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At least 775 records · Page 43

Build Orientation Effects on Texture and Mechanical Properties of Selective Laser Melting Inconel 718

The production of components via selective laser melting (SLM) metal additive manufacturing results in microstructures unique to the process that are highly dependent on laser processing parameters and orientation of part geometry relative to the build direction. This study investigates the variation in tensile properties of SLM Inconel 718 at varying angles with respect to build direction. ASTM E8 tensile specimens were built in XY, Z, and B+45 from Z orientations to near-net shape, HIP and heat treated, and tensile tested at room temperature. Orientation dependence of mechanical properties was observed; Z samples had the lowest strength and highest elongation, while XY samples had the highest strength and lowest elongation. Optical, SEM, and EBSD analysis were conducted to probe for microstructure variation that could be the cause of the difference in mechanical properties. Analysis of pole figures and grain maps suggests a preferred grain texture and twinning orientation that aligns with the build direction, which may contribute to the anisotropic enhancement in ductility.

36 MATERIALS SCIENCE↗

A Coupled Small and Wide-Angle X-Ray Scattering Study of Phase Transformation Mechanisms in U-6Wt Pct Nb

The elevated temperature phase transformation kinetics of U-6wt%Nb in both wrought and cast conditions were investigated using in-situ high energy synchrotron X-ray scattering. The evolution of the phase content, γ-phase composition, and microstructure morphology was determined through the analysis of simultaneously collected wide-angle diffraction and small-angle scattering (SAXS) data. The results of the wide-angle scattering analysis, especially the phase fractions and average composition of the γ-phase, provide model parameters to enable a quantitative analysis using the SAXS data. Greater clarity regarding the kinetics of different precipitation mechanisms, namely the continuous precipitation (CP) of α-U within the γ-phase matrix and the discontinuous (DP) grain boundary precipitation of a lamellar microstructure, consisting of α-U and Nb-rich γ-phase are obtained from the coupled measurement modes. These results indicate that the CP mechanism is responsible for the initial precipitation of α-U at all temperatures considered. Near the nose in the time-temperature-transformation (TTT) diagram at ~798 K, both mechanisms are active during the early stages of phase transformation. However, the DP mechanism has an increasingly long incubation period with decreasing temperature below the TTT nose. In conclusion, the average interlamellar spacing obtained from the SAXS analysis increases with time, providing further evidence of the so-called divergent DP behavior previously observed in U-6wt%Nb alloys.

36 MATERIALS SCIENCE↗

Deformation Mechanism Transition in Additively Manufactured Compositionally Graded Fe-Base Alloys

Microstructure-dependent deformation and fracture behavior was investigated for an additively manufactured compositionally graded alloy (CGA) printed using the laser-directed energy deposition (L-DED) method to explore an alternative approach for dissimilar metal joints in nuclear energy systems. The electron backscatter diffraction (EBSD) maps from scanning electron microscopy (SEM) display a clear microstructural transition with decreasing austenite-forming elements (Ni and Mn), from an austenite (γ) dominant structure, to a complex composite structure containing ferrite (α), martensite (α') and retained austenite, and then to a fully ferritic structure. EBSD data were recorded in situ during tensile testing in SEM, and the evolution of the deformation mechanism and microstructure was characterized using Kikuchi diffraction pattern analysis. Complementary analysis for high-resolution features was also performed using scanning transmission electron microscopy (STEM). The Ni/Mn-rich austenite-dominant microstructures showed a complex deformation mechanism of two-step martensitic transformation (γ→ε→α'), whereas the minor austenite phase retained in the ferrite and/or martensite matrix showed a single transformation route (γ→α'). Ordinary dislocation glide and twinning via partial dislocation glide were observed in the austenite deformation. Meanwhile, the ferrite and martensite grains deformed mainly by ordinary dislocation slips and grain rotation. Furthermore, static tensile fracture was also highly dependent on local composition and phase constituents.

