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At least 991 records · Page 55

Effect of polyphenols on the rheology, microstructure and in vitro digestion of pea protein gels at various pH

Polyphenols exist widely in plants and interact with plant proteins distinctly depending on the environmental pH. This could potentially affect the gelling property of plant proteins and their digestion. In the present study, pea protein suspensions containing 0 %, 0.5 % and 1 % green tea polyphenols (GTP) were heated to form gels at pH5, pH7, and pH8.5. A strain amplitude sweep showed that the storage modulus (G’) and critical strain of pea protein gels decreased with increased GTP concentration at all examined pH. Gelation dynamic showed gelling of pea protein-GTP was delayed at pH7 and pH8.5 compared to the control. Differential scanning calorimetry showed that pea proteins became less heat resistant in the presence of GTP at pH5 and pH7, but not at pH8.5. Ultra-small and small-angle X-ray scattering showed that the radius of gyration of small- and medium-sized aggregates in pea protein gels was increased ~10–16 % and 22–30 % at pH7 and pH8.5, respectively when 1 % GTP was present. Finally, under such pH conditions, the proportion of structure with a radius of ~10–200 nm was increased in pea protein-GTP gels based on the volume size distribution. In vitro digestion found the soluble protein content of digesta of pea protein-GTP gels had a 5–8.5 % decrement with the presence of larger peptides when compared to pea protein gels.

59 BASIC BIOLOGICAL SCIENCES↗

Temperature-Dependent Thermal and Mechanical Properties of a Wire Arc Additively Manufactured Low Transformation Temperature Steel

Recent research has studied the use of low transformation temperature (LTT) martensite steel as feedstock for wire arc additive manufacturing (WAAM) and low tensile residual stresses or compressive residual stresses were detected in the printed walls. These residual stress states help to improve printed product properties such as fatigue strength and corrosion resistance. However, the thermal and mechanical properties of WAAM printed LTT martensite steel walls are largely unknown. In this work, a printed LTT martensite steel was characterized for its thermal, metallurgical, and mechanical behavior at room and elevated temperatures. The temperature-dependent specific heat capacity, thermal expansion, atomic lattice spacing, and tensile properties were measured during both heating and cooling and related to observed microstructural features and computational thermodynamics predictions. These results revealed a large hysteresis in the martensitic transformation, with a martensite start temperature of 240 °C and austenite start temperature of 680 °C. Additional thermal cycles and specimen orientation did not affect the printed specimen austenite and martensite transformations. However, it was observed that the printed metal may exhibit tempering embrittlement at about 350 °C but further studies are needed to confirm that. Further, these results suggest that a temperature control of 250 °C to 350 °C during WAAM is needed to maximize the stress reduction potential of the LTT250 martensite steel. Opportunities for future implementation of LTT martensite steels and optimization of additive manufacturing process conditions are identified.

36 MATERIALS SCIENCE↗

Amorphous complexions alter the tensile failure of nanocrystalline Cu-Zr alloys

Grain boundary-based mechanisms are known to control the plastic deformation and failure of nanocrystalline metals, with manipulation of the boundary structure a promising path for tuning this response. In this study, the role of interfacial structural disorder on plasticity and failure of nanocrystalline Cu-Zr alloys is investigated with in situ scanning electron microscopy tensile deformation experiments. Two model materials are created, one with only the typical ordered grain boundaries and another with amorphous intergranular films interspersed into the boundary network, while the microstructures are otherwise identical. Hence, the importance of complexion type on plasticity and failure is isolated by only varying complexion structure. Here, the tensile experiments show that failure of the samples containing amorphous films is significantly retarded, as evidenced by an increase in the cross-sectional area reduction, a decrease in the occurrence of shear-dominated failure, a decrease in strain localization, and fracture surfaces with more elongated dimple features. As a whole, this study provides direct evidence that structural disorder at the grain boundaries can be beneficial for improving the ductility of nanocrystalline metals.

