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At least 1,045 records · Page 58

Dynamic recrystallization kinetics and microstructure evolution of an AZ91D magnesium alloy during hot compression

Highlights: • DRX kinetic model is developed for the aged AZ91D magnesium alloy. • The DRX behavior in different strained regions was investigated. • Four morphologies of the second phase were proposed during the hot compression tests. • The nucleation mechanisms of the DRX grains were clarified. - Abstract: The flow behavior of as-cast AZ91D magnesium alloy was evaluated by isothermal compression tests within the temperatures of 220 °C, 260 °C, 300 °C, 340 °C, and 380 °C, and the strain rates of 0.001, 0.01, 0.1, 1 and 10s{sup −1}. Based on the stress-strain curve and hyperbolic sine function, the thermal activation energy and the strain rate sensitivity of the material were determined to be 142.2726 kJ·mol{sup −1} and 0.142, respectively. The S type evolution of the dynamic recrystallization with the increasing strain that dynamic recrystallization (DRX) model obtained from stress and strain data. There was a good consistency between the proposed DRX kinetics model and microstructure observation results. Combining isothermal compression specimens with finite element and scanning electron microscopy (SEM) analysis indicated that the sample can be divided into rarely recrystallized region, partially recrystallized region and completely recrystallized region, which falls within the dense deformation zone, free deformation zone and severe deformation zone, respectively. The different forms of the β-Mg{sub 17}Al{sub 12} phase induced by compression tests were confirmed by SEM. Nucleation mechanisms of the DRX were discussed with reference to the transmission electron microscope (TEM) analysis results.

36 MATERIALS SCIENCE↗

Halo-independent analysis of direct dark matter detection through electron scattering

Sub-GeV mass dark matter particles whose collisions with nuclei would not deposit sufficient energy to be detected, could instead be revealed through their interaction with electrons. Analyses of data from direct detection experiments usually require assuming a local dark matter halo velocity distribution. In the halo-independent analysis method, properties of this distribution are instead inferred from direct dark matter detection data, which allows then to compare different data without making any assumption on the uncertain local dark halo characteristics. Furthermore, this method has so far been developed for and applied to dark matter scattering off nuclei. Here we demonstrate how this analysis can be applied to scattering off electrons.

79 ASTRONOMY AND ASTROPHYSICS↗

Simulation study of the effects of near- and far-field heating during focused ultrasound uterine fibroid ablation using an electronically focused phased array: A theoretical analysis of patient safety

Purpose: Assess the feasibility of using large-aperture, flat ultrasonic transducer arrays with 6500 small elements operating at 500 kHz without the use of any mechanical components for the thermal coagulation of uterine fibroids. This study examines the benefits and detriments of using a frequency that is significantly lower than that used in clinical systems (1–1.5 MHz). Methods: Ultrasound simulations were performed using the anatomies of five fibroid patients derived from 3D MRI. Using electronic steering solely, the ultrasound focus from a flat, 6500-element phased array was translated around the volume of the fibroids in various patterns to assess the feasibility of completing full treatments from fixed physical locations. Successive temperature maps were generated by numerically solving the bioheat equation. Using a thermal dose model, the bioeffects of these simulations were quantified and analyzed. Results: The simulations indicate that such an array could be used to perform fibroid treatments to 18 EM{sub 43} at an average rate of 90 ± 20 cm{sup 3}/h without physically moving the transducer array. On average, the maximum near-field thermal dose for each patient was below 4 EM{sub 43}. Fibroid tissue could be treated as close as 40 mm to the spine without reaching temperatures expected to cause pain or damage. Conclusions: Fibroids were successfully targeted and treated from a single transducer position to acceptable extents and without causing damage in the near- or far-field. Compared to clinical systems, treatment rates were good. The proposed treatment paradigm is a promising alternative to existing systems and warrants further investigation.

