Microstructures and properties of Ti/TiC composites fabricated by laser-directed energy deposition
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The fast loss of fluidity of sodium silicate-activated slag (SS-AAS) systems have been widely studied in the literature. In this study, the rheology of these cements has been correlated with the evolution of the reaction products formed over time. For this purpose, a combination of experimental characterization techniques, to study the pore solution composition and microstructure of SS-AAS pastes and thermodynamic calculations have been applied. The initial precipitation of ill-defined N-A-S-H and C-N-A-S-H producta leads to a fast increase of the storage modulus after 40 min of reaction. These products are formed from the reaction of the Na{sup +} ions and silicate ions of the activator with the Ca{sup 2+} and aluminate species dissolved from the slag. However, when a shear is applied, the structure breaks down and fluidity is recovered, that infers that the attractive forces between the particles are low at the early stages of hydration.
INCONEL® alloy 740H® is an age-hardenable nickel-based alloy approved for pressure vessels and piping within ASME Section I, VIII, and B31.1. Currently, the code applies a weld strength reduction factor (WSRF) of 0.7 to the allowable stresses for longitudinal seam welds in the time dependent creep regime. In this work, a full-scale seam weld was successfully produced using typical industrial practices. The component was solution heat-treated and aged after fabrication to improve the performance of the weldment. Tensile, bend, impact, and low-cycle fatigue tests showed the component met all the specification requirements and elevated temperature properties were within base metal expectations with failures predominately in the weld metal. Long-term creep tests, including large samples more representative of the entire weldment, were fabricated and tested to times in excess of 10,000 h at multiple temperatures. Analysis of the creep data supports a WSRF of 0.9 for the solution annealed + aged weldments in contrast to the WSRF of 0.7 currently applied to welded + aged weldments. Metallurgical analysis shows that the solution annealing causes recrystallization of the weld metal and reduces the chemical compositional and microstructural gradients in the weldments resulting in acceptable short-term performance. In long-term creep, evidence for coarsened zones in the weldments due to discontinuous coarsening reactions were identified as the mechanism leading to accelerated creep damage formation in the weld metal and sample failure.
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High-entropy alloys (HEAs) fabricated by powder metallurgy are considered to exhibit extremely-great potential application values in the field for high-speed impact deformation due to their uniform microstructures and compositions. The mechanical behavior of a powder-metallurgy-fabricated (PM) CoCrFeMnNi HEA was investigated at room temperature with strain rates ranging from 1200 s -1 to 2800 s -1 . It was found that the serration behavior and shear localization of the alloy under dynamic conditions occurred. Results also indicated that the serrated flow took place in the PM CoCrFeMnNi HEA during mechanical deformation at high strain rates (>1000 s -1 ) and became more pronounced as the strain rate increased. Furthermore, it was determined that the yield-strength values of the PM CoCrFeMnNi HEA were sensitive to strain rates, where the values increased from 500 MPa to 700 MPa when the strain rates increased from 1200 s -1 to 2800 s -1 . Shear bands with a width of about 20 μm were generated in the PM CoCrFeMnNi HEA after the shear stress reached a maximum value of 635 MPa, which corresponded to a nominal strain of about 8.71. Nanotwins and ultrafine-equiaxed grains with a diameter of about 150 nm also developed at the core of the shear band during deformation. The results revealed that the strength of the shear band was much higher than that of the matrix grain. Nanotwins in the shear band were composed of a single face-centered-cubic (FCC) structure with the twin plane of ($\bar{1}$1$\bar1$), which could be formed via a rotational dynamic recrystallization (RDR).
Coating the surface of Zircaloy-4 light water reactor fuel cladding tube is of considerable interest for enhancing its accident tolerance. In this study, thermal annealing of FeCrAl-coated Zircaloy-4 at 725 °C for 500 h, was used to induce interfacial reactions between Zircaloy-4 and FeCrAl. The interface zones were then irradiated by 3.5 MeV Zr ions at 400 °C, up to 50, 100, 150 peak dpa values. Transmission electron microscopy (TEM) and scanning TEM were used to characterize microstructural and composition changes before and after ion irradiation. Three interfacial phases were identified: FeZr 3 , (Fe,Cr) 2 Zr, and ZrC. The widest intermetallic layer, FeZr3, had large grains. The narrower phases, (Fe,Cr)2Zr and ZrC, contained small grains and were often mixed. The unexpected observation of the ZrC phase was attributed to the presence of very small impurity level concentrations of carbon in the powder material. No void swelling was observed in any of the phases, including the FeCrAl coating and Zircaloy-4 substrate. (Fe,Cr) 2 Zr, however, fully amorphized after irradiation, even at the lowest dpa.
Ferritic iron-chromium-aluminum (FeCrAl) alloys with varying Cr content were subjected to in-situ irradiation-corrosion with energetic protons or electron beams in pure water with various oxygen concentrations. Oxide microstructure and composition were characterized to compare the corrosion under irradiation with the thermal corrosion in the same water conditions. The dominant effect seems to be the production of H 2 O 2 at the surface by the intense proton and electron beams. The corrosion potential of FeCrAl under BWR-NWC condition is somewhat above the Cr 2 O 3 /CrO 4 2- phase boundary, oxidizing the Cr(III) to Cr(VI) in the outer part of the film, but with some Cr(III) remaining in the interior of the oxide. The beam increases the corrosion potential, significantly reducing Cr(III) content throughout the oxide. Finally, the crystallites on the surface, which form by re-precipitation from solution, do not contain Cr because at low potential Cr(III) is not soluble, and at high potential Cr(VI) is quite soluble.
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An experimentally validated mesoscale model was developed to simulate the effective thermal conductivity (ETC) of metallic U and U–Zr nuclear fuels. The effects of microstructure, temperature, composition, and interfacial thermal resistance (ITR) were investigated. Companion experiments were conducted to validate the model. The numerical simulations clearly demonstrate that accounting for the interface (Kapitza) thermal resistance and Zr precipitation is necessary to improve the model predictions. The dependence of the effective Kapitza resistance of depleted-U and U-10Zr on temperature was determined. Finally, for both materials, the largest difference between the model calculations and the experimental data was about 4.5%, which is within the precision of the experimental measurements.
Here, this study reports on the microstructural and compositional evolutions, deuterium release and lithium loss behavior in lithium silicates. Pellets of biphasic Li 4 SiO 4 and Li 2 SiO 3 were fabricated using hot pressing of powders. Sequential irradiation with Si + , He + and D + ions was performed up to 773 K to emulate one-year 6 Li burnup in 6 Li 4 SiO 4 inside the SlimCS DEMO. Crystalline Li 4 SiO 4 phase was not observed in the irradiated depth region of all the samples in this study. In spite of full amorphization in the near-surface region, Li 2 SiO 3 irradiated to a high dose at 773 K remained crystalline in the damage peak region, suggesting that Li 2 SiO 3 is more irradiation resistant to amorphization than Li 4 SiO 4 . Radiolysis may be primarily responsible for silicate decomposition and amorphization. Data from this study also show that D release from the pellet is very efficient during ion irradiation at 773 K, which is accompanied with a significant Li loss. Thermal annealing for 10 min at 773 K for the room-temperature irradiated pellet leads to a nearly complete D release without an observable Li loss. A concept of Ni coating on tritium breeder materials is discussed with supporting data to minimize Li loss without a significant impact on tritium diffusion and release.
A comparative study was conducted to evaluate the corrosion susceptibility of 316L, 316H, Ni 200, Inconel 625, and Hastelloy N in molten FLiNaK at 700 °C for 100 h. Top-view and cross-sectional scanning electron microscopy (SEM) imaging, combined with energy-dispersive X-ray spectroscopy (EDS) mapping, was performed to investigate microstructural and compositional changes. SEM images were further processed by introducing a contrast threshold to map cavity distribution. Using EDS mapping, intergranular and intragranular Cr loss were separately characterized. The ranking of mass loss after corrosion, from highest to lowest, is as follows: 316H > 316L > Inconel 625 > Hastelloy N > Ni 200. Cr loss was found to be correlated with Mo concentration, in agreement with many previous studies, with higher Mo content resulting in reduced Cr loss. On the other hand, there is no evidence that the high carbon content in 316H enhances corrosion resistance. The relatively low solubility of carbon in austenite at the testing temperature limits the amount of dissolved carbon. Therefore, the carbon-retarded vacancy diffusion, and consequently the reduced Cr diffusion, were not observed.
Two technologies, friction surfacing (FS) and cold spray deposition (CSD), have been investigated for field repair of cracks in 304L austenitic stainless steel. Both technologies are low-heat-input, solid-state technologies that do not introduce the detrimental effects of solidification, such as compositionally segregated microstructures and shrinkage stresses. Friction surfacing was performed using a 304L stainless steel rod over the substrate of the same material. Further, the process was performed at a high spindle speed of 20,000 RPM allowing for process forces below 500N to be used effectively. Spherical gas-atomized 304L stainless steel powder, in size range of 25–44 µm, was used as feedstock powder for the cold spray process for deposition on 304L substrates. Both technologies showed leak-tight crack repair capabilities on ~30–50 µm wide simulated through-crack specimens based on helium leak tests.
High surface area nanostructured electrodes are essential for understanding charge storage mechanisms in high capacitance supercapacitors. Additionally, a growing number of studies provide credible evidence that the highest capacitance in carbon nanomaterials is attainable only when the pore size is in micropore range. In this study therefore, micropore-dominatedcarbon materials derived from Parinari curatellifolia (PC) waste seeds are prepared via pyrolysis and subsequent chemical activation with KOH. SEM, EDAX, TEM, Raman, and XRD studies show that the microstructure and composition of the as-prepared microporous carbon materials are influenced by adjusting the KOH to carbon mass ratio. Sorption studies demonstrate a very high BET surface area of 1898 m 2 g –1 , type I isotherm, and 99% micropore content in all the samples. The BET surface area, S micro , V micro , and total volume increased with increasing KOH content during activation. The fabricated electrodes exhibit high specific capacitances of 423 F g –1 at 5 mV s –1 and cyclic stability of 98% after 50000 cycles both of which are indicative of our carbon materials huge potential in making high performance supercapacitors. The specific capacitance increased with the micropore content in the samples signifying that the pores enhanced diffusion and hence the charge storage. The PC carbon materials deliver high specific capacitance due to the enhancement of diffusion and charge storage stemming from the synergetic interplay of the aforementioned textural parameters. As a result, the PC carbon materials therefore provide good prospects for supercapacitor applications.
This study exposed novel fine-grain dispersion-strengthened tungsten (W) to high fluence, low energy deuterium (D) and helium (He) plasmas to evaluate how material microstructure and composition affect hydrogen retention and surface morphology. Tested materials included fine-grain dispersion-strengthened tungsten (DSW) with 3 wt% zirconium carbide (ZrC) dispersoids, fine-grain dense W without any dispersoids (FGW), and coarse-grained polycrystalline ‘ITER-grade’ W. Samples were exposed to D 2 + and He + plasmas at fusion-relevant fluences (∼10 25 m -2 ) and ion energies (75 eV) over a range of temperatures (200 °C, 300 °C, 450 °C for D, 850 °C for He). Helium ion microscopy was performed on the exposed samples to evaluate surface morphology changes and material integrity. After D plasma exposure, the ZrC dispersoids showed near-surface degradation at exposure temperatures above 300 °C, but no detrimental morphology changes were observed for the adjacent W grains. After He plasma-exposure, nano-structured fuzz formation was observed in the tungsten matrix of all samples. The ZrC dispersoids maintained their integrity despite the surrounding fuzz growth, with clear delineation between the W fuzz and dispersoid regions. Thermal desorption spectroscopy showed that ZrC DSW consistently retained more D than the FGW by about a factor of 2 across all temperatures. At 200 °C and 300 °C, the ITER-W displayed lower D retention than both the DSW and FGW, however at 450 °C ITER-W showed the highest retention, about 50% more than DSW. He retention was comparable across all samples, with the highest retention observed in the fine-grain W, only 26% higher than in ITER-W. These insights on retention behavior will inform further optimization of these novel fine-grained tungsten materials with and without dispersoid additives.
In-situ formation of ZrB 2 –SiC composites was investigated by reactive spark plasma sintering of precursor powders according to the reaction B4C + 2ZrC + 3Si → 3SiC + 2ZrB 2 . The reaction and process presented here involves a diffusion reaction between B4C and ZrC which facilitates the formation of ZrB 2 , while liquid phase sintering of silicon facilitates atomic diffusion and combines with free C from the B4C and ZrC reaction to form SiC within minutes of heating and there were some residual unreacted precursor materials. An interpenetrating matrix of ZrB 2 –SiC was formed that shows increased fracture toughness (6.03 ± 0.45 MPa m 1/2 ) despite relatively low density (95 %).
Silicon oxycarbide (SiOC) is a versatile ceramic material with tunable microstructure and compositions that can be modulated through precursor chemistry and processing conditions. Though there are several noteworthy uses of SiOC across a range of application spaces, the difficulties in elucidating the short- to medium-range order within these materials have limited the maturation of strategies to precisely control SiC x O 4–x compositions for user-tailored applications. In this contribution, we implement a range of synchrotron scattering and spectroscopy methods coupled with stochastic modeling techniques to elucidate changes in local chemistry and structure associated with the pyrolysis of a commercially available SiOC polymer precursor. Stochastic modeling approaches provide valuable insights into decoupling local Si–O and Si–C environments while confirming predominate heterogeneous phases in materials. Using pyrolysis temperatures between 250 to 800 °C results in a heterogeneous material predominately composed of SiOC and amorphous SiO 2 domains. At 1100 °C, redistribution of Si–C pairs in the SiOC network and Si–O from the SiO 2 domains create a more ordered SiOC phase with local cubic SiC-like ordering. In addition, residual carbon leads to a detectable carbon phases at 1100 °C that persist at higher temperatures. These efforts address the difficulties of obtaining atomic-scale insights into the local structure and nanoscale heterogeneities in SiOC, providing pathways toward establishing structure–property relationships for future materials development.
Abstract Geothermal energy plays a vital role in decarbonizing electricity and heat supply. Effective utilization of geothermal resources hinges on identifying or generating permeable reservoir zones and understanding how effective pressure variations affect fluid circulation and reservoir properties by poroelastic deformation. Hydrothermal alteration can modify the petrophysical properties of geothermal reservoir rocks, which may increase or decrease its productivity. Understanding these alteration effects is essential to predict and optimize long‐term sustainable geothermal operations. Here, we investigate the impact of hydrothermal alteration on poroelastic and hydraulic properties of diverse lithologies in a series of deformation tests performed at several confining (0–80 MPa) and pore pressure (10–30 MPa) levels. Experimental results of hydrothermally altered dikes and phyllites obtained from the Blue Mountain geothermal field (Nevada, USA) are compared to thermally cracked La Peyratte granite (France) and correlated with petrophysical properties, mineral composition, and microstructures. Argillic alteration of dikes increases porosity and storage capacity but lowers thermal conductivity and increases pore compressibility. Conversely, silicate precipitation in phyllites increases stiffness and thermal conductivity but also reduces porosity and permeability. Experimentally determined effective pressure coefficients range from 0.1 to 0.9, differ for permeability and volumetric strain and decrease with increasing effective pressure. The presence of compliant microcracks and crack‐like pores significantly increases the stress sensitivity of La Peyratte granite and silicified phyllites. This study demonstrates how thermal and chemical alteration impacts poromechanical and petrophysical characteristics of geothermal targets, which ultimately govern reservoir stability and subsidence, induced seismicity as well as fluid and heat extraction efficiency during geothermal operations.
The ability of thermoelectric (TE) materials to convert thermal energy to electricity and vice versa highlights them as a promising candidate for sustainable energy applications. Despite considerable increases in the figure of merit zT of thermoelectric materials in the past two decades, there is still a prominent need to develop scalable synthesis and flexible manufacturing processes to convert high-efficiency materials into high-performance devices. Scalable printing techniques provide a versatile solution to not only fabricate both inorganic and organic TE materials with fine control over the compositions and microstructures, but also manufacture thermoelectric devices with optimized geometric and structural designs that lead to improved efficiency and system-level performances. In this review, we aim to provide a comprehensive framework of printing thermoelectric materials and devices by including recent breakthroughs and relevant discussions on TE materials chemistry, ink formulation, flexible or conformable device design, and processing strategies, with an emphasis on additive manufacturing techniques. Additionally, we review recent innovations in the flexible, conformal, and stretchable device architectures and highlight state-of-the-art applications of these TE devices in energy harvesting and thermal management. Perspectives of emerging research opportunities and future directions are also discussed. While this review centers on thermoelectrics, the fundamental ink chemistry and printing processes possess the potential for applications to a broad range of energy, thermal and electronic devices.