36 MATERIALS SCIENCE↗

Designed Iron Single Atom Catalysts for Highly Efficient Oxygen Reduction Reaction in Alkaline and Acid Media

Abstract Single atom catalysts (SACs) have attracted much attentions due to their advantages of high catalysis efficiency and excellent selectivity. However, for industrial applications, synthesis of SACs in large and practical quantities is very important. The challenge is to develop synthesis methods with controllability and scalability. Herein, a well‐characterized and scalable method is demonstrated to synthesize atomically dispersed iron atoms coordinated with nitrogen on graphene, SAFe @ NG, with high atomic loading (≈4.6 wt%) through a one‐pot pyrolysis process. The method is scalable for the fabrication of Fe SACs with high quantities. The Fe–N–G catalyst exhibits high intrinsic oxygen reduction reaction (ORR) performance, reaching half potential of 0.876 and 0.702 V in alkaline and acidic solutions, respectively, with excellent microstructure stability. Furthermore, the density functional theory (DFT) simulation confirms that the Fe atoms in coordination with four nitrogen atoms, FeN4, in graphene is the active center for the 4‐electron ORR process. This work demonstrates an efficient design pathway for single atom catalysts as highly active and stable electrocatalysts for high‐performance ORR applications.

Zhao, Shiyong↗

Cost Models for MMC Manufacturing Processes

The quality cost modeling (QCM) tool is intended to be a relatively simple-to-use device for obtaining a first-order assessment of the quality-cost relationship for a given process-material combination. The QCM curve is a plot of cost versus quality (an index indicating microstructural quality), which is unique for a given process-material combination. The QCM curve indicates the tradeoff between cost and performance, thus enabling one to evaluate affordability. Additionally, the effect of changes in process design, raw materials, and process conditions on the cost-quality relationship can be evaluated. Such results might indicate the most efficient means to obtain improved quality at reduced cost by process design refinements, the implementation of sensors and models for closed loop process control, or improvement in the properties of raw materials being fed into the process. QCM also allows alternative processes for producing the same or similar material to be compared in terms of their potential for producing competitively priced, high quality material. Aside from demonstrating the usefulness of the QCM concept, this is one of the main foci of the present research program, namely to compare processes for making continuous fiber reinforced, metal matrix composites (MMC's). Two processes, low pressure plasma spray deposition and tape casting are considered for QCM development. This document consists of a detailed look at the design of the QCM approach, followed by discussion of the application of QCM to each of the selected MMC manufacturing processes along with results, comparison of processes, and finally, a summary of findings and recommendations.

Elzey, Dana M.↗

Effect of Weld Tool Geometry on Friction Stir Welded Ti-6Al-4V

In this study, flat 0.250" thick Ti-6Al-4V panels were friction stir welded (FSWed) using weld tools with tapered pins. The five different pin geometries of the weld tools included: 0 degree (straight cylinder), 15 degree, 30 degree, 45 degree, and 60 degree angles on the frustum. All weld tools had a smooth 7 degree concave shoulder and were made from microwave sintered tungsten carbide. For each weld tool geometry, the FSW process parameters were optimized to eliminate internal defects. All the welds were produced in position control with a 2.5 degree lead angle using a butt joint configuration for the panels. The process parameters of spindle rpm and travel speed were varied, altering the hot working conditions imparted to the workpiece. Load cells on the FSWing machine allowed for the torque, the plunge force, and the plow force to be recorded during welding. Resulting mechanical properties were evaluated from tensile tests results of the FSWjoints. Variations in the material flow were investigated by use of microstructural analysis including optical microscopy (OM), scanning electron microscopy (SEM), and orientation image mapping (aIM).

Querin, Joseph A.↗

Vitrification of Inactive Incineration Ash in a Full Industrial Scale In Can Melter - 20502

In the framework of the H2020 THERAMIN project funded by the European Commission, CEA performed a pilot-scale trial consisting of the vitrification of inactive ash (Al, Ca, Si, Zn, Bi, K, Mg, etc.) using the In- Can Melter technology. These ashes were coming from incineration of simulated technological wastes such as cotton, latex, neoprene, polyethylene. The borosilicate glass feasibility was first evaluated at a laboratory scale (10-100 g of glass). The volatile behavior of fly ash was controlled by pelletizing to avoid pipes clogging when performing the pilot scale test. A 10 wt.% inorganic binder was added to obtain cohesive pellets. The glass frit composition was selected and its ratio was fixed at 50 wt.%. After this step, a bench test (1 kg of glass) was done to verify the absence of container corrosion. Finally, it was followed by a pilot scale test (50 kg of glass) with 75,000 ash pellets used. The same glass microstructure and chemical composition were observed at each scale. Typical crystals of apatites (Ca, P), zincochromites (Zn, Cr, Al) and bismuth alloys (Bi, Sb) dispersed into a borosilicate glass matrix were observed. The chemical durability of the wasteform was measured during 28 days in a 90 deg. C water. Although there were durable crystalline phases, the hydrolysis rate of the vitreous part is relatively high because of the B and Na contents. However, leach rate profiles suggest that an alteration layer will form, leading to an alteration rate decrease. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Establishing an acoustic-property relationship in laser powder bed fusion with machine learning

Quality control of Laser Powder Bed Fusion (PBF-LB) additively manufactured parts is an important hurdle inhibiting the technology’s use structural applications. Acoustic monitoring of the laser powder bed fusion process can detect defects in-situ that are known to degrade mechanical properties. However, processing-structure-property (PSP) relationships are required to extrapolate from detected defects to part performance. Here, this study explores how acoustics may be a suitable signature linking processing conditions to properties, thus effectively substituting for structure in the PSP relationship. Establishing such a relationship would enable a part’s mechanical performance to be directly predicted from its acoustic signature, reducing the need for destructive testing or microstructural analysis to ensure a part will meet performance requirements. One hundred CoCrFeMnNi high entropy alloy tensile bars were printed across 13 process conditions in a series of 6 prints. The acoustic signatures of these tensile bars were used to train machine learning models to predict each part’s mechanical properties. By using both process information and acoustic information to predict mechanical properties, yield strength was predicted 18% more accurately and ductility to failure was predicted 10% more accurately than is achieved when using duplicate parts to predict part performance. Finally, individual acoustic frequencies were investigated to determine why acoustic signatures improve mechanical property predictions and the potential physical origins of these signatures. This work demonstrates how blending acoustics, process information, and machine learning can provide in-situ diagnostics of mechanical properties and improve the reliability of the PBF-LB process.

Acoustic emission↗

Spatially correlated incommensurate lattice modulations in an atomically thin high-temperature Bi 2.1 Sr 1.9 CaCu 2.0 O 8+y superconductor

Strong variations in superconducting critical temperatures in different families of the cuprate perovskites, even with similar hole doping in their copper-oxygen planes, suggest the importance of lattice modulation effects. The one-dimensional incommensurate lattice modulation (ILM) of Bi 2 Sr 2 CaCu 2 O 8+y , with the average atomic positions perturbed beyond the unit cell6, offer s an ideal test ground for studying the interplay between superconductivity and the long-range incommensurate lattice fluctuations. Here we report Scanning nano X-ray Diffraction (SnXRD) imaging of incommensurate lattice modulations in Bi 2 Sr 2 CaCu 2 O 8+y Van der Waals heterostructures of thicknesses down to two-unit cells. Using SnXRD, we probe that the long-range and short-range incommensurate lattice modulations in bulk sample surface with spatial resolution below 100 nm. We find that puddle-like domains of ILM of size uniformly evolving with dimensionality. In the 2-unit cell thin sample, it is observed that the wavevectors of the long- and short-range orders become anticorrelated with emerging spatial patterns having a directional gradient. The emerging patterns, originated by tiny tuning of lattice strain, induce static mesoscopic charge density waves. Finally, our findings thus demonstrate that the strain can be used to tune and control the electromagnetic properties of two-dimensional high-temperature superconductors.

36 MATERIALS SCIENCE↗

Chemical durability and corrosion-induced microstructure evolution of compositionally complex titanate pyrochlore waste forms with uranium incorporation

Chemical durability of compositionally-complex rare-earth titanate pyrochlore solid solutions with or without uranium incorporation was investigated by semi-dynamic leaching testing. A Ti-enriched amorphous passivation film formed on the surface due to the surface alteration-reorganization mechanism with preferential release of the weakly oxygen-bonded rare earth elements. Elemental release was found to be strongly correlated with chemical disorder, with a negligible correlation with entropy. The release rate of the uranium gradually decreased with increasing numbers of components, implying a possibility of designing and optimizing waste form performance with enhanced chemical durability by controlling composition complexity and chemical disorder for effective nuclear waste management.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Towards Thermomechanical Processing of Alloy 709: Progress in Defining High-Temperature Deformation-Recrystallization "Space"

The Advanced Reactor Technologies (ART) Program has established a multi-year plan to develop Alloy 709 advanced stainless steel, generate the data package and develop material-specific design parameters in qualifying it as a new structural material for Class A construction in the American Society of Mechanical Engineers (ASME) Boiler and Pressure Vessel Code, Section III, Division 5, High Temperature Reactors (ASME 2025). In collaboration with material vendors, the Advanced Materials Development activities under ART have successfully scaled the Alloy 709 plate form production from a laboratory heat of 500 pounds to commercial heats totaling 133,000 pounds of Alloy 709 plate fabricated from three heats. The goal of the overall Alloy 709 development program is to establish the necessary microstructural and mechanical properties relationship for Alloy 709 to ultimately develop fabrication parameters for other product forms such as bars, pipes, and forgings using the available ART Alloy 709 materials. This study will enable its deployment in the industry as an advanced construction material for high-temperature components. The objective of this Alloy 709 development work in FY 2025 is to experimentally determine the high-temperature deformation-recrystallization response of the Alloy 709 heats and to experimentally generate true stress-true strain data for Alloy 709 using the available commercial heat plate materials. Integral to this work is the previous characterization of the as-rolled materials and the determination of an effective solution-annealing process, which was reported in Y. Wang et al., 2023, and the evaluation of the effect of controlled cooling on the resultant precipitation in these commercial heats. This report summarizes and builds on the results of the previous reports to assess the high-temperature deformation behavior as a function of deformation temperature, strain and strain rate using commercial Alloy 709 heat 58776-3RB fabricated by G. O. Carlson and heat 529900-02 fabricated by Allegheny Technologies Incorporated (ATI) Specialty Rolled Products.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Growth parameters for aligned microstructures in directionally solidified aluminum-bismuth monotectic

Microstructures are shown for directionally solidified Al-3.4 wt pct Bi alloys with 0.2 wt pct Fe and 0.6 wt pct Fe additions. The third element causes the LI/SI + LII growth interface to become cellular. The bismuth forms at the cell nodes, appearing either as uniformly spaced arrays of spheres in the case of 0.2 wt pct Fe, or as an irregular network in the case of 0.6 wt pct Fe. Changes in the growth conditions which are known to control cellular structure are seen to have a similar effect on the bismuth spacing, with the cross sectional spacing varying as the inverse of G (Temperature gradient) x R(Growth rate).

Parr, R. A.↗

The low cycle fatigue behavior of a plasma-sprayed coating material

Single crystal nickel-base superalloys employed in turbine blade applications are often used with a plasma spray coating for oxidation and hot corrosion resistance. These coatings may also affect fatigue life of the superalloy substrate. As part of a large program to understand the fatigue behavior of coated single crystals, fully reversed, total strain controlled fatigue tests were run on a free standing NiCoCrAlY coating alloy, PWA 276, at 0.1 Hz. Fatigue tests were conducted at 650 C, where the NiCoCrAlY alloy has modest ductility, and at 1050 C, where it is extremely ductile, showing tensile elongation in excess of 100 percent. At the lower test temperature, deformation induced disordering softened the NiCoCrAlY alloy, while at the higher test temperature cyclic hardening was observed which was linked to gradual coarsening of the two phase microstructure. Fatigue life of the NiCoCrAlY alloy was significantly longer at the higher temperature. Further, the life of the NiCoCrAlY alloy exceeds that of coated, /001/-oriented PWA 1480 single crystals at 1050 C, but at 650 C the life of the coated crystal is greater than that of the NiCoCrAlY alloy on a total strain basis.

Gayda, J.↗

Low cycle fatigue behaviour of a plasma-sprayed coating material

Single crystal nickel-base superalloys employed in turbine blade applications are often used with a plasma spray coating for oxidation and hot corrosion resistance. These coatings may also affect fatigue life of the superalloy substrate. As part of a large program to understand the fatigue behavior of coated single crystals, fully reversed, total strain controlled fatigue tests were run on a free standing NiCoCrAlY coating alloy, PWA 276, at 0.1 Hz. Fatigue tests were conducted at 650 C, where the NiCoCrAlY alloy has modest ductility, and at 1050 C, where it is extremely ductile, showing tensile elongation in excess of 100 percent. At the lower test temperature, deformation induced disordering softened the NiCoCrAlY alloy, while at the higher test temperature cyclic hardening was observed which was linked to gradual coarsening of the two phase microstructure. Fatigue life of the NiCoCrAlY alloy was significantly longer at the higher temperature. Further, the life of the NiCoCrAlY alloy exceeds that of coated, /001/-oriented PWA 1480 single crystals at 1050 C but at 650 C the life of the coated crystal is greater than that of the NiCoCrAlY alloy on a total strain basis.

Gayda, J.↗

Detailed analysis of Honeywell In-Space Accelerometer data - STS-32

The Honeywell In-Space Accelerometer (HISA) system collected data in the mid-deck area of the Shuttle Columbia during the flight of STS-32, January 1990. The resulting data were to be used to investigate the response of crystal microstructure to different types of residual acceleration. The HISA is designed to detect and record transient and oscillatory accelerations. The sampling and electronics package stored averaged accelerations over two sampling periods; two sampling rates were available: 1 Hz and 50 Hz. Analysis of the HISA data followed the CMMR Acceleration Data Processing Guide, considering in-house computer modelling of a float-zone indium crystal growth experiment. Characteristic examples of HISA data showing the response to the primary reaction control system, Orbiter Maneuvering System operations, and crew treadmill activity are presented. Various orbiter structural modes are excited by these and other activities.

Rogers, Melissa J. B.↗

Pulsed laser deposition and structural evolution of BaF 2 nanolayers in Eu-doped BaF 2 /Al 2 O 3 layered optical nanocomposite thin films

Here, we have developed a pulsed laser deposition (PLD) geometry for the growth of uniform BaF 2 nanoscale thin films, through control of the deposition conditions. Our goal is to use the BaF 2 layers with controllable structure as component layers in layered optical nanocomposites. The structure of the BaF 2 nanolayer evolves as a function of the layer thickness: BaF 2 grows via a layer-by-layer growth mode on Al 2 O 3 ; the layers are amorphous for a thickness < 3 nm, and then become nanocrystalline as the layer thickness increases. The BaF 2 nanocrystals have an FCC crystal structure with a weak < 111 > texture that becomes stronger for thicker films. We then demonstrate that our BaF2 films can be introduced into layered Al 2 O 3 /BaF 2 /EuO x nanocomposite films, which allows for control of the relative position of the Eu ions and the BaF 2 layer. Cross-section samples of the multilayered films show interfacial intermixing between the layers, which is related to implantation during the PLD process. This intermixing enables the incorporation of Eu ions into BaF 2 layers and form a thin Eu-doped BaF 2 nanolayer at the interface. The layered nanocomposite films show photoluminescence (PL) emission from Eu 3+ ions, and the PL intensity changes can be correlated with the crystallinity and crystal size changes in the BaF 2 layer. Our results provide guidance for achieving thin film nanocomposite materials with controllable structure and photoluminescence behavior for light emitting diodes, photovoltaics and other optical applications.

36 MATERIALS SCIENCE↗

Coupled Growth in Hypermonotectics

The overall objective of this project is to obtain a fundamental understanding of the physics controlling solidification processes in immiscible alloy systems. The investigation involves both experimentation and the development of a model describing solidification in monotectic systems. The experimental segment was designed to first demonstrate that it is possible to obtain interface stability and steady state coupled growth in hypermonotectic alloys through microgravity processing. Microgravity results obtained to date have verified this possibility. Future flights will permit experimental determination of the limits of interface stability and the influence of alloy composition and growth rate on microstructure. The objectives of the modeling segment of the investigation include prediction of the limits of interface stability, modeling of convective flow due to residual acceleration, and the influence of surface tension driven flows at the solidification interface. The study of solidification processes in immiscible alloy systems is hindered by the inherent convective flow that occurs on Earth and by the possibility of sedimentation of the higher density immiscible liquid phase. It has been shown that processing using a high thermal gradient and a low growth rate can lead to a stable macroscopically planar growth front even in hypermonotectic alloys. Processing under these growth conditions can avoid constitutional supercooling and prevent the formation of the minor immiscible liquid phase in advance of the solidification front. However, the solute depleted boundary layer that forms in advance of the solidification front is almost always less dense than the liquid away from the solidification front. As a result, convective instability is expected. Ground based testing has indicated that convection is a major problem in these alloy systems and leads to gross compositional variations along the sample and difficulties maintaining interface stability. Sustained low gravity processing conditions are necessary in order to minimize these problems and obtain solidification conditions which approach steady state.

Andrews, J. Barry↗

Forging of Advanced Disk Alloy LSHR

The powder metallurgy disk alloy LSHR was designed with a relatively low gamma precipitate solvus temperature and high refractory element content to allow versatile heat treatment processing combined with high tensile, creep and fatigue properties. Grain size can be chiefly controlled through proper selection of solution heat treatment temperatures relative to the gamma precipitate solvus temperature. However, forging process conditions can also significantly influence solution heat treatment-grain size response. Therefore, it is necessary to understand the relationships between forging process conditions and the eventual grain size of solution heat treated material. A series of forging experiments were performed with subsequent subsolvus and supersolvus heat treatments, in search of suitable forging conditions for producing uniform fine grain and coarse grain microstructures. Subsolvus, supersolvus, and combined subsolvus plus supersolvus heat treatments were then applied. Forging and subsequent heat treatment conditions were identified allowing uniform fine and coarse grain microstructures.

Gabb, Timothy P.↗