36 MATERIALS SCIENCE↗

Microstructural characterization and assessment of mechanical properties of concrete based on combined elemental analysis techniques and Fast-Fourier transform-based simulations

This paper presents a pixel-based modeling approach of concrete which combines an experimental characterization of concrete and the Fast-Fourier transform simulations. High-resolution phase maps created from experimental characterization by micro X-ray fluorescence, energy dispersive X-ray analysis, and X-ray diffraction contain 9 different phases, including 22.17 vol.% of hydrated cement paste, 54.21 vol.% of minerals, and 23.62 vol.% of interfaces. These phases provide the input for determining the effective elastic properties, coupled with Fast-Fourier transform-based simulation. The simulation results show that the effective range of Young’s modulus of concrete is comparable with the range of experimental values ~ 37 ± 4 GPa with the assumption of realistic properties of interfaces.

36 MATERIALS SCIENCE↗

Reconstruction of concrete microstructure using complementarity of X-ray and neutron tomography

The concrete microstructure was successfully reconstructed using the complementarity of X-ray and neutron computed tomography (CT). Neither tomogram alone was found to be suitable to properly describe the microstructure of concrete under this study. However, by merging the information revealed by the two modalities, and using image segmentation, noise reduction, and image registration techniques we reconstruct the concrete microstructure. Void, aggregate, and cement paste phases are successfully captured down to the images' spatial resolution, even though the aggregate consists of multiple minerals. The coarse-aggregate volume fraction of the reconstructed microstructure was similar to that of the mixing proportions. Furthermore, image-based finite element analysis is performed to demonstrate the effects of microstructure on stress concentration and strain localization.

36 MATERIALS SCIENCE↗

Strength-ductility synergy through microstructural and compositional heterogeneity in directed energy deposition additive manufacturing of face-centered cubic materials

Directed energy deposition (DED) is an additive manufacturing (AM) process based on welding technology and offers the advantages of large build volume, high deposition rate, and ability to fabricate multi-material parts. Epitaxial continuous columnar grain growth is a characteristic microstructural feature of DED processed alloys. In this study, a bamboo-like microstructure (periodic alternation of equiaxed and columnar structure) was produced by adopting an intermittent deposition strategy in 316L stainless steel and Inconel 625. The formation of a bamboo-like alternating microstructure was confirmed through electron backscattered diffraction (EBSD) analysis. Hardness mapping showed that the columnar to equiaxed transition (CET) occurred at the region right below the fusion line. A finite element (FE) model was used to investigate the relationship between the temperature gradient (G) and the solidification rate (R). The FE model showed a low G/R ratio at the region right below the interface promoting the CET. The grain size and material-dependent deformation behaviors are analyzed using digital image correlation (DIC). The lower deformation on the fine-grain regions observed in DIC analysis is attributed to a higher strain hardening rate, which is confirmed through dislocation density analysis on a tensile-interrupted specimen. The periodically alternating grain size coupled with the microstructural changes caused by intermittent deposition strategy result in a better strength-ductility synergy in both single-material and bimetallic specimens.

36 MATERIALS SCIENCE↗

Trace Impurities Identified as Forensic Signatures in CMX-5 Fuel Pellets Using X-ray Spectroscopic Techniques

We report that small-particle analysis is a highly promising emerging forensic tool for analysis of interdicted special nuclear materials. Integration of microstructural, morphological, compositional, and molecular impurity signatures could provide significant advancements in forensic capabilities. We have applied rapid, high-sensitivity, hard X-ray synchrotron chemical imaging to analyze impurity signatures in two differently fabricated fuel pellets from the 5th Collaborative Materials Exercise (CMX5) of the IAEA Nuclear Forensics International Working Group. The spatial distributions, chemical compositions, and morphological and molecular characteristics of impurities were evaluated using X-ray absorption near-edge structure (XANES) and X-ray fluorescence chemical imaging to discover principal impurities, their granularity, particle sizes, modes of occurrence (distinct grains vs incorporation in the UO 2 lattice), and sources and mechanisms of incorporation. Differences in UO 2+x stoichiometry were detected at the microscale in nominally identical UO 2 ceramics (CMX5-A and CMX5-B), implying the presence of multiple UO 2 host phases with characteristic microstructures and feedstock compositions. Al, Fe, Ni, W, and Zr impurities and integrated impurity signature analysis identified distinctly different pellet synthesis and processing methods. For example, two different Al, W, and Zr populations in the CMX5-B sample indicated a more complex processing history than the CMX5-A sample. K-edge XANES measurements reveal both metallic and oxide forms of Fe and Ni but with different proportions between each sample. Altogether, these observations suggest multiple sources of impurities, including fabrication (e.g., force-sieving) and feedstock (mineral oxides). This study demonstrates the potential of synchrotron techniques to integrate different signatures across length scales (angstrom to micrometer) to detect and differentiate between contrasting UO 2 fuel fabrication techniques.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Examination of Intergranular Crack on SC0234

The microstructure of the SC0234 weld was evaluated per DA-SPEC-01067, ''General Purpose Heat Source (GPHS) Plutonium-238 Dioxide Fueled Clad Product Specification'' and it was determined that the weld microstructure conformed to the quality requirements. During the examination of weld cross section, the metallographic analysis revealed the presence of a surface crack. Prior visual examination per RPS-TA55-303 had not revealed the crack, nor did the surface photography performed per RPS-TA55-302. The presence of the crack does not violate any of the product specifications called out on DA-SPEC-01067. Although there is a well-documented history of weld hot crack susceptibility in the early development of the DOP-26 iridium alloy, a surface crack such as this had not been documented during welding at Los Alamos. In the interest of better understanding the cause; the product engineer/program recommended further examination of the crack. This report discusses the examination of the crack found in the weld cross section of simulant clad SC0234. Metallography, Scanning Electron Microscopy (SEM) and Energy Dispersive Spectroscopy techniques (EDS) where used in the analysis of the crack and the surrounding weld microstructure.

36 MATERIALS SCIENCE↗

Influence of Thermal Treatment on the Microstructure, Mechanical Properties, and Corrosion Resistance of Newly Developed Ti20Nb13Zr Biomedical Alloy in a Simulated Body Environment

The effect of thermal treatments on the microstructure, hardness, and electrochemical performance in a simulated body fluid were studied for the newly developed (β + α) Ti20Nb13Zr alloy (TNZ) for biomedical applications. The alloy was heat-treated for 1 h at 900 °C and then cooled at different cooling rates. Then, the solution-treated samples were aged at 400, 500, or 600 °C for 5 h. The phase evolution and microstructure of the treated alloy were examined using XRD and SEM/EDX analysis. The mechanical properties were assessed using microindentation. The surface protection performance against corrosion was assessed by potentiodynamic polarization and electrochemical impedance spectroscopic analysis. The obtained results showed that the wide range of microstructure with varied volume fraction and morphology of β and α were obtained with different heat treatment conditions. The different phases’ sizes and distributions influenced the microstructure obtained during the heat treatment, thereby affecting the mechanical properties. The corrosion performance significantly altered with variations in the microstructure of the TNZ alloy as a result of the different thermal treatments. The heat treatment of TNZ conferred enhanced combination of mechanical and corrosion protection compared to that of the commercial Ti6Al4V alloy.

36 MATERIALS SCIENCE↗

Microstructure Reconstruction of Sheet Molding Composite Using a Random Chips Packing Algorithm

Fiber-reinforced polymer composites are strong candidates for structural materials to replace steel and light alloys in lightweight vehicle design because of their low density and relatively high strength. In the integrated computational materials engineering (ICME) development of carbon fiber composites, microstructure reconstruction algorithms are needed to generate material microstructure representative volume element (RVE) based on the material processing information. The microstructure RVE reconstruction enables the material property prediction by finite element analysis (FEA)This paper presents an algorithm to reconstruct the microstructure of a chopped carbon fiber/epoxy laminate material system produced by compression molding, normally known as sheet molding compounds (SMC). The algorithm takes the result from material’s manufacturing process as inputs, such as the orientation tensor of fibers, the chopped fiber sheet geometry, and the fiber volume fraction. The chopped fiber sheets are treated as deformable rectangle chips and a random packing algorithm is developed to pack these chips into a square plate. The RVE is built in a layer-by-layer fashion until the desired number of lamina is reached, then a fine tuning process is applied to finalize the reconstruction. Compared to the previous methods, this new approach has the ability to model bended fibers by allowing limited amount of overlaps of rectangle chips. Furthermore, the method does not need SMC microstructure images, for which the image-based characterization techniques have not been mature enough, as inputs. Case studies are performed and the results show that the statistics of the reconstructed microstructures generated by the algorithm matches well with the target input parameters from processing.

Huang, Tianyu↗

The effects of material anisotropy on secondary processing of additively manufactured CoCrMo

Components produced by near net shape additive manufacturing processes often require subsequent subtractive finishing operations to satisfy requisite surface finish and geometric tolerances. It is well established that the microstructure and properties of the as-built component are sensitive to the additive processing history. Therefore, downstream secondary processes may be affected by the as-built components’ mechanical behavior. In this work we study the sensitivity of secondary machining operations on CoCrMo samples produced via laser powder bed fusion. Utilizing novel high-throughput mechanical testing, microstructure characterization, and a rigorous statistical analysis we investigate the degree of material anisotropy present in the as-built material. We then study the effects of this anisotropy on secondary processing via slot milling experiments. Our results indicate that mechanical anisotropy is driven by both the morphology of the microstructure as well as crystallographic texture. Furthermore, the machining force response is correspondingly sensitive to these sources of anisotropy, which has the potential to impact how manufacturers finish additively built parts.

36 MATERIALS SCIENCE↗

Post irradiation examination of a uranium-zirconium hydride TRIGA fuel element

Low-enriched (LEU) U-ZrH fuel, with a 235 U content less than 20% of the total uranium, is being evaluated for possible use in different types of reactors, including space nuclear systems, light water reactors (LWRs) and micro-reactors. As a result, it is beneficial to better understand the macrostructural and microstructural changes that occur in this fuel during irradiation. This paper reports the results of the post irradiation examination of an LEU U-ZrH fuel element (30 wt.% U, <20% 235 U) using neutron radiography, precision gamma scanning, chemical analysis, optical metallography and scanning electron microscopy combined with energy dispersive spectroscopy and wavelength dispersive spectroscopy, where the fuel element was irradiated in a Training, Research, Isotope, General Atomics (TRIGA) reactor. Results of microstructural characterization indicated some dehydriding and cracking of the U-ZrH fuel occurred during irradiation; an axial and radial burnup gradient existed in the fuel during irradiation, as measured by gamma scanning and chemical analysis; negligible microstructural changes transpired during irradiation, based on comparison of irradiated and as-fabricated U-ZrH fuel microstructures; and, negligible, fission product-rich, phases could be resolved in a U-ZrH fuel that was irradiated to a calculated 20% depletion of 235 U.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Relationship between dislocations and residual stresses in cold-drawn pearlitic steel analyzed by energy-dispersive X-ray diffraction

We analyzed the dislocation distribution of cold-drawn pearlitic-steel wire by using the line-profile analysis based on the energy dispersive X-ray diffraction (EDXD). Although this line-profile analysis requires a high resolution in reciprocal space, the resolution for EDXD is generally poor due to the energy resolution of the detector. Our analysis demonstrated that the resolution in the reciprocal space can be maximized at small scattering angles. Using the line-profile analysis based on the EDXD, the microstructural parameters such as the crystallite size and the dislocation density of the ferrite phase in the pearlitic steel were successfully analyzed. In addition, the distribution of the residual stress of the ferrite phase of a pearlitic steel wire was also analyzed using the EDXD measurement. - Highlights: • Energy dispersive X-ray diffraction is applied to the line-profile analysis. • Distribution of dislocations in ferrite in the pearlitic steel wire is analyzed. • Relationship between dislocations and residual stress is discussed.

36 MATERIALS SCIENCE↗

Advances and Achievements in In Situ Analysis of Corrosion and Structure–Property Relationship in Mg Alloys

Every year, TMS Magnesium Committee carefully selects a special topic in magnesium (Mg) related research and development not only having the hottest subject from both academic and industrial perspectives but also demonstrating major achievements within this subject. Following last year’s topic on Mg microallying [1], this year’s focus is on in-situ methods and associated techniques in their broad definition spanning from laboratory- to large- scale facilities to process monitoring. The applications of in-situ techniques have a wide spectrum from the analysis of melts and liquid-solid transitions to solid-state phenomena during thermo-mechanical processing and heat treatments to surface interactions with various environments. Therefore, such works are of significant interest to scientists working in the area of Mg alloy development as well as to a much broader audience from both academia and industry. This interest is primarily caused by challenges in the analysis of structure-property relationship in Mg alloys, and even cursory glance of literature reveals sharp increase of publications relevant to this topic recently. For instance, very high reactivity of Mg as well as its well-known propensity to substantially alter structure upon unloading in mechanical testing makes it difficult to understand and thus to simulate correlation between microstructures observed in post-mortem analysis and physical processes during testing or fabrication. However, recent advances in in-situ analysis based on large-scale research facilities such as neutron scattering and synchrotron radiation sources as well as microscopy-based, acoustic emission, and other more traditional techniques allowed significant achievements. Apart from apparent development of relevant experimental techniques, a significant part of this success should also be attributed to increasing accessibility of the facilities and simplification of their use from a user perspective. The selection of articles in this special topic is quite far from comprehensive review covering all aspects of in-situ methods available for metallic materials development. However, this was not the purpose in any case. Instead, this selection is intended to present several studies on Mg alloys and Mg-based composites with the use of in-situ techniques. In addition, it overviews two techniques, ‘Acoustic Emission’ (AE) and ‘Ambient-Pressure X-ray Photoelectron Spectroscopy’ (AP-XPS), that are rather novel to the Mg community. These studies are supposed to give readers representative examples of such techniques potential and to help in navigating the spectrum of modern state-of-the-art analytical methods facilitating the development of Mg alloys. These articles are organized in the order corresponding to typical Mg alloy lifecycle from material preparation and solidification to thermo-mechanical processing and product fabrication to degradation.

36 MATERIALS SCIENCE↗

Electrochemically deposited BiTe-based nanowires for thermoelectric applications

Nanostructured materials systems such as thin-films and nanowires (NWs) are promising for thermoelectric power generation and refrigeration compared to traditional counterparts in bulk, due to their enhanced thermoelectric figures-of-merit. BiTe and its derivative compounds, in particular, are well-known for their near-room temperature thermoelectric performance. In this work, both the binary and ternary BiTe-based nanowires namely, BiTe and BiSbTe, were synthesized using template-assisted electrodeposition. Diameters of the nanowires were controlled by the pore sizes of the anodised alumina (AAO) templates used. Systematic study on the compositional change as a function of applied potential was carried out via Linear Sweep Voltanmetry (LSV). Chemical compositions of the nanowires were studied using Energy Dispersive X-ray Spectrometry (EDXS) and their microstructures evaluated using diffraction and imaging techniques. Results from chemical analysis on the nanowires indicated that while the Sb content in BiSbTe nanowires increased with more negative deposition potentials, the formation of Te{sup 0} and Bi{sub 2}Te{sub 3} were favorable at more positive potentials.

36 MATERIALS SCIENCE↗

Thermal stability of additively manufactured austenitic 304L ODS alloy

Thermal stability and high-temperature mechanical properties of a 304L austenitic oxide dispersion strengthened (ODS) alloy manufactured via laser powder bed fusion (LPBF) are examined in this work. Additively manufactured 304L ODS alloy samples were aged at temperatures of 1000, 1100, and 1200 °C for 100 h in an argon atmosphere. Microstructure characterization of LPBF 304L ODS alloy before and after the thermal stability experiments revealed that despite the annihilation of dislocations, induced cellular substructure by the LPBF process was partially retained in the ODS alloy even after aging at 1200 °C. The size of Y-Si-O nanoparticles after aging at 1200 °C increased from 25 to 50 nm. EBSD analysis revealed that nanoparticles retained the microstructure of LPBF 304L ODS and hindered recrystallization and further grain growth. At 600 °C and 800 °C, the yield stress of the 290 and 145 MPa were measured, respectively, which are substantially higher than 113 MPa, and 68 MPa for 304L at the same temperatures. Furthermore, the creