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Flow Patterns, Microstructure and Mechanical Properties of AZ31/Al6061 Dissimilar Friction Stir-Welded Joints

Dissimilar joints between die-cast AZ31 and extruded Al6061-T6 were joined using friction stir welding technology at a constant transverse speed (50 mm/min) and rotation rate of 800 or 1000 rpm. The flow patterns, microstructure evolution and intermetallic compounds in dissimilar joints were studied by optical and scanning electron microscopy. The relationship between microstructure and tensile properties was analyzed. The microhardness distribution along the horizontal centerline in cross section was investigated. Local flow without obvious mixing existed between Mg and Al metals in the tool shoulder-affected zone. For the tool-pin-affected zone, two typical zones, namely, the “extrusion zone” and “flow zone” existed because of the different flow modes of the plastic metals. The phase analysis showed that intermetallic compounds, including Al{sub 12}Mg{sub 17} and Al{sub 3}Mg{sub 2} formed in banded structures. Phase analysis showed that a joint with welding parameters of 800 rpm and 50 mm/min (Joint-500) had good mechanical properties because of the more uniform microstructure distribution and fewer intermetallic compounds. Fracture analysis indicated some microvoids and lamellate intermetallic compounds in the fracture surface of the joint with welding parameters of 1000 rpm and 50 mm/min (Joint-1000), which deteriorated its tensile strength significantly.

36 MATERIALS SCIENCE↗

The Effect of Different Annealing Conditions on the Anisotropy of the Fracture Toughness of Ti-6Al-4V

The room-temperature tensile and fracture toughness properties of Ti-6Al-4V plate were tested to characterize the effect of rolling direction on the fracture toughness in two different heat treatment conditions. Optical and scanning electron microscopy was used to characterize the microstructure and fracture surfaces. It was found that beta annealing increased the fracture toughness compared to a mill annealed product in all three orientations relative to the rolling direction; however, it had minimal effects on strength and modulus. Ti-6Al-4V was found to be isotropic in fracture toughness, varying 0.48% in the beta annealed condition and 6.4% in the mill annealed condition.

36 MATERIALS SCIENCE↗

Microstructural Characterization of the U-9.1Mo Fuel/AA6061 Cladding Interface in Friction-Bonded Monolithic Fuel Plates Irradiated in the RERTR-6 Experiment

Low-enrichment (U-235 < 20%) U-Mo monolithic fuel is being developed for use in research and test reactors. The earliest design for this fuel that was investigated via reactor testing was comprised of a nominally U-10Mo fuel foil encased in AA6061 (Al-6061) cladding. For a fuel design to be deemed adequate for final use in a reactor, it must maintain dimensional stability and retain fission products throughout irradiation, which means that there must be good integrity at the fuel foil/cladding interface. To investigate the nature of the fuel/cladding interface for this fuel type after irradiation, fuel plates that were tested in INL's Advanced Test Reactor (ATR) were subsequently characterized using optical metallography, scanning electron microscopy, and transmission electron microscopy. Results of this characterization showed that the fuel/cladding interaction layers present at the U-Mo fuel/AA6061 cladding interface after fabrication became amorphous during irradiation. Up to two main interaction layers, based on composition, could be found at the fuel/cladding interface, depending on location. After irradiation, an Al-rich layer contained very few fission gas bubbles, but did exhibit Xe enrichment near the AA6061 cladding interface. Another layer, which contained more Si, had more observable fission gas bubbles. Adjacent to the AA6061 cladding were Mg-rich precipitates, which was in close proximity to the region where Xe is observed to be enriched. In samples produced using a focused ion beam at the interaction zone/AA6061 cladding interface were possible indications of porosity/debonding, which suggested that the interface in this location is relatively weak.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Modeling of heat transfer, fluid flow and solidification microstructure of nickel-base superalloy fabricated by laser powder bed fusion