60 APPLIED LIFE SCIENCES↗

Drift and ion acoustic wave driven vortices with superthermal electrons

Linear and nonlinear analysis of coupled drift and acoustic mode is presented in an inhomogeneous electron-ion plasma with {kappa}-distributed electrons. A linear dispersion relation is found which shows that the phase speed of both the drift wave and the ion acoustic wave decreases in the presence of superthermal electrons. Several limiting cases are also discussed. In the nonlinear regime, stationary solutions in the form of dipolar and monopolar vortices are obtained. It is shown that the condition for the boundedness of the solution implies that the speed of drift wave driven vortices reduces with increase in superthermality effect. Ignoring density inhomogeniety, it is investigated that the lower and upper limits on the speed of the ion acoustic driven vortices spread with the inclusion of high energy electrons. The importance of results with reference to space plasmas is also pointed out.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

The use of electrical impedance spectroscopy for monitoring the hydration products of Portland cement mortars with high percentage of pozzolans

In this paper, mortars and pastes containing large replacement of pozzolan were studied by mechanical strength, thermogravimetric analysis (TGA), scanning electronic microscopy (SEM), mercury intrusion porosimetry (MIP) and electrical impedance spectroscopy (EIS). The effect of metakaolin (35%) and fly ash (60%) was evaluated and compared with an inert mineral addition (andalusite). The portlandite content was measured, finding that the pozzolanic reaction produced cementing systems with all portlandite fixed. The EIS measurements were analyzed by the equivalent electrical circuit (EEC) method. An EEC with three branches in parallel was applied. The dc resistance was related to the degree of hydration and allowed us to characterize plain and blended mortars. A constant phase element (CPE) quantified the electrical properties of the hydration products located in the solid–solution interface and was useful to distinguish the role of inert and pozzolanic admixtures present in the cement matrix.

36 MATERIALS SCIENCE↗

The role of alumina on performance of alkali-activated slag paste exposed to 50 °C

The strength and microstructural evolution of two alkali-activated slags, with distinct alumina content, exposed to 50 °C have been investigated. These two slags are ground-granulated blast furnace slag (containing 13% (wt.) alumina) and phosphorous slag (containing 3% (wt.) alumina). They were hydrated in the presence of a combination of sodium hydroxide and sodium silicate solution at different ratios. The microstructure of the resultant slag pastes was assessed by X-ray diffraction, differential thermogravimetric analysis, and scanning electron microscopy. The results obtained from these techniques reveal the presence of hexagonal hydrates: CAH{sub 10} and C{sub 4}AH{sub 13} in all alkali-activated ground-granulated blast-furnace slag pastes (AAGBS). These hydrates are not observed in pastes formed by alkali-activated ground phosphorous slag (AAGPS). Upon exposure to 50 °C, the aforementioned hydration products of AAGBS pastes convert to C{sub 3}AH{sub 6}, leading to a rapid deterioration in the strength of the paste. In contrast, no strength loss was detected in AAGPS pastes following exposure to 50 °C. -- Highlights: •Strength of alkali-activated slag (AAS) pastes after exposure to 50 °C is studied. •AAS pastes with high alumina content lose strength after the exposure. •C{sub 4}AH{sub 13} and CAH{sub 10} form in these AAS pastes. •Conversion of these calcium alumina hydrates is associated with the strength loss. •AAS pastes with low alumina content maintain its strength after the exposure.

36 MATERIALS SCIENCE↗

Changes in microstructure characteristics of cement paste on carbonation

This study investigates the influence of carbonation on the microstructure of cement paste cast with Ordinary Portland Cement (OPC), fly ash based Portland Pozzolana Cement (PPC) and Limestone Calcined Clay Cement (LC{sup 3}) using X-ray diffraction (XRD), thermal analysis (TGA), scanning electron microscope (SEM) and mercury intrusion porosimeter (MIP). A comparison is made between samples exposed to 3% carbon dioxide concentration and those exposed to natural CO{sub 2} concentrations. It is observed that the products formed on carbonation are similar in both the exposure conditions. Distinct rims corresponding to decalcified C-S-H are observed around clinker grains in the carbonated samples. Coarsening of pore structure is observed on carbonation in all the cements and an increase in the total porosity is observed in blended cements. Thermodynamic modeling indicates irrespective of the type of cement the total solid volume is reduced on complete carbonation. The volume change occurring on carbonation obtained from experimental results and thermodynamic modeling are compared.

