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At least 1,135 records · Page 63

Characterization of compositional variation and solidification condition on rapid solidification behavior of beta stabilized titanium

Rapid solidification (RS) is a field of study that has increased in importance due to the rise of additive manufacturing (AM) techniques. The breakdown of equilibrium at the solid-liquid interface results in an inability to use traditional solidification models that have been applied to great success in casting. As such, there is a current need for a high-throughput testing method to screen alloys at rapid solidification conditions without the significant cost for powder atomization. In this work, twin hammer splat quenching (SQ) is utilized and theoretically developed as a technique uniquely placed to test alloy systems for AM applications. Using analytical thermal spray models and numerical heat transfer simulations, the cooling rate and solidification conditions of splat quenching are compared across several parameters to evaluate the key parameters for generating cooling rates relevant to AM process. Once a framework for the cooling rates and relevancy of SQ are developed, SQ was used to process alloy compositions in the Ti5553 alloy space (AMS 7026) to study the formation of detrimental secondary phases occurring upon rapid quenching from the melt. A martensitic phase is found to occur at the lower end of the standard, but the composition listed in the standard were found to be safe. Finally, the rapid solidification behavior of Ti-5553 is evaluated by comparing splat quenching, laser welding, and plasma atomization that offer a wide window of solidification conditions. The segregation and solidification structure are analyzed and compared to models to provide a deeper understanding of the solidification behavior of beta stabilized titanium alloys.

Williamson, Christopher J.↗

Investigation of the Effect of Foaming Agent on the Fabrication of NiTi Foams Using the Self-Propagating, High-Temperature Synthesis Process

Fabrication of NiTi intermetallic foams using the self-propagating, high-temperature synthesis (SHS) process was investigated. Weighed amounts of powders taken from an equimolar mixture of Ni and Ti powders along with 0.5, 1, and 1.5 wt pct of different foaming agents were cold pressed to form cylindrical compacts 10 mm in diameter, 20 mm in height, and 7 to 8 g in weight. A novel, induction-assisted ignition method was used for indirect heating and igniting the compressed mixtures at one end. As a result of intensive exothermic reaction between Ni and Ti and decomposition of foaming agents and liberation of gases, highly porous products were obtained. Characterization of the products was carried out using X-ray diffraction (XRD) and a scanning electron microscope equipped with an energy-dispersive spectroscope (SEM-EDS). The main phase in the products was detected to be B2(NiTi) with minor amounts of NiTi{sub 2} as the secondary phase. Other undesirable phases, such as Ni{sub 4}Ti{sub 3} and Ni{sub 3}Ti, were not detected. The effect of type and percentage of foaming agent on the formation and distribution of pores within the products was studied. Final products with porosities up to ~ 80 vol pct were obtained by adding foaming agent. Under the conditions of this study, CaH{sub 2} proved to be the most effective foaming agent considering its ability to generate a uniform distribution of pores, while TiH{sub 2} was not considered favorable due to its decomposition at relatively low temperatures. In general, the addition of foaming agents in amounts higher than 1wt pct is not recommended; due to the endothermic nature of thermal decomposition reactions of foaming agents, excessive use of these agents can result in suppression of the exothermic reaction.

36 MATERIALS SCIENCE↗

The role of microstructural evolution during spark plasma sintering on the soft magnetic and electronic properties of a CoFe–Al2O3 soft magnetic composite

Abstract For transformers and inductors to meet the world’s growing demand for electrical power, more efficient soft magnetic materials with high saturation magnetic polarization and high electrical resistivity are needed. This work aimed at the development of a soft magnetic composite synthesized via spark plasma sintering with both high saturation magnetic polarization and high electrical resistivity for efficient soft magnetic cores. CoFe powder particles coated with an insulating layer of Al 2 O 3 were used as feedstock material to improve the electrical resistivity while retaining high saturation magnetic polarization. By maintaining a continuous non-magnetic Al 2 O 3 phase throughout the material, both a high saturation magnetic polarization, above 1.5 T, and high electrical resistivity, above 100 μΩ·m, were achieved. Through microstructural characterization of samples consolidated at various temperatures, the role of microstructural evolution on the magnetic and electronic properties of the composite was elucidated. Upon consolidation at relatively high temperature, the CoFe was to found plastically deform and flow into the Al 2 O 3 phase at the particle boundaries and this phenomenon was attributed to low resistivity in the composite. In contrast, at lower consolidation temperatures, perforation of the Al 2 O 3 phase was not observed and a high electrical resistivity was achieved, while maintaining a high magnetic polarization, ideal for more efficient soft magnetic materials for transformers and inductors.

36 MATERIALS SCIENCE↗

Manufacturing of Thermoset Polyimide Composites by Laser Sintering

Selective Laser Sintering (SLS) is an additive manufacturing technique that builds 3D models layer by layer using a laser to selectively melt cross sections in powdered polymeric materials, following sequential slices of the computer-aided design (CAD) model. SLS generally uses thermoplastic polymeric powders such as polyamides. The resultant 3D-printed objects are often weaker in their strength compared to traditionally processed materials, due to their higher porosity. This paper described the process development of using melt-processable imide oligomers terminated with reactive 4-phenylethynylphthalic anhydride (4-PEPA) to conduct laser sintering (LS). The first successful 3D-printing of high temperature RTM370 thermoset polyimide carbon fiber composites were further post-cured to promote additional crosslinking for achieving higher temperature (T g = 370°C) capability. Another novel imide oligomer, RTM385-SLS, formulated with a complex melt viscosity [ƞ*] of ~104-105 poise is also suitable for LS. RTM385-SLS resin powder was mixed with 20-25% of hexagonal boron nitride (h-BN) and subjected to LS to print out “Green” specimens which could be further post-cured to afford a thermally conductive but electrically insulating composites with high T g of 385 °C. The cured composite specimens were then subjected to mechanical testing, thermal conductivity and porosity measurements as well as SEM characterization.

additive Manufacturing↗

CHARACTERIZATION OF FATIGUE BEHAVIORS OF NOTCHED 316L DED AM SPECIMENS

ASME Codification of Additive Manufacturing • Integration of AM into ASME Codes and Standards • The ASME goal is to have AM requirements in ASME Code Cases preceding the 2025 Edition. • The ASME Special Committee on AM has drafted criteria for two Code Cases for Additive Manufacturing. • AM Construction of Pressure Equipment using the Direct Energy Deposition Process with Wire Feedstock. • Includes Gas Metal Arc Welding. • Time-independent material properties. • Status - Criteria endorsed by AM Committee. • AM Construction of Pressure Equipment using the Powder Bed Fusion AM Process. • Includes Laser and Electron Beam Energy Sources. • Austenitic and Nonferrous materials. • Time-independent material properties. • Status – Approval ballot circulating to the AM Committee.

Krentz, Timothy M.↗

Wyoming CarbonSAFE: Advancing Commercialization of Low-Carbon Energy Technologies in Fossil-Rich Wyoming

Wyoming’s Powder River Basin (PRB) is the most prolific coal producer and exporter in the United States and the State of Wyoming’s largest oil-producing basin. In addition to being a leading energy producer, the PRB is the site of research programs whose aim is to develop and integrate low-carbon technologies into existing fossil fuel energy industries. Much of the PRB’s low-carbon research is focused around Dry Fork Station (DFS), which is the newest coal-fired power station in the western US. Currently, DFS hosts five carbon capture projects, including pilot-scale capture projects that utilize different capture technologies and a full front-end engineering and design (FEED) study, a commercial CO 2 pipeline for nearby CO 2 -enhanced oil recovery industry, and is also co-located with the Wyoming Integrated Test Center, which is a host facility for unconventional carbon utilization research (i.e. flue gas carbon-to-products innovations). DFS is also the host site for the Wyoming CarbonSAFE project. Wyoming CarbonSAFE, funded by the Department of Energy/National Energy Technology Laboratory, is a multi-phased program (currently in Phase II) whose core objective is developing and validating storage sites within a complex capable of storing 50 million metric tonnes of CO 2 over a 30 year project period using carbon capture, utilization and storage (CCUS). This paper will provide an overview of the project to-date, showing that CarbonSAFE goals are achievable with respect to geologic, environmental, regulatory, CO 2 source and economic conditions, and why the State of Wyoming offers one of the more favorable environments to advance the commercialization studies. In 2019, the project team designed and completed a ~10,000 foot stratigraphic test well just south of DFS. From this well, the team collected over 600 feet of core, fluid samples from target injection zones, and a full petrophysical log suite. In addition, legacy 2D seismic lines were acquired and a 3D seismic survey was acquired in the fall of 2020. The objective of these field activities has been to identify and characterize target storage reservoirs and associated caprock. This complex has several reservoirs that could meet commercial injection goals, and over 4000 feet of associated caprock. Simulations of site performance suggest that stacked injection provides the most effective storage strategy, and would necessitate several sites within the greater complex to meet final project injection goals. Other work within this project includes the development of a business-case around proximal fields with CO 2 -enhanced oil recovery potential and existing tax credits, assessment of regulatory conditions, including pore space ownership and Class VI injection well permitting requirements, implementation of a robust public outreach Electronic copy available at: https://ssrn.com/abstract=3821220 GHGT-15 McLaughlin 2 program, and surface site characterization activities that have focused on environmental factors. In the PRB and at DFS, the State of Wyoming and other entities have made carbon management a priority of its future energy industry by providing a regulatory and business framework that is favorable to advancing these technologies. These endeavors will become more realistic with the successful implementation of Wyoming CarbonSAFE, and its ability to secure and validate commercial-scale CCUS at the center of Wyoming’s premier low-carbon research efforts.

McLaughlin, Fred↗

Assessing Manufacturability of the Oxide Dispersion Strengthened (ODS) 14YWT Alloy Fuel Cladding Tube Using SolidStir™ Technology

The 14YWT (Fe–14Cr–3W–0.4Ti–0.3Y2O3 (wt.%)) alloy is a potential candidatematerial for fabricating fuel cladding tubes and other structural components to be used in next-generation advanced nuclear reactors. Due to inherent limitations of current processing routes, this research explored a new variant of friction stir processing, commercially referred to as SolidStir™ Extrusion (patent pending) technology from Enabled Engineering to consolidate and extrude 14YWT powder into a fuel cladding tube. Several single-layer and multiple-layer consolidation experiments were carried out in an Inconel 625 die to determine the suitable processing parameters for SolidStir™ extrusion of the 14YWT alloy cladding tube. With these processing parameters, a 16–18 mm long tube of the 14YWT alloy with no visible defects was successfully extruded using this novel technology. Microstructural characterization results obtained using optical microscopy, scanning electron microscopy, energy dispersive spectroscopy, electron backscatter diffraction, and transmission electron microscopy will be presented.

Advanced Materials and Manufacturing Technology↗

Repairing High γ’ Hot Section Gas Turbine Components Using Advanced Manufacturing

This article describes the ability to use laser-blown powder deposition to repair high γ' IN-100 superalloy gas turbine components. The influence of various process conditions on the ability to make crack-free IN-100 deposits over surrogate high γ' alloys was investigated to identify cracking mechanisms in the deposit and heat-affected zones (HAZs). The various crack formation mechanisms, such as solidification cracking and liquation cracking, were evaluated using multiscale characterization and numerical simulation. The cracking in the deposit region was predominantly solidification cracking, while those observed in the HAZ were liquation cracking. The results showed that controlling thermally induced residual stresses is the key to eliminating cracking, and the optimum preheat temperature was determined. In conclusion, the results were then contrasted with those in published literature and an approach to effectively repair hot section parts was presented.

36 MATERIALS SCIENCE↗

Laser Sintering of Thermoset Polyimide Composites

Selective Laser Sintering (SLS) is an additive manufacturing technique that builds 3D models layer by layer using a laser to selectively melt cross sections in powdered polymeric materials, following sequential slices of the CAD model. SLS generally uses thermoplastic polymeric powders, such as polyamides (i.e. Nylon), and the resultant 3D objects are often weaker in their strength compared to traditionally processed materials, due to the lack of polymer inter-chain connection in the z-direction. Our previous effort showed the challenges of printing a melt-processable RTM370 imide resin powder terminated with reactive 4-phenylethynylphthalic anhydride by LS, due to its inherently low viscosity of these oligomers. This paper presented the first successful 3D printing of high temperature carbon fiber filled thermoset polyimide composites, followed by post cure cycles to promote additional crosslinking for achieving higher temperature (Tg = 370 °C) capability. The processes to build tensile specimens and a component by LS, and the characterization of RTM370 imide resin by DSC and rheology as well as evaluation of the LS printed polyimide composite specimens by SEM and mechanical tests will be discussed.

Polyimide Composites↗

Role of scan strategies and heat treatment on grain structure evolution in Fe-Si soft magnetic alloys made by laser-powder bed fusion

A major goal in printing soft magnetic Fe-Si steels using additive manufacturing is to take advantage of the potential for complex geometric designs and site-specific grain control. One major step in the processing of these alloys is understanding how processing parameters might impact how the as-built microstructure responds to annealing (i.e. the annealing response). The impact of scan strategy on the annealing response for thin wall geometries is specifically explored. Two scan strategies were explored for a thin wall geometry that produced a strongly columnar grain structure and equiaxed grain structure. Additionally, samples from both scan strategies annealed at 1200 °C showed a marked difference in annealing response with the more equiaxed sample seeing full recrystallization and grain growth, while the more columnar grain structure saw little change in microstructure. After analysis through characterization techniques and thermal-mechanical simulations Differences in internal energy within the grains were ruled out because calculated GND density values were similar for both samples. The formation of secondary particles was ruled out as a contributing factor due to the type of oxide formations and their size. It was concluded that the contributing factor to the difference in the annealing response were a difference in the resulting grain size and the density of high angle grain boundaries. These two differences were largely attributed to differences in the thermal gradient conditions due to grains preferentially growing in the direction of the steepest thermal gradient.

36 MATERIALS SCIENCE↗

Spark plasma sintered, MoNbTi-based multi-principal element alloys with Cr, V, and Zr

MoNbTi, MoNbTiZr, CrMoNbTiZr, and MoNbTiVZr multi-principal element alloys (MPEAs) were fabricated via spark plasma sintering (SPS) and investigated for use in high-strength applications. The fabrication method by SPS and powder metallurgy differs from those presented in the prior literature, where most MPEAs are fabricated using arc melting (AM) methods. Here cryogenic milling was used to maximize potential defect sinks (grain boundaries) for radiation resistance and to increase ultimate tensile strength through the Hall-Petch effect. SPS was chosen for consolidation in order to maintain a fine-grained structure during densification. Each alloy was characterized using x-ray diffraction and scanning electron microscopy for phase identification and compositional homogeneity. The base ternary alloy MoNbTi presented a predominantly single BCC system with minor cubic phases. The introduction of additional alloying elements—Zr, V, and Cr—heightened the phase complexity and increased the fractions of a secondary BCC phase and an HCP phase from Zr. The addition of Cr induced a larger fraction of the Laves phase to form. The addition of V caused the precipitation of small Mo inclusions. Thermodynamic analysis was performed to understand the separation of phases in each alloy. Discrepancies among the phase predictions generated by thermodynamic models, phases previously presented in the literature, and the characterization results suggest that MPEA fabrication methods, especially solid-state methods, require significant investigation to ensure that alloys can remain stable throughout their anticipated service lifetimes.

36 MATERIALS SCIENCE↗

$In-situ$ synchrotron x-ray diffraction and thermal expansion of TiB2 up to ~3050 °C

There is an increasing interest in understanding the performance and properties of ultra-high temperature ceramics due to their high melting points (<3000 °C) that make them promising for extreme environment applications. In-situ high temperature X-ray diffraction experiments were performed on TiB 2 beads up to ~3050 °C. For these experiments, TiB 2 powders were fabricated into spherical beads via gel casting methods and densified in a high temperature graphite furnace. These sample beads were then levitated in a conical nozzle levitator with reducing atmosphere (3% H 2 -Ar) while being heated using a 400 W CO 2 laser. During levitation a collimated synchrotron X-ray source was used to perform in-situ, temperature-dependent structural characterizations. The anisotropic coefficients of thermal expansion of TiB 2 were characterized as a function of temperature up to ~3050 °C. Elucidation of these properties are critical for the advancement of TiB 2 ceramics and other transition metal di-borides for use in high temperature applications such as hypersonic platforms, nuclear reactors, and atmospheric re-entry.

36 MATERIALS SCIENCE↗

Local Atomic Structure in Photo-isomerized Ruthenium Sulfur Dioxide Complexes Revealed by Pair Distribution Function Analysis

SO 2 linkage photoisomerization in crystalline ruthenium-based complexes has demonstrated nanophotonic phenomena such as optical switching and nano-optomechanical transduction. Molecular insights into these materials have been explored largely via the characterization of their photoinduced crystal structures via in situ single-crystal X-ray diffraction, known as photocrystallography. Photoinduced molecular disorder is present, which photocrystallography can model to the extent that it is confined within the periodic boundary of a unit cell. However, non-periodic molecular disorder is suspected to exist as well. In situ total scattering experiments were therefore carried out on finely powdered crystals of four ruthenium-sulfur dioxide complexes. Data were modeled using light-minus-dark' difference pair distribution function analysis, which afforded photoinduced structural changes exclusively. This revealed structural features that were first compared against models of photoinduced crystal structures known a priori from photocrystallography. Furthermore, statistical inference was then employed, which evidenced generally good agreement between the total scattering data and the photocrystallographic models, while revealing real differences that are indicative of a structure with only a short-range order. Overall, our findings demonstrate that in situ light-induced total scattering experiments on finely powdered crystals are able to reveal the photoinduced structure. Overall, the evidence suggests that such structure could include a short-range order as well as photocrystallographic content. Our demonstration experiment offers a pathway to develop studies that capture the short-range order in linkage photoisomers, while we have outlined the procedure for testing the validity of associated structural models.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Investigation of MgO additives on microstructure and properties of thin LLZO electrolytes for all-solid-state batteries

To realize high-energy density lithium lanthanum zirconate (LLZO)-based solid-state batteries (SSB), LLZO electrolytes should be fabricated with low thickness and high mechanical strength. An effective strategy for strengthening ceramic materials is to use additives. Here, we employed MgO nanopowders and fibers as additives for the thin LLZO electrolyte in order to improve the mechanical strength. The microstructure, mechanical properties, and electrochemical properties are characterized to investigate the effects of adding MgO and sintering time. The MgO remains at grain boundaries after sintering, making the microstructure of LLZO fine and uniform. The mechanical strength of the MgO-added LLZO was enhanced by more than 60% while maintaining high ionic conductivity (1 × 10 -4 S cm -1 ) at room temperature. Li symmetric cells using the MgO fiber–LLZO and MgO powder–LLZO exhibit 2 and 3 times higher critical current density (CCD) than those of pure LLZO, and a solid-state full cell exhibits stable cycling performance. Further, these results demonstrate that the use of MgO nanopowder or fiber as an additive for thin LLZO is beneficial for high-current density cycling, by improving mechanical properties and microstructure.

25 ENERGY STORAGE↗

Mössbauer Studies and the Microwave Properties of Al{sup 3+}- and In{sup 3+}-Substituted Barium Hexaferrites

The correlation of the chemical composition, the structure, and the microwave characteristic of solid solutions of the BaFe{sub 12–x}D{sub x}O{sub 19} (0.1 ≤ x ≤ 1.2) barium hexaferrite substituted with diamagnetic Al{sup 3+} and In{sup 3+} ions has been studied. The precise data on the crystal structure have been obtained by powder neutron diffraction using a high-resolution Fourier diffractometer (Dubna, JINR). The data on the distribution of the diamagnetic substituting ions in the hexaferrite structure have been obtained by Mössbauer spectroscopy. The microwave properties (the transmittance and the reflectance) have been studied in the frequency range 20–65 GHz and in external magnetic fields to 8 kOe. It is found that the transmission spectra are characterized by a peak that corresponds to the resonant frequency of the electromagnetic energy absorption, which is due to the ferromagnetic resonance phenomenon. The correlation of the chemical composition, the features of the ion distribution in the structure, and the electromagnetic properties has been revealed. It is shown that external magnetic fields shift the absorption peak of electromagnetic radiation to higher frequencies due to an increase in the magnetocrystal anisotropy. The results enable the conclusion that the features of the intrasublattice interactions and the electromagnetic properties should be explained using the phenomenological Goodenough–Kanamori model.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Thermodynamics of Bimetallic Joints between Titanium and Tantalum Produced by Laser Powder Bed Fusion

Laser powder bed fusion (LBPF) is currently the most mature metal additive manufacturing (AM) technology. While it does not have the same flexibility as directed energy deposition techniques to produce compositional gradients, LPBF can still be used to generate bimetallic parts by depositing one metal on a build plate made of another. Here, in this study, we print combinations of Ti-6Al-4V with Ta and characterize defects that occur at the interface. We use thermodynamic modeling to explain the formation of keyhole porosity and solidification cracks when Ta is built on a Ti baseplate, and the lack of defects when the materials are reversed. By understanding the mechanisms that lead to defect formation, the methodology demonstrated here can be applied to other material systems to efficiently design bimetallic LPBF processes.

36 MATERIALS SCIENCE↗

Investigation into Interfacial Mixing Behavior of Blown Powder Deposited Inconel 625-Copper Alloy Bimetallic for Improvement of Bimetallic Joint Strength

Use of laser blown powder, directed energy deposition (DED) provides a method for fabrication of bimetallic functional materials for high heat flux applications. However, this relatively new process currently has a low technology readiness level (TRL). Key to increasing the TRL is a better understanding of the factors that control mixing of the bi-metallic materials at the interface. The resulting interfaces in specimens obtained from three vendors were characterized using optical and electron microscopy with electron dispersion spectroscopy in addition to mechanical testing. Based on the range of process parameters and resulting interfaces, a model is being developed to predict interfacial mixing for development of specifications for improved and repeatable microstructures.

Additive Manufacturing↗