdenum (U-10 wt-% Mo). While there is a large amount of data available on the microstructure and thermal properties of this new fuel type currently there is insufficient data available on the mechanical properties. Small scale mechanical testing techniques can be used to evaluate the mechanical properties of the as-fabricated U-10 wt% Mo components at their intended operating temperature which should improve the accuracy of the input parameters employed by modelers. In this study the mechanical properties of a U-10 wt% Mo fuel meat sample taken from an as-fabricated fuel plate for a new fuel design were evaluated using in-situ scanning electron microscopy microcantilever testing under varying temperatures between room temperature and 200 °C.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Tensile behavior and microstructural evolution of a Fe-25Ni-20Cr austenitic stainless steel (alloy 709) from room to elevated temperatures through in-situ synchrotron X-ray diffraction characterization and transmission electron microscopy

Uniaxial tensile tests were done on Fe-25Ni-20Cr Austenitic Stainless Steel (Alloy 709) along with in-situ synchrotron measurement at different temperatures (25 degrees C, 500 degrees C, 700 degrees C and 900 degrees C). The X-Ray diffraction data was collected in-situ in order to follow the phases present as well as to derive the dislocation density as a function of strain through peak broadening analysis based on the modified Williamson-Hall method and see how trends are affected as a function of temperature. The XRD data were complemented by TEM and STEM-EDX characterization done on the post-experiment samples to observe the deformed microstructures. Finally, the paper presents a depiction of the tensile behavior of this advanced steel by interpreting the stress-strain curves and the effect of temperature through the information gained by in-situ XRD and TEM observations as well as fractography done ex-situ on the samples tested to rupture.

36 MATERIALS SCIENCE↗

Microstructural and compositional evolutions in $γ$-LiAlO 2 pellets during ion irradiation at an elevated temperature

This study reports on the microstructural, phasic and compositional evolutions of γ-LiAlO 2 during ion irradiation. Polycrystalline γ-LiAlO 2 pellets were irradiated sequentially with He + and D 2 + ions to the same combined fluences of up to 3 × 10 17 (He + +D + )/cm 2 at 773 K. The irradiated pellets were characterized using scanning transmission electron microscopy and atom probe tomography. Surface amorphization likely due to radiolysis and planar defects as a possible precursor for formation of precipitates are created at 5 × 10 16 (He + +D + )/cm 2 , followed by the formation of nano-sized precipitates and fractures at higher doses. Spinel-like precipitates of non-stoichiometric LiAl 5 O 8 and gas-filled cavities are observed to grow with increasing dose. Faceted precipitates and rounded cavities appear at 2 × 10 17 (He + +D + )/cm 2 . With further increasing ion fluence to 3 × 10 17 (He + +D + )/cm 2 , amorphization of the precipitates takes place and micron-sized fractures appear. Surface exfoliation could occur at an extremely high ion fluence. There are compositional changes in the γ-LiAlO 2 pellets during the microstructural evolution. In the precipitate and amorphized regions, Li concentrations decrease to ~7 and 3.7 at.% from 25 at.% in γ-LiAlO 2 , respectively. This study reveals a full-cycle microstructural evolution with corresponding compositional changes in γ-LiAlO 2 pellets during ion irradiation at 773 K. In conclusion, the data could help model, assess, and predict the material performance during neutron irradiation in reactors.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

Hydrogen motion in near stoichiometric yttrium dihydride at elevated temperatures

The high-temperature motion of hydrogen in near stoichiometric yttrium dihydride (YH x , x = 1.62 and 1.87 at.%) was investigated using incoherent quasi-elastic neutron scattering and Density Functional Theory (DFT) calculations as a function of hydrogen stoichiometry. Translational motion (diffusivity) of hydrogen in yttrium dihydride was only observed in a temperature range of 1073–1173 K under vacuum environment. Here, the hydrogen motion was found to be limited to the tetrahedral sublattice, and diffusivity of hydrogen was observed to increase with decreasing hydrogen stoichiometry. The same behavior was also supported with DFT calculations. The DFT results also indicated that certain migration paths with smaller energy barriers favored H jump resulting in higher diffusivities.

08 HYDROGEN↗

Origins of radiation-induced optical attenuation in neutron-irradiated single-crystal sapphire at elevated temperatures

Sapphire (α-Al 2 O 3 ) is a candidate fiber-optic sensor material for extreme temperature environments, potentially including those of nuclear reactors. However, its optical transmission under high-dose neutron irradiation is not well understood compared with that of conventional fused silica. This study examined dimensional changes, optical transmission, and irradiation-induced defects in neutron-irradiated α-Al 2 O 3 at temperatures of 298 °C to 688 °C and doses of 3.2 to 12 dpa. Although previous studies attributed radiation-induced attenuation (RIA) at the highest irradiation temperatures to increased optical scattering from radiation-induced voids, our findings indicate that scattering from neither voids nor dislocation loops can explain the measured attenuation. Instead, absorption due to aluminum vacancy centers appears more likely based on a comparison of the spectral features of the measured optical attenuation with previous literature. Significant c-axis swelling (5.51 % ± 0.83 %) was observed in the 12 dpa, 592 °C irradiated sample, much higher than earlier measurements, suggesting temperature sensor drift of 543 °C to 1,140 °C. Void patterning was predominantly observed along the a-axis, differing from previous studies on polycrystalline samples, which showed c-axis patterning. Dislocation loops evolved into network dislocations with increasing temperature and dose; voids formed within these structures, showing no size or density changes, indicating an atypical growth mechanism.

Neutron irradiation↗

Tensile properties of co-rolled Zr/U-10Mo fuel at ambient and elevated temperatures

The United States High Performance Research Reactor (USHPRR) initiative is currently interested in replacing high-enriched uranium fuel in research reactors with high-assay low-enriched uranium fuel. Here, this work aimed to assist in that mission by providing tensile and bend test data on bare U-Mo and tensile test data on co-rolled Zr/U-10Mo plates at differing thicknesses (0.285 mm, 0.300 mm, and 0.465 mm) and temperatures (293 K, 473 K, and 623 K). Yield strength and ultimate tensile strength values are reported along with an in-depth comparison of how temperature, rolling direction, thickness, and the presence of the Zr-interlayer affect mechanical properties. Results showed that yield strength and ultimate tensile strength in Zr/U-10Mo foils lower as temperature increases by approximately 300 MPa from 293 to 473 K, and another 100 MPa from 473 to 623 K. Additionally it was found that with increased temperature, there is less differentiation in fuel necking and delamination behavior, as well as a greater perceived elongation to fracture. The elastic modulus of co-rolled mini-plates does not follow the volumetric rule of mixtures in terms of averaged strength and is actually lower than the reported moduli of both Zr and U-10Mo.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Characterization of carrier states in CuWO₄ thin-films at elevated temperatures using conductometric analysis

CuWO₄ thin-films were deposited by pulsed laser deposition onto an insulating substrate. The temperature dependence of the electronic conductivity of CuWO₄ thin-films was determined over 100–500 °C temperature range in a synthetic air atmosphere. Additionally, variations of conductivity at 300 °C and 500 °C have been measured for oxygen partial pressures (0.1 atm<p(O₂)<0.9 atm) in nitrogen. The apparent activation energy ΔE{sub a} for the electrical conduction has been estimated. The study of the temperature effect on the electron transport properties of CuWO₄ thin-films reveals the operation of two temperature-dependent oxygen states. The effect of varying oxygen concentration on the electronic properties is discussed in detail. The electrochemical nature of the operating oxygen states for 100–500 °C temperature range is deduced using a physicochemical model that relates electronic conductivity with oxygen partial pressure and temperature. - Graphical abstract: Formation of oxygen states in n-type semiconducting metal-oxides and its effect on the surface electrochemical potential and electron transport. Highlights: • The study of surface species in CuWO₄ thin-films was carried using conductometry. • The determination of the apparent activation energy of conduction with temperature is outlined. • Temperature and O₂ concentration effects on the oxygen states was established. • For the ranges of temperature studied, the identified operating oxygen states were O₂⁻ and O⁻.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Defect equilibrium in PrBaCo{sub 2}O{sub 5+δ} at elevated temperatures

A defect equilibrium model for PrBaCo{sub 2}O{sub 5+δ} is suggested based on oxygen non-stoichiometry data. The model includes reactions of oxygen exchange and charge disproportionation of Co{sup 3+} cations. The respective equilibrium constants, enthalpies and entropies for the reactions entering the model are obtained from the fitting of the experimental data for oxygen non-stoichiometry. The enthalpies of oxidation Co{sup 2+}→Co{sup 3+} and Co{sup 3+}→Co{sup 4+} are found to be equal to 115±9 kJ mol{sup –1} and 45±4 kJ mol{sup –1}, respectively. The obtained equilibrium constants were used in order to calculate variations in concentration of cobalt species with non-stoichiometry, temperature and oxygen pressure. - Graphical abstract: Variations in concentration of cobalt species with oxygen content in PrBaCo{sub n}{sup 2+}Co{sub z}{sup 3+}Co{sub p}{sup 4+}O{sub 5+δ} at 650 °S. Display Omitted - Highlights: • The defect equilibrium model based on oxygen non-stoichiometry data is suggested. • Disproportionation of Co{sup 3+} cations gives significant contribution to defect equilibrium. • The hole concentration obtained from the model is in accord with electrical properties.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Diffusion behavior of copper atoms under Cu(II) reduction in Cucurbit[8]uril cavity at elevated temperatures

In this paper we describe copper clusters and nanoparticles formation by the reduction of copper (II) ions inside cavities of macrocycle molecules using supramolecular compound [Cu(Cyclen)(H{sub 2}O)@CB[8]](NO{sub 3}){sub 2}·12H{sub 2}O followed by Cu atoms diffusion between macrocycle CB[8] molecules. To understand the copper cluster genesis and nanoparticles formation x-ray powder diffraction (XRD), electron paramagnetic resonance (EPR), FTIR-spectroscopies, HRTEM and thermal analysis were used. It was found that atomic Cu(0) was not fixed in the cavity under heating, and Cu clusters and nanoparticles were formed by heating of supramolecular compound powder at 200–340 °C in He, but more preferably in H{sub 2}. The process was partially reversible after heating the powder up to 300 °C for 15 min and air exposure for a few months. The process was irreversible after heating of the sample at temperatures higher than 340 °C due to CB[8] cavitand decomposition. In general, exposure of the samples to air leads to oxidation and hydration clusters of Cu. Nanoparticles up to 600 nm in size formed on the surface of agglomerated polycrystalline powder at temperatures lower than 200 °C. The clusters less than 7 nm and 40 nm in size were formed at 300 °C inside and outside agglomerating polycrystalline powder, respectively. The diffusion coefficient of copper atoms inside polycrystalline CB[8] agglomerates equal to 10{sup −10} cm{sup 2}/s by heating the samples at 300 °C was found. - Graphical abstract: Copper nanoparticles and clusters are formed by the reduction of copper (II) ions inside cavities of macrocycle molecules at 200–340 °C in He, but more preferably in H{sub 2} using supramolecular compound [Cu(Cyclen)(H{sub 2}O)@CB[8]](NO{sub 3}){sub 2}·12H{sub 2}O followed by Cu atoms diffusion between macrocycle CB[8] molecules. Nanoparticles up to 600 nm in size formed on the surface of agglomerated polycrystalline powder at temperatures lower than 200 °C. The clusters less than 7 nm and 40 nm in size were formed at 300 °C inside and outside agglomerating polycrystalline powder, respectively. - Highlights: • We considered Cu NP's formation at CuCyclen thermolysis in H{sub 2} and He. • Initial complex CuCyclen was located inside cavitand CB[8]. • Cu(0) reduced in cavities diffuse between CB[8] molecules and Cu nuclei appear. • NPs less than 7 and 50 nm were formed inside and outside the CB[8] powder. • Coefficient of Cu(O) diffusion is 10{sup −10} cm{sup 2}/s for temperature at 300 °C.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Microstructural evolution in nickel alloy C-276 after Ar-ion irradiation at elevated temperature

In present work, the irradiation damage in nickel-base alloy C-276 irradiated with Ar-ions was studied. Specimens of C-276 alloy were subjected to an irradiation of Ar-ions (with 120 keV) to dose levels of 6 and 10 dpa at 300 and 550 Degree-Sign C, respectively. The size distributions and densities of dislocation loops caused by irradiation were investigated with transmission electron microscopy. Irradiation hardening due to the formation of the loops was calculated using the dispersed barrier-hardening model, showing that irradiation hardening was greatest at 300 Degree-Sign C/6 dpa. The microstructure evolution induced by Ar-ion irradiation (0-10 dpa) in nickel-base alloy C-276 has been studied using a multi-scale modeling code Radieff constructed based on rate theory, and the size of dislocation loops simulated by Radieff was in good agreement with the experiment. - Highlights: Black-Right-Pointing-Pointer High density of dislocation loops appeared after Ar ions irradiation. Black-Right-Pointing-Pointer Irradiation hardening due to the formation of loops was calculated by the DBH model. Black-Right-Pointing-Pointer Size of loops simulated by Radieff was in good agreement with the experiment.

36 MATERIALS SCIENCE↗

Microstructure evolution and mechanical performance of nickel based superalloy C1023 at elevated temperatures

Highlights: • Growth and strengthening mechanisms of carbide in superalloy C1023 were investigated. • Carbide dendrite primary arm grows selectively based on the vertex of blocky carbonitride. • Monolayer or multilayer carbide dendrite arm has certain crystal relationship with γ′ and γ. • Plastic deformation of γ hinders interior crack propagating from MC to matrix at 650 °C. • Oxidation of GBs significantly weakens the tensile strength of the superalloy at 850 °C. - Abstract: Microstructure evolution of polycrystalline nickel based superalloy C1023 casting was investigated by comparing as cast superalloy and heat treated superalloy in the paper. Influences of strengtheners and carbides on the tensile behaviors of heat treated superalloy at different temperatures (20 °C, 650 °C, and 850 °C) were studied. Resulting data from deep corrosion suggested that growth mode of scripted carbide included nucleation on the vertex of blocky carbonitride, expansion of dendrite arm in C-rich area, and enlargement of dendrite cap. Decomposition of MC carbide generated numerous octahedral M{sub 23}C{sub 6} carbide as well as nanoscale Cr-Mo-rich nuclei. Diffusion of Mo from γ to precipitates such as γ', MC, and M{sub 23}C{sub 6}, occurred during the heat treatment while irregular γ' (4 nm–500 nm) transformed into cuboidal particles. At 650 °C, no significant deterioration of tensile strength was found while plastic deformation ability of γ base was improved. Oxidation of grain boundaries (GBs) dominated the crack behavior of the superalloy at 850 °C.

77 NANOSCIENCE AND NANOTECHNOLOGY↗