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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 613 records · Page 34

Pyrolysis Vacuum-Assisted Plasma Ionization Ion Mobility–Mass Spectrometry for Insoluble Polymer Analysis

Wire-based metal additive manufacturing utilizes the ability of additive manufacturing to fabricate complex geometries with high deposition rates (above 7 kg/h), thus finding applications in the fabrication of large-scale components, such as stamping dies. Traditionally, the workhorse materials for stamping dies have been martensitic steels. However, the complex thermal gyrations induced during additive manufacturing can cause the evolution of an inhomogeneous microstructure, which leads to a significant scatter in the mechanical properties, especially the toughness. Therefore, to understand these phenomena, arc-based additive AISI 410 samples were fabricated using robotic gas metal arc welding (GMAW) and were subjected to a detailed characterization campaign. The results show significant scatter in the tensile properties as well as Charpy V-notch impact toughness data, which was then correlated to the microstructural heterogeneity and delta (δ) ferrite formation. Post-processing (austenitizing and tempering) treatments were developed and an ~70% reduction in the scatter of tensile data and a four-times improvement in the toughness were obtained. The changes in mechanical properties were rationalized based on the microstructure evolution during additive manufacturing. Based on these, an outline to tailor the composition of “printable” steels for tooling with isotropic and uniform mechanical properties is presented and discussed.

36 MATERIALS SCIENCE↗

Mitigating Scatter in Mechanical Properties in AISI 410 Fabricated via Arc-Based Additive Manufacturing Process

Wire-based metal additive manufacturing utilizes the ability of additive manufacturing to fabricate complex geometries with high deposition rates (above 7 kg/h), thus finding applications in the fabrication of large-scale components, such as stamping dies. Traditionally, the workhorse materials for stamping dies have been martensitic steels. However, the complex thermal gyrations induced during additive manufacturing can cause the evolution of an inhomogeneous microstructure, which leads to a significant scatter in the mechanical properties, especially the toughness. Therefore, to understand these phenomena, arc-based additive AISI 410 samples were fabricated using robotic gas metal arc welding (GMAW) and were subjected to a detailed characterization campaign. The results show significant scatter in the tensile properties as well as Charpy V-notch impact toughness data, which was then correlated to the microstructural heterogeneity and delta (δ) ferrite formation. Post-processing (austenitizing and tempering) treatments were developed and an ~70% reduction in the scatter of tensile data and a four-times improvement in the toughness were obtained. The changes in mechanical properties were rationalized based on the microstructure evolution during additive manufacturing. Based on these, an outline to tailor the composition of “printable” steels for tooling with isotropic and uniform mechanical properties is presented and discussed.

36 MATERIALS SCIENCE↗

Effect of Aluminum Addition on the Evolution of Microstructure, Crystallographic Texture and Mechanical Properties of Single Phase Hexagonal Close Packed Mg-Li Alloys

In the present investigation, an effort has been made to understand the effect of aluminum addition to α Mg-Li alloys. The corresponding composition Mg-4Li-xAl (x = 0, 2, 4 and 6 wt.%) alloys have been prepared by stir casting route under an argon environment. Extrusion was carried out at 300 °C with the extrusion ratio of 15:1. Significant grain refinement was observed after extrusion. X-ray diffraction-based investigation of the cast and extruded alloys showed the presence of intermetallic compounds such as Mg{sub 17}Al{sub 12} and AlLi in the Al-rich alloys namely, Mg-4Li-xAl (x = 4 and 6 wt.%). These precipitates were also present in the extruded plus annealed samples, indicating the stability of the precipitates at high temperature. The bulk x-ray texture measurement revealed a crystallographic texture where the c-axis of the h.c.p crystals was perpendicular to the extrusion direction (ED) for extruded sample. A texture transition was observed on annealing. The c-axis was oriented parallel to the ED. Mechanical properties of the cast, extruded and extruded plus annealed material illustrate that the addition of Al led to enhancement in hardness, yield strength and ultimate tensile strength.

36 MATERIALS SCIENCE↗

Evolution of Microstructure, Residual Stress, and Tensile Properties of Additively Manufactured Stainless Steel Under Heat Treatments

This study investigated the microstructure, residual stress and tensile properties of the directed energy deposited stainless steel 316L (SS316L) under thermal annealing. Microstructure characterization shows the as-printed sample has laser-generated patterns where dendritic structure is observed at the edge of the patterns and cellular structure dominates the interior region. Here, the thermal annealing at 983 and 1093°C effectively removes the dendritic/cellular structures. Synchrotron X-ray diffraction reveals that the as-fabricated SS316L exhibits compressive residual stress of -197.4 MPa. The stress is greatly relieved to -53.8 MPa after annealing at 1093°C. The room temperature tensile testing indicates that the yield strength and ultimate tensile strength drop from 378 and 502 MPa in the as-printed sample to 258 and 446 MPa in the annealed samples (1093°C), respectively. Our study provides insights into the relationship between microstructure, residual stress, and tensile properties of laser additive manufactured SS316L.

36 MATERIALS SCIENCE↗

Phase structures and morphologies of tempered CA6NM stainless steel welded by hybrid laser-arc process

The post-weld tempered microstructure of hybrid laser-arc welded CA6NM, a cast low carbon martensitic stainless steel, was investigated. The microstructural evolutions from the fusion zone to the base metal were characterized in detail using optical microscopy, scanning electron microscopy (SEM), electron backscatter diffraction (EBSD), X-ray diffraction (XRD) and microhardness techniques. The fusion zone, in its post-weld tempered condition, consisted of tempered lath martensite, residual delta-ferrite with various morphologies, reversed austenite and chromium carbides. The reversed austenite, which can be detected through both EBSD and XRD techniques, was found to be finely dispersed along the martensite lath boundaries, particularly at triple junctions. Based on the EBSD analysis, the orientation relationship between the reversed austenite and the adjacent martensite laths seemed to follow the Kurdjumov-Sachs (K-S) model. The results also revealed the presence of the reversed austenite in the different regions of the heat affected zone after post-weld tempering. The microindentation hardness distribution was measured, and correlated to the evolution of the corresponding microstructure across the welds. - Highlights: •The EBSD analysis was performed on hybrid laser-arc welded CA6NM. •The FZ consisted of tempered lath martensite, reversed austenite, carbides and δ ferrite after tempering. •The reversed γ was formed along the α′ lath boundaries, particularly at triple junctions.

36 MATERIALS SCIENCE↗

Evolution of microstructures and mechanical properties during solution treatment of a Ti–V–Mo-containing high‑manganese cryogenic steel

Highlights: • High-Mn cryogenic steels are getting the spotlight in the cryogenic market. • The grain size grew slowly and the yield strength remained almost stabilized with an increase of solutionizing temperature. • The Hall–Petch strengthening coefficient for yield strength was small, estimated to be 153 MPa μm{sup 0.5}. • The weakening effect of solutionizing temperature on grain size was attributed to the nano-sized (Ti, V, Mo)C precipitate. - Abstract: The effect of solution treatment on the microstructure and mechanical properties of a high‑manganese (Mn) twin-induced plastic (TWIP) cryogenic steel that was alloyed from elemental titanium (Ti), vanadium (V) and molybdenum (Mo) was investigated by a variety of techniques such as microstructural characterization, room tensile testing and − 196 °C impact testing. The austenite grain size grew slowly with an increase of the solutionizing temperature (ST). The relatively weak effect of the ST on the austenite grain size is attributed to the superior thermal stability and coarsening resistance of the (Ti, V, Mo)C precipitate, which hindered austenite grain growth. An increase in ST improved the low-temperature toughness (LTT) significantly and decreased the strain hardening rate (SHR), but had no significant effect on the yield strength. The Hall–Petch strengthening coefficient for yield strength was small, and was estimated to be 153 MPa μm{sup 0.5}. Undissolved large-sized chromium (Cr) carbide can deteriorate the LTT significantly. Because of its excellent mechanical properties, high-Mn steel that was alloyed by elemental Ti, V and Mo can be used to manufacture storage tanks for liquefied natural gas.

36 MATERIALS SCIENCE↗

Effects of W on creep behaviors of novel Nb-bearing high nitrogen austenitic heat-resistant cast steels at 1000 °C

Highlights: • The synergistic CALPHAD and experimental approaches are adopted. • Creep behaviors of high nitrogen austenitic alloys are investigated at 1000 °C. • Creep properties are improved through the W solid solution strengthening. • W additions promote the formation of (Cr,Fe,W){sub 23}C{sub 6} instead of (Cr,Fe,W){sub 7}C{sub 3}. • (Cr, W)-rich precipitates severely degrade the creep properties. - Abstract: Recently, there is an urgent demand from automotive industries to develop new austenitic heat-resistant cast steels that withstand exhaust gas temperatures as high as 1000 °C. In this study, the effect of W additions on the creep behavior of a series of Nb-bearing high nitrogen austenitic heat-resistant cast steels was investigated at 1000 °C and 50 MPa. Microstructures before and after creep rupture tests were carefully characterized to illustrate the microstructural evolution during creep deformation. Microstructural analyses revealed that the W addition did not affect the formation of primary Nb(C,N), whereas significantly promoted the precipitation of primary (Cr, W)-rich phases, particularly those cellular structures along grain boundaries. The W solid solution strengthening and the secondary precipitation strengthening of submicron-scale (Cr, W)-rich phase improved the creep resistance of the alloys through increasing the hardness of γ-austenite and pinning the dislocations. However, the primary cellular (Cr, W)-rich structures significantly accelerated the nucleation and propagation of creep cracks along grain boundaries, thereby increasing the creep rate and decreasing the creep life.

36 MATERIALS SCIENCE↗

Evolution of microstructure and mechanical properties of selective laser melted Ti-5Al-5V-5Mo-3Cr after heat treatments

Titanium alloy Ti5553 (Ti-5Al-5Mo-5V-3Cr) is an excellent candidate for structural applications and additive manufacturing processes, since, unlike Ti6Al4 V, when built via selective laser melting and/or post additive manufactured welding, it maintains a near-beta microstructure that is both ductile and high strength. Another feature is that Ti5553 properties are adaptable through post build heat treatment. This study explores the heat treatability of selective laser melted Ti5553 up to temperatures approaching the β-transus. Here the results show strength increases while maintaining ductility at high temperatures (700–800°C), but embrittlement occurs at intermediate temperatures (400–600°C) likely due to changes in volume fraction and morphology of the α-phase and/or the presence of the ω-phase. Microstructure and X-ray diffraction are reported after heat-treating to better understand this mechanical response.

42 ENGINEERING↗

FRACTURE RESISTANCE OF CAST AUSTENITIC STAINLESS STEELS

Cast austenitic stainless steels (CASS) possess excellent corrosion resistance and mechanical properties and are used alongside with wrought stainless steels (SS) in light water reactors for primary pressure boundaries and reactor core internal components. In contrast to an austenitic microstructure of wrought SS, CASS alloys consist of a dual-phase microstructure of delta ferrite and austenite. While the delta ferrite is critical for the service performance of CASS alloys, it is also vulnerable to embrittlement when exposed to reactor service temperatures and fast neutron irradiations. In this study, the combined effect of thermal aging and neutron irradiation on the degradation of CASS alloys was investigated. Static casts of CF-3 and CF-8 grades with > 23% delta ferrite were selected for the study, and specimens with and without prior thermal aging were irradiated at ~320°C to about 0.08 dpa. Crack growth rate and fracture toughness J-integral resistance curve tests were performed in simulated light water reactor environments with low corrosion potential. While no elevated crack propagation rates were detected, significant reductions in fracture toughness were observed after either thermal aging or neutron irradiation. The loss of fracture toughness due to neutron irradiation seemed more evident in the samples without prior thermal aging. Transmission electron microscope (TEM) examination showed that both neutron irradiation and thermal aging affect the microstructural evolution of delta ferrite. A high density of G-phase precipitates was observed in both thermally aged and irradiated specimens The evolution of the precipitate microstructure is more extensive in the samples subjected to both thermal aging and neutron irradiation. The similarity of precipitate microstructures resulting from thermal aging and neutron irradiation are consistent with the fracture toughness results, suggesting a common microstructural origin of the observed embrittlement among the tested specimens.

cast austenitic stainless steels↗

New Mechanistic Models of Long Term Evolution of Microstructure and Mechanical Properties of Nickel Based Alloys

The report describes the development of a discrete element method (DEM) based modeling approach to quantitatively predict deformation and failure of typical nickel based superalloys. A series of experimental data, including microstructure and mechanical property characterization at 600°C, was collected for a relatively simple, model solid solution Ni-20Cr alloy (Nimonic 75) to determine inputs for the model and provide data for model validation. Nimonic 75 was considered ideal for this study because it is a certified tensile and creep reference material. A series of new DEM modeling approaches were developed to capture the complexity of metal deformation, including cubic elastic anisotropy and plastic deformation both with and without strain hardening. Our model approaches were implemented into a commercially available DEM code, PFC3D, that is commonly used by engineers. It is envisioned that once further developed, this new DEM modeling approach can be adapted to a wide range of engineering applications.

36 MATERIALS SCIENCE↗

Microstructure Experiments-Enabled MARMOT Simulations of SiC/SiC-based Accident Tolerant Nuclear Fuel System

We have undertaken an experimental-computational project that addresses a few key technology gaps associated with the use of SiC/SiC composites for light water reactor fuel cladding. Two principal endeavors in this project are to assess the irradiation-induced microstructural changes and swelling in SiC/SiC composites, and to characterize and model the porous oxide surface layer (when exposed to steam) along SiC recession that is detrimental to the clad integrity under accident conditions. The project tasks are: (i) ion irradiation and characterization (University of Tennessee, Knoxville), (ii) mechanical tests and analysis (University of South Carolina), (iii) steam exposure tests (Oak Ridge National Laboratory), (iv) electron microscopy and spectroscopic characterization (NC State University), (v) x-ray microscopy and reconstruction (University of South Carolina and NC State University), (vi) phase field modeling and simulations (NC State University and Idaho National Laboratory). The effects of 10 MeV Au ion irradiation at 350°C on the microstructure evolution in SiC/SiC composites are investigated at doses up to 400 displacements per atom (dpa) at the University of Tennessee, Knoxville. Atomic force microscopy and optical profilometry reveal irradiation induced axial and radial shrinkage of the fibers for doses greater than 10 dpa. Based on detailed electron microscopy characterization, the primary cause of the fiber shrinkage is attributed to irradiation-induced loss of carbon packets. Additionally, the multilayer PyC interface is observed to portray high resistance to irradiation damage. The mechanical response and failure mechanisms of un-irradiated samples is also assessed through loading tests and X-ray imaging at the University of South Carolina. Steam exposure tests are performed at the Oak Ridge National Laboratory in a facility that represents a reactor pressure vessel under a loss-of-coolant-accident scenario. The samples that are analyzed methodically in this report are tested for 32/31 hours at 1200°C with a velocity of 0.25 cm/s for the pressures: 0.1 MPa, 0.45 MPa, 0.92 MPa and 1.38 MPa. Scanning/transmission electron microscopy analysis conducted at the NC State University (NCSU) shows that the oxide layer thickness increases with the steam pressure. While the oxide layer is crystalline (α- cristobalite) for the pressures 0.45 MPa, 0.92 MPa and 1.38 MPa, the layer is amorphous at 0.1 MPa. Results from Raman spectroscopy have also confirmed the formation of α-cristobalite phase of SiO₂. The abrupt increase in the integrated Raman intensity ratio between steam pressures 0.1 and 0.45 MPa suggests the onset of accelerated crystallization. Non-destructive three dimensional X-ray microscopy/tomography (XCT) and computational image processing techniques are employed by the University of South Carolina to probe the porous oxidation features on SiC samples at varying pressures. Interestingly, most pores are observed to be located away from the surface as well as the oxide-SiC interface. The average oxide layer thickness assessed from the XCT analysis is seen to be in excellent agreement with the values determined through scanning electron microscopy analysis for the highest pressures where the oxide layer is relatively more uniform. A phase-field model developed by the NC State University and Idaho National Laboratory for simulating oxidation of SiC by steam captures the paralinear kinetics of SiC oxidation with a high degree of fidelity. Results from quasi-one-dimensional and two dimensional simulations show that the pores with oxidizing species lead to a higher volatilization rate. These simulations indicate that the enhanced apparent volatilization rates at higher pressures observed in experiments can be rationalized by the increased volatilization from the pores. The project team has also successfully developed the capability to import images from experiments for realistic evolution of the oxidizing microstructure.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

The effect of fiber microstructure on evolution of residual stresses in silicon carbide/titanium aluminide composites

This paper examines the effect of the morphology of the SCS6 silicon carbide fiber on the evolution of residual stresses in SiC/Ti composites. A micromechanics model based on the concentric cylinder concept is presented which is used to calculate residual stresses in a SiC/Ti composite during axisymmetric cooling by a spatially uniform temperature change. The silicon carbide fiber is modeled as a layered material with five distinct transversely isotropic and orthotropic, elastic layers, whereas the titanium matrix is taken to be isotropic, with temperature-dependent elastoplastic properties. The results arc compared with those obtained based on the assumption that the silicon carbide fiber is isotropic and homogeneous.

Pindera, Marek-Jerzy↗