Laser-Powder Bed Fusion (L-PBF), an additive manufacturing process, produces a distinctive microstructure that closely resembles the weld metal microstructure but at a much finer scale. The solidification parameters, particularly temperature gradient and solidification rate, are important to study the as-built microstructure. In the present paper, a computational framework with meso-scale resolution is developed for L-PBF of Inconel ® 718 (IN718), a Ni-base superalloy. The framework combines a powder packing model based on Discrete Element Method and a 3-D transient heat and fluid flow simulation. The latter, i.e., the molten pool model, captures the interaction between laser beam and individual powder particles including free surface evolution, surface tension and evaporation. The solidification parameters, calculated from the temperature fields, are used to assess the solidification morphology and grain size using existing theoretical models. The IN718 coupon built by L-PBF are characterized using optical and scanning electron microscopies. Finally, the experimental data of molten pool size and solidification microstructure are compared to the corresponding simulation results.

36 MATERIALS SCIENCE↗

Large-scale additive manufacturing of self-heating molds

Large-scale material extrusion additive manufacturing technology is becoming the new mainstream technology for scaled-up composite mold and die applications. This paradigm shift in composite processing technology is primarily driven by out-of-autoclave tooling applications, in which fiber reinforced composite molds with scaled-up sizes and embedded heating elements are attractive. The present research describes the design, manufacturing, and testing of self-heating composite molds fabricated via a large-scale pellet extrusion 3D printing machine with an integrated wire co-extrusion tool. Polycarbonate (PC) composites reinforced with carbon fiber (PC/CF; 20 wt.%) and glass fiber (PC/GF; 20 wt.%) were used to fabricate mold parts. Joule heating thermal test results showed that uniform temperatures (~100 °C) were achieved for both PC/CF and PC/GF mold surfaces, using a custom-made feedback control power supply and infrared thermography. Mechanical characterizations, including tensile and flexural testing were performed on the wire-embedded and un-wired PC/CF and PC/GF base specimens to investigate the impact of the fiber reinforcement as well as the embedded wires. In the direction of extrusion, the ultimate tensile stress of PC/CF was 105 MPa, and that of PC/GF was 73 MPa, while the neat PC value was 64 MPa. Inner-bead voids and interfacial gaps were observed and characterized via optical and scanning electron microscopy. The embedded wires and inner bead impacted the mechanical properties of the composites. Furthermore, the stiffness of the wire-embedded mold was still satisfactory, proving that the technology can be used to fabricate additively manufactured out-of-oven/autoclave molds.

36 MATERIALS SCIENCE↗

An attempt to validate the ultra-accelerated microbar and the concrete performance test with the degree of AAR-induced damage observed in concrete structures

There is little knowledge about the relation between AAR-induced damage observed in structures and the expansion potential obtained with accelerated tests. In this study, aggregates used in structures damaged by AAR were tested with the microbar test (MBT/AFNOR XP 18-594) and the concrete performance test (CPT/AFNOR P18-454). After the tests, the samples were examined using optical and scanning electron microscopy. Based on the results, the significance of the microbar test has to be examined very critically. The agreement of measured expansion, reacted rock types and the composition of the reaction products between the on-site concrete and the reproduced concrete subjected to the CPT clearly indicates that the reaction mechanisms in the structure and in the concrete performance test are comparable. As such, the concrete performance test seems to be an appropriate tool to test the potential reactivity of specific concrete mixtures.

36 MATERIALS SCIENCE↗

Observations on dedolomitization of carbonate concrete aggregates, implications for ACR and expansion

Some carbonate aggregates used in concrete are unstable in a high alkaline solution, which is present also in pore solution of cement binder. This paper investigates the process of dedolomitization of carbonate aggregate rocks and mortar bars. Selected aggregates, limestone and dolostone are of high purity without reactive silica involvement confirmed by the XRD and the XRF. For the process of dedolomitization the effect of various temperatures, solutions and time was examined. In this investigation, measurements of expansion, optical and scanning electron microscopy (SEM), energy dispersive spectrometry (EDS) and X-ray diffraction were used. Te results indicate that the process of dedolomitization occurred not only in the NaOH solution but also in the water on the mortar bar with virgin dolostone aggregate. Elevated temperature, 60 °C, increased the rate of reaction. Furthermore, the rate of reaction significantly correlates with time, which has also been confirmed through the Rietveld analysis. -- Highlights: •The dedolomitization caused no expansion. •It occurs in the dolostone aggregate without reactive silica involvement. •It has taken place already with the presence of the cement binder. •A significant alteration occurred: formation of rims, new pores and phases.

36 MATERIALS SCIENCE↗

Processing and mechanical characterization of short carbon fiber-reinforced epoxy composites for material extrusion additive manufacturing

Fiber-reinforced polymer composites have been extensively utilized in recent years as feedstock materials for material extrusion additive manufacturing (AM) processes to improve strength, stiffness, and functionality of printed parts over unfilled printed polymers. However, the widespread adoption of AM of fiber-reinforced polymer composites requires a deeper understanding of the process-structure-property relationships in printed components, and such relationships are not well understood yet. Fiber length is critically important to the mechanical performance of short fiber composites, but very few studies to-date have focused on how the fiber length distribution (FLD) evolves during processing of composite feedstocks and how this evolution affects printing behavior and mechanical properties in 3D-printed composites. Here, FLD is measured for carbon fiber reinforced epoxy composites over a wide range of ink compositions and shear mixing times, and the distributions are fit with a Weibull-type distribution function. The effects of FLD on the tradeoff between ink processability, ink rheology, printing behavior and mechanical properties are investigated. Furthermore, the effects of printing parameters (nozzle size and print speed) on mechanical anisotropy and fiber orientation distribution (FOD) in printed composites are explored. Mechanical properties of printed composites are characterized via 3 pt-flexural testing, and microstructure is investigated using optical and scanning electron microscopy (SEM), and x-ray computed tomography. Finally, the fitted Weibull parameters are fed into a composite model that incorporates FLD and FOD, and model predictions are found to be in excellent agreement with experimental observations.

3D printing↗

Macro-level mechanical interlocking: A rapid joining approach for additively manufactured compression molded composite panels

Composite joining typically involves multiple steps, such as drilling and surface treatment, as part of the manufacturing process, which leads to low throughput and long cycle times. In the present study, we demonstrated a macro-level mechanical interlocking (MI) based, rapid joining technique to assemble additively manufactured compression molded (AMCM) panels, enabling the production of parts larger than the mold dimensions. Composite panels made of 20 wt% short carbon fiber reinforced acrylonitrile butadiene styrene (CF/ABS) were joined using MI features of various geometries, namely tree (TR), dovetail (Dov), rectangle 2 (Rect2), and rectangle 1 (Rect1), and their in-plane strength was evaluated. The resultant strength of the tested MI joints reached up to 74 % of the baseline tensile strength (i.e., the ‘no joint’ case). Observations from optical and scanning electron microscopy revealed inadequate polymer diffusion between the adherends, indicating that the joint strength was primarily derived from mechanical interlocking. Additionally, the fracture surfaces exhibited stress-whitening marks, which were characterized using differential scanning calorimetry (DSC). The increase in melting enthalpy suggested local stretching of polymer chains due to MI. Finite element analysis (FEA) indicated that the Rect1 MI feature, which generated the lowest stress concentration, outperformed the others in terms of joint strength, achieving 42 MPa. As a demonstration of the MI joining method, a battery box tray measuring 108 cm × 34 cm using a mold with an effective dimension of 36 cm × 34 cm successfully manufactured, resulting in a part with an area three times larger than the mold. In conclusion, this study presents a promising approach to improving composite joining techniques while minimizing production complexities.

In-plane joining↗

Formation of zinc carbonate phases on dissolving calcite, aragonite, and vaterite in acidic aqueous solutions

Calcium carbonate (CaCO 3 ) minerals serve as a major sink to retain metal ions through mineral-water interfacial reactions in which the capacity and long-term stability of contaminant uptake are influenced by coupled dissolution and precipitation reactions of both primary and secondary carbonate minerals (i.e., mineral replacement). Notably, recent studies of calcite reactivity in acidic solutions containing high levels of metal ions demonstrated complex behavior under conditions of sustained disequilibrium. Here, we explored the reactivity of three CaCO 3 polymorphs (calcite, aragonite, and vaterite) with acidic Zn 2+ -containing aqueous solutions using a suite of imaging techniques including optical and scanning electron microscopies, synchrotron-based micro X-ray fluorescence, and transmission X-ray microscopy. Zn uptake by calcite occurred through a two-step process: the formation of a thin layer of the zinc precipitate on the substrate surface followed by the growth of fibrous and radiating hydrozincite particles from the layer. In contrast, Zn uptake by aragonite occurred by mineral replacement where the secondary Zn carbonate phase preserved the external morphology of the original crystal (i.e., a pseudomorph). The replacement of vaterite by hydrozincite occurred within the confined space beneath the porous shell of vaterite, signifying that the primary mechanism driving Zn carbonate precipitation was chemical exchange through the pores. When multiple CaCO 3 polymorphs coexisted, the replacement of aragonite and vaterite occurred preferentially over that of calcite. These results demonstrate the distinct morphological and mineralogical controls over the reactivities of calcium carbonate minerals with Zn 2+ under acidic conditions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Impacts of irregularly-distributed acidified brine flow on geo-chemo-mechanical alteration in an artificial shale fracture under differential stress

The efficacy of geological carbon sequestration is reliant on the integrity of the caprock and its resistance to physical and chemical alteration. Caprocks with high abundance of reactive carbonates like calcite are susceptible to acid-promoted dissolution and can result in structural weakening. This work investigates the effect of acidified brine flow through an artificially fractured, high-carbonate (30 % by XRD) shale under differential compressive stress. Cylindrical samples were cut in half vertically and milled to create an artificial fracture with interlocking asperities and open channels. Samples were sheared with a single applied stress in a custom flow cell housed within an industrial CT scanner. Further, either acidic (pH 4) or reservoir-simulated (pH 9.5) brine was flowed through the artificial fracture for 7–8 days under reservoir pressure and room temperature. Model simulations indicate flow mainly occurred in open channels, with limited flow between overlapping asperities. Analysis of fracture surfaces by optical and scanning electron microscopy show increased surface alteration and roughness after exposure to pH 4 versus pH 9.5 brine indicating mineral dissolution/loss, and this effect is greater in areas that receive the highest brine flows. Similarly, surface analysis by scratch testing shows fracture toughness decreases more after exposure to acidic versus reservoir-simulated brine, with the greatest alteration in areas of highest acidic brine flows. Despite weakening, no shear slip occurred. Overall, the results indicate that acidified brine can result in significant physical and geomechanical alteration of irregular fracture surfaces in shale caprock, with greatest effects in preferential flow regions.

58 GEOSCIENCES↗

Effect of high temperature preoxidation treatment on the oxidation behavior of MoSi 2 - and WSi 2 –Al 2 O 3 composites

Composites of 30 vol% MoSi 2 -70 vol% Al 2 O 3 and 30 vol% WSi 2 -70 vol% Al 2 O 3 were prepared via sintering at 1600 °C in argon. The high-temperature preoxidation treatments were applied at 1000°-1200 °C for 10–120 min in air. The non-isothermal oxidation tests were conducted in air at temperatures ranging between 50° and 870 °C to study and understand the influence of the alumina phase and preoxidation process on the low-temperature oxidation behavior. The optical and scanning electron microscopy, X-ray diffraction, X-ray photoelectron and Raman spectroscopy were used to characterize the surface layers formed. The oxidation-induced mass gains were substantially reduced by 82.1–99.8%, implying their enhanced oxidation resistance. This was due to the formation of highly dense, protective surface layers with a sufficient thickness (3.1–14.2 μm). The structural and surface analyses revealed their complex chemistries, since the ternary (Mo–Si–Al, W–Si–Al) intermetallic, mullite, alumina and silica phases with high oxidation resistances were identified within these surface features. In addition, the high-temperature electrical properties of the composites were highly preserved after the preoxidation treatment, and their electrical conductivities were measured as 45.1–78.6 S/cm at 800 °C and 40.1–69.1 S/cm at 900 °C.

36 MATERIALS SCIENCE↗

Electron backscatter diffraction analysis of a CZT growth tip from a vertical gradient freeze furnace

Electron backscatter diffraction (EBSD) was used to characterize the growth-tip region of a 4.2-cm diameter CdZnTe (CZT) boule grown using low-pressure Bridgman method in a vertical gradient freeze furnace. The boule was sectioned and polished and a section taken along the boule longitudinal centerline with an approximate surface area of 1-cm 2 was used for optical and scanning electron microscopy. A collage was assembled using EBSD/SEM images to show morphological features, e.g., twin structure, grain structure, and overall crystal growth direction. Severely twinned regions originating from the tip and side walls were observed. The overall growth orientation was close to (1 1 0) and (1 1 2) directions. In some regions, the (0 0 1) poles of the CZT matrix aligned with the growth direction, while twins aligned such that (1 1 1) and (1 1 2) poles aligned with the growth direction. Finally, in some other areas, (1 1 2) or (0 1 1) poles of the CZT matrix aligned with the growth direction. New relationships between the CZT matrix and large Te polycrystalline particles were revealed: {1 1 2 - } CZT ΙΙ{1 1 - 0 0} Te and {0 0 1} CZT II{0 1 - 1 - 1} Te .

58 GEOSCIENCES↗

Survey of the mechanical and physical behaviors of yttria-stabilized zirconia from multiple dental laboratories

Background: When selecting zirconia for a dental restoration, laboratory prescriptions often refer to high strength and high translucency. In this survey, zirconia specimens were ordered from various dental laboratories for posterior (high strength) and anterior (high translucency) clinical indications. The specimens were then tested and evaluated for their mechanical and physical behaviors. Methods: In a double-blinded manner, 9 laboratories provided 32 specimens from 17 different zirconia blanks, which were tested in the American Dental Association laboratory. Flexural strength tests were performed on standard specimens, and fracture surfaces were examined using both optical and scanning electron microscopy. Chemical composition, Vickers hardness, and absolute transmittance measurements were also performed. Results: A large scatter in the strength values was observed. The zirconia intended for posterior applications displayed strengths (SD) from 195 through 783 MPa (490 [183] MPa), which overlapped greatly with the strengths (SD) of the zirconia intended for anterior applications, 320 through 768 MPa (581 [136] MPa). However, when the strength values were recalculated on the basis of yttria content, the strengths (SD) were 584 (158) MPa for 3 mol% yttria and 373 (104) MPa for 5 mol% yttria. Conclusions: When a prescription was given to dental laboratories to request zirconia on the basis of clinical requirements, there was a large scatter and no consistency in the resulting strength values partly because of mixed use of 3 mol% and 5 mol% yttria zirconia. The 3 mol% materials had much higher strength when the strength values were grouped according to yttria content. Strength was also highly dependent on processing and finishing at the dental laboratories.

3 mol% yttria-tetragonal zirconia polycrystal (3Y-↗

Leak-tight crack repair for 304L stainless steel using friction surfacing

Here, friction surfacing (FS) was investigated as a method for sealing 50 μm wide thru-cracks in 3-mm-thick 304L stainless steel (304L) plate. Friction surfacing was performed using two sizes of 304L consumable rod, with diameters of 9.52 mm and 12.7 mm, on two substrate conditions (clean and oxidized). Friction surfacing was able to deposit a 600 μm thick coating and repair cracks to a depth of 100 μm - 200 μm below the original surface, when using the 12.7-mm-diameter consumable rod for both substrate conditions. Helium leak rates of 10 -10 atm-cc/s were achieved on crack repairs, designating them as leak-tight by the ANSI N14.5 standard. Optical and scanning electron microscopy were used to investigate the coating microstructure and bond interfaces. In this study, the 12.7-mm-diameter rod performed better with disruption of the oxide layer on the oxidized substrate and providing a more homogenous coating. Mechanical properties of the coated samples were evaluated by performing micro-indentation, tensile, bending, and adhesion testing. Higher hardness in the coatings was observed due to the fine equiaxed grains resulting from dynamic recrystallization. Complete consolidation of plastically deformed material on the substrate and a strong diffusion bond across the interface was observed. This was reflected in tensile and bending properties of the FS coatings being comparable to those of uncoated specimen. No delamination of the FS coating was observed during adhesion testing. The results demonstrate that friction surfacing is a viable option to seal cracks in stainless steels.

36 MATERIALS SCIENCE↗

Parameter development and characterization of laser powder directed energy deposition of Nb – Alloy C103 for thin wall geometries

This work focuses on the parameter development and microstructural characterization of Nb-based alloy C103 for thin wall structures produced via laser powder – directed energy deposition (LP – DED). Laser power and scanning speeds were varied as part of a design of experiments to identify adequate print parameters. Combinations were evaluated for relative density, porosity, and geometrical accuracy. A combination of a laser power of 1420 W and scanning speed of 14 mm/s resulted in a relative density >99%, exhibited a consistent weld bead profile and was used for further microstructural evaluation. A mix of optical and scanning electron microscopy (SEM) revealed small, slightly elongated grains along the edges and large epitaxial grains in the central region along the Build – Transverse view. Scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) analysis revealed Hf rich columnar cells in the center that transition into an evenly spaced cellular structure towards the edges of the built sample. Electron backscatter diffraction (EBSD) scans show a sharp [001] texture when looking at the cross section of the sample along the build direction. The Build – Scan view revealed a zig – zag pattern that follows the back – and – forth deposition strategy that was used. Finally, microhardness measurements were taken in the as – built (AB) and stress relieved (SR) conditions to baseline preliminary mechanical properties. The AB condition exhibited a large amount of scatter in the data and averages up to 11% larger than the SR condition. The reduction in scatter upon applying the SR cycle are indicative of a large concertation of dislocations present in the AB condition.

36 MATERIALS SCIENCE↗

Investigation of constituent redistribution in U-Pu-Zr fuels and its dependence on varying Zr content

This contribution investigates fuel constituent segregation and fuel-cladding chemical interactions (FCCI) in three U-Pu-Zr fuel pins irradiated to ~11% burnup in Experimental Breeder Reactor-II as part of the X441 DP-1 experiment. In examined pins, Zr content ranged from 6 to 10 and 14 wt.%, while Pu concentration was constant at 19 wt.% Pu. The primary goal of the investigation was to determine the role Zr content plays in fuel performance and this manuscript provides assessment of both constituent redistribution and FCCI as a function of axial position. FCCI was observed in all pins, though no cladding failure was noted. Optical and scanning electron microscopy (SEM) results show that variation in Zr content alters the number and relative size of constituent redistribution zones in the fuel. For example, larger Zr-rich central regions and smaller U-rich intermediate regions were observed in 14 wt.% Zr fuels. More importantly, all examined fuels have four or more discrete constituent redistribution regions, where each region has dissimilar morphological features. The existence of four to six distinctive regions deviates from traditionally accepted three region redistribution model, highlights complexity of constituent redistribution in this metal fuel, and identifies the need to conduct additional studies using state-of-the-art instrumentation.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Laser repair welding of irradiated alloy 182

Welding repair of irradiated nickel-based alloys, such as Alloy 182, poses a significant challenge due to helium-induced cracking (HeIC) and grain boundary degradation (GBD) in the heat affected zone, driven by helium accumulation at grain boundaries and welding-induced tensile stresses. This study investigates the weldability of irradiated Alloy 182 up to 15 wppm doped boron using both conventional laser welding and the Auxiliary Beam Stress Improved (ABSI) laser welding technique. While HeIC was observed at the weld toe of the entry pass in both methods due to the higher effective heat input associated with the initial pass directly on the base metal, no additional cracking occurred elsewhere, even at elevated helium concentrations. Optical and scanning electron microscopy analysis revealed that the ABSI technique, which introduces additional compressive stresses to counteract solidification-induced tensile stresses, significantly reduced GBD formation, lowering its total count from 1,230 to 339 and decreasing both average and maximum GBD lengths. In conclusion, these results demonstrate that the ABSI technique is a promising approach to mitigate helium-induced damage and improve the weldability of irradiated Alloy 182, offering a viable solution for structural repairs for long-term operation of existing nuclear reactors.

grain boundary degradation↗

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