36 MATERIALS SCIENCE↗

Optimizing dicyandiamide pretreatment conditions for enhanced structure and electronic properties of polymeric graphitic carbon nitride

Graphitic carbon nitride, a polymeric semiconductor, possesses a distinctive electronic band structure and exceptional chemical stability, making it a highly promising material for various catalytic applications such as electrocatalysis, photocatalysis, and photo-electrocatalysis. However, its practical applications remain limited due to its low active site density and poor electrical conductivity. In this study, to overcome such limitations, we have conducted a thorough investigation to explore the impact of dicyandiamide (DCDA) precursor pretreatment prior to thermal polymerization to graphitic carbon nitride. The DCDA precursor was subjected to various pretreatment methods including grinding using mortar and pestle, recrystallization through stirring or probe sonication after dissolving in deionized water, and freeze drying, prior to thermal polymerization at 550 °C for 2 hours. The structural and morphological properties of the catalysts prepared were compared and characterized by X-ray diffraction (XRD), attenuated total reflectance–Fourier transform infrared (ATR-IR) spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS) analysis while the electronic band gap properties were determined based on density functional theory (DFT) calculations for a set of crystalline systems having C/N ratios similar to those identified experimentally. In comparison to direct thermal polymerization, pretreated samples rendered the same product yield, diverse morphologies with flat or wrinkle structures, and reduced electrochemical resistance, making them suitable for use in various catalytic processes.

36 MATERIALS SCIENCE↗

Electrochemical cofactor recycling of bacterial microcompartments

Bacterial microcompartments (BMCs) are prokaryotic organelles that consist of a protein shell which sequesters metabolic reactions in its interior. While most of the substrates and products are relatively small and can permeate the shell, many of the encapsulated enzymes require cofactors that must be regenerated inside. We have analyzed the occurrence of an enzyme previously assigned as a cobalamin (vitamin B 12 ) reductase and, curiously, found it in many unrelated BMC types that do not employ B 12 cofactors. We propose Nicotinamide adenine dinucleotide (NAD+) regeneration as the function of this enzyme and name it Metabolosome Nicotinamide Adenine Dinucleotide Hydrogen (NADH) dehydrogenase (MNdh). Its partner shell protein BMC-T SE (tandem domain BMC shell protein of the single layer type for electron transfer) assists in passing the generated electrons to the outside. We support this hypothesis with bioinformatic analysis, functional assays, Electron Paramagnetic Resonance spectroscopy, protein voltammetry, and structural modeling verified with X-ray footprinting. This finding represents a paradigm for the BMC field, identifying a new, widely occurring route for cofactor recycling and a new function for the shell as separating redox environments.

bacterial microcompartment↗

Physicochemical Properties and Structure of the Bone Matrix in Simulated Tuberculous Osteitis

The physicochemical properties and structure of the bone matrix are studied in a case of simulated tuberculous osteitis without treatment and after a full course of specific antibacterial therapy. Using X-ray diffraction, infrared spectroscopy, thermal analysis, and scanning electron microscopy, we revealed that tuberculous osteitis causes fine disintegration of the bone matrix due to an increase in nonstoichiometric hydroxyapatite, formation of amorphous calcium phosphates, and a decrease of the organic phase, which is accompanied by embrittlement of the bone matrix. Excessive growth of carbonate-hydroxyapatite crystals of a mixed AB substitution type leads to excessive osteogenesis, accompanied by the uncontrolled growth of bone trabeculae. The presence of “liming” regions in the crystal lattice of hydroxyapatite increases the “binding” properties of the bone matrix in which mycobacteria are immobilized and removed in the composition of detritus.

60 APPLIED LIFE SCIENCES↗

Imaging and Analysis of Insoluble Electrorefiner Material

Throughout pyroprocessing efforts at the Hot Fuel Examination Facility (HFEF), insoluble material has accumulated in the Electrorefiner (ER) vessel. The objective of this effort was to analyze the accumulated material to determine its origin. Material was removed from the ER salt bath and distilled to remove excess salt prior to performing analysis. Three samples were sent for chemical and isotopic analysis and underwent an ethyl acetate-bromine dissolution to segregate the oxide fraction from the metal fraction. Actinide concentrations were determined using a quadrupole–inductively coupled plasma–mass spectrometer (Q-ICP-MS). Three additional samples were sent for morphologic and elemental analysis by scanning electron microscopy (SEM) with Energy Dispersive X-ray (EDX) analysis at the Irradiated Materials Characterization Laboratory (IMCL). Analyses suggest that the material is primarily composed of UO2. with a small fraction of metal. This study draws no single conclusion as to the origin of the insoluble material in the ER. The particle sizes and morphologies observed in SEM micrographs indicate that the larger particles observed may be a result of introducing material to the ER that has not been completely reduced in Oxide Reduction (OR) operations, which precede electrorefining. Smaller particles may be due to reactions with oxygen and moisture present in HFEF. This research suggests that microscopic analysis of fuel particles before and after OR operations (including after distillation) as well as the uranium product collected on the cathode in the ER would increase understanding about particle morphology within the pyrochemical process.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Synergistic effect of cationic and anionic surfactants for the modification of Ca-montmorillonite

Highlights: ► The basal spacing of MMT–CTAB–SDS reaches 5.30 nm. ► MMT–CTAB–SDS shows perfect dispersion property and excellent heat resistance. ► SDS helped to improve the heat resistance and decrease the surface energy of the MMT–CTAB–SDS particles. - Abstract: The synergistic effect of cationic surfactant (CTAB) and anionic surfactant (SDS) for the modification of Ca-montmorillonite (Ca-MMT) has been developed, and the novel cation–anion modified organomontmorillonite (MMT–CTAB–SDS) was prepared. X-ray diffraction (XRD) analysis indicates that the interlayer spacing of montmorillonite was well expanded by the intercalation of CTAB and SDS and the basal spacing increased from 1.54 nm (Ca-MMT) to 5.30 nm (MMT–CTAB–SDS). Thermogravimetric analysis (TG) showed that the MMT–CTAB–SDS displayed excellent heat resistance. Scanning electron microscopy (SEM) analysis proved that the MMT–CTAB–SDS exhibited excellent dispersion property and the plates with few silicate layers can be observed. Contact angle tests indicated that the hydrophilicity of MMT–CTAB–SDS was lower than that of Ca-MMT and higher than that of MMT–CTAB. It was verified that SDS contributed to expanding the interlayer space, further improved the heat resistance of the MMT–CTAB and decreased the surface energy of the MMT–CTAB–SDS particles.

36 MATERIALS SCIENCE↗

Synthesis of one-dimensional porous Co{sub 3}O{sub 4} nanobelts and their ethanol gas sensing properties

Graphical abstract: 1D porous porous Co{sub 3}O{sub 4} nanobelts were synthesized via a facile route without use of any surfactants or organic solvent, exhibiting ethanol gas sensing properties superior to the commercial Co{sub 3}O{sub 4} powders. - Highlights: • One-dimensional porous Co{sub 3}O{sub 4} nanobelts were synthesized. • The belt-like morphology can be finely controlled via adjusting the reaction parameters. • The evolution process of porous Co{sub 3}O{sub 4} nanobelts was investigated. • Porous Co{sub 3}O{sub 4} nanobelts exhibit superior ethanol gas sensing properties. - Abstract: In this paper, one-dimensional porous Co{sub 3}O{sub 4} nanobelts were synthesized via a facile template-free hydrothermal method and subsequent the thermal decomposition. Their microstructures and morphologies were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, thermogravimetric analysis, fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy and N{sub 2} adsorption–desorption techniques. The results indicate that the reaction parameters such as the molar ratio of Co(NO{sub 3}){sub 2}·6H{sub 2}O to C{sub 2}H{sub 4}N{sub 4}, the amount of Co(NO{sub 3}){sub 2}·6H{sub 2}O, the hydrothermal temperature and time play crucial rules in controlling the microstructures and morphologies of the as-prepared cobalt precursors. A possible formation mechanism was proposed. Moreover, the obtained porous Co{sub 3}O{sub 4} nanobelts exhibit ethanol gas sensing properties superior to the commercial Co{sub 3}O{sub 4} powders at a working temperature of 200 °C, suggesting their potential applications as nanosensors.

36 MATERIALS SCIENCE↗

An integrated approach to examine fuel-cladding chemical interaction in HT9/U-10Zr metallic fast reactor fuels: Coupling machine learning with electron microscopy and local mechanical properties analysis

The metallic U-Zr nuclear fuel alloy has garnered renewed interest as a promising candidate for next-generation sodium-cooled fast reactors. Recent studies and technology assessments have identified several areas requiring improvements, enhanced knowledge, and reliable data to strengthen the U-Zr fuel design basis for qualification and commercial applications. One of the most challenging phenomena impacting this fuel system’s performance is fuel-cladding chemical interaction (FCCI). This work aimed to harvest FCCI data by examining selected HT9/U-10Zr (wt. %) fuel samples of prototypic full-length fuel pins through an integrated approach. This approach integrated scanning electron microscopy (SEM) microstructure characterization with localized mechanical properties examination to deepen understanding of FCCI phenomenon in HT9/U-10Zr fuel system. Particularly, this study focused on MFF fuel pins irradiated at Fast Flux Test Facility (FFTF), which aimed to qualify metallic fuel as a driver fuel for FFTF and to assess its viability for larger-scale fast reactors. Electron microscopy provided high confidence in detecting and distinguishing the different FCCI layers, while small-scale mechanical testing (SSMT) probed the mechanical properties of these layers. SEM examination of a MFF-2 pin 192167, with a time averaged inner cladding temperature (TICT) slightly over 500°C, revealed minimal cladding-side FCCI (cladding wastage). In contrast, significantly thicker cladding wastage comprising two distinct sublayers was observed in samples from the thermally hot MFF-3 pin 193045 and MFF-5 pin 195011 where the TICT ranged from 610-635°C. SSMT indicated complete embrittlement in the sublayer adjacent to the fuel and a tendency toward embrittlement in the other sublayer. Additionally, a new machine learning method was developed, validated, and used to quantify cladding wastage thickness. The machine learning method reliably predicted the wastage thickness across various fuel pins and sample cross-sections. Furthermore, the available cladding wastage data from HT9/U-10Zr fuel system demonstrated a strong temperature dependency. However, the dataset remains small, and ongoing research activities are essential to further understand the FCCI phenomenon and develop a reliable FCCI model for enhanced fuel performance simulation under various conditions.

36 - MATERIALS SCIENCE↗

Microstructure, mechanical properties and texture evolution of AZ31 alloy containing trace levels of strontium

The effect of low levels of Sr (0.01, 0.03, 0.05 wt.%) on the microstructure, mechanical properties and texture of AZ31 magnesium alloy has been investigated. Thermodynamic modeling has been used to study the effect of Sr on phase precipitation at different temperatures. Cooling curve analysis reveals a decrease in solidification superheat with the addition of 0.03 wt.% Sr to AZ31. The as-cast microstructures of the alloys have been studied using optical microscopy (OM) and electron probe micro analysis (EPMA). Results show the refining effect of Sr on the grain size and on the {beta}-Mg{sub 17}Al{sub 12} precipitates through growth poisoning and inoculation, respectively. To investigate the mechanical properties of the alloys, as-cast samples were compression tested at elevated temperatures. Hot compression peak stress ({sigma}{sub max}) and critical strain before recrystallization ({epsilon}{sub c}) initially drop but then increase. {sigma}{sub max} first decreases due to the depletion of Al from solid solution and then increases when the amount of the Al-Sr precipitates reach a significant amount. {epsilon}{sub c} drops due to the acceleration of dynamic recrystallization kinetics as a result of grain refinement. It increases with increasing Sr when the concentration Sr in solid solution is increased leading to dislocation pinning and retardation of recrystallization. X-ray texture measurements on the hot compressed and extruded samples show a decrease in maximum intensity of the basal pole figures with increasing Sr as a result of reduced twining and the changes in Al and Sr concentrations in solid solution. - Research Highlights: {yields} Microstructures/precipitates of AZ31+trace levels of Sr were examined by OM and EPMA. {yields} Thermodynamic calculations and cooling curve analysis were used to predict ppt formation. {yields} It has been shown that Sr refines the grains and Mg17Al12 precipitates. {yields} Mechanical properties and texture were studied using hot compression and X-ray diffraction. {yields} Different micro-mechanisms were responsible for mechanical and texture changes.

36 MATERIALS SCIENCE↗

Economic analysis of precious metal recovery from electronic waste through gas-assisted microflow extraction

The recycling of end-of-life (EoL) electronic products is motivated by the enormous investment of resources in their creation and the environmental concerns associated with electronic waste (e-waste). Hydrometallurgical methods that utilize conventional leaching and solvent extraction are often applied to extract target materials from e-waste; however, these techniques have significant technical and economic limitations when extracting high-value, low concentration metals from complex waste streams. This study proposes and evaluates a novel process based on gas-assisted microflow extraction (GAME) that efficiently recovers precious metals from waste printed circuit boards (WPCBs). Further, an economic analysis is conducted to verify the economic feasibility of the GAME-based process at an industrial scale. The economic outputs are further investigated to identify the most cost-effective production strategies, particularly with respect to the plant feedstock rate. It is envisioned that this study may establish a paradigm for making economically-informed decisions for sustainable technologies.

42 ENGINEERING↗

Role of the interface on radiation damage in the SrTiO{sub 3}/LaAlO{sub 3} heterostructure under Ne{sup 2+} ion irradiation

We systematically investigated the microstructural evolution of heteroepitaxial SrTiO{sub 3} (STO) thin films grown on a single crystal LaAlO{sub 3} (LAO) (001) substrate, focusing on the response of the STO/LAO interface to Ne{sup 2+} irradiation at room temperature. Cross sectional transmission electron microscope (TEM) analysis reveals that the LAO crystal amorphizes first after a relatively low dose of damage followed by the amorphization of the STO film after irradiation to a higher dose. While the critical dose to amorphize differs between each material, amorphization begins at the interface and proceeds outward in both cases. Thus, a crystalline/amorphous interface first forms at the STO/LAO interface by a dose of 1 dpa, and then an amorphous/amorphous interface forms when the dose reaches 3 dpa. Scanning TEM and x-ray energy dispersive spectroscopy indicate no significant heavy cation elemental diffusion, though electron energy loss spectroscopy reveals a redistribution of oxygen across the film/substrate interface after Ne{sup 2+} irradiation. Atomistic calculations are used to interpret the experimental findings in terms of the defect properties in each of the two component phases.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Effects of Neutron Irradiation on the Micro/Nano Scale Structure and Fission Product Distribution of TRISO Coated Particle Fuel Kernels from AGR Experiments

The Advanced Reactor Technologies (ART) Program at Idaho National Laboratory (INL) includes the Advanced Gas Reactor (AGR) fuel development and qualification program that consists of fuel fabrication, experiment irradiations, post-irradiation examination (PIE) and safety testing to assess tristructural isotropic (TRISO) fuel performance during normal irradiation and under potential accident conditions. Advanced microscopy work on selected AGR-1 and AGR-2 unirradiated and irradiated fuel specimens is performed as part of the PIE effort. PIE work on fuel from the first experiment irradiation, AGR-1, began at INL in April 2010, and AGR-2 PIE began at INL in July 2014. This work scope includes University of Florida (UF) performing advanced electron microscopy examination and analysis using facilities at the Center for Advanced Energy Studies (CAES), INL or UF’s electron microscopy facilities. Electron microscopic examination and analysis may include scanning transmission electron microscopy (STEM), transmission electron microscopy (TEM), selected area diffraction (SAD), electron energy loss spectroscopy (EELS), electron dispersive spectroscopy (EDS) and atom probe tomography (APT) on the fuel kernels of TRISO-coated fuel particles. The electron microscopy lamellae will be provided by INL and will be available at CAES or Irradiated Materials Characterization Laboratory (IMCL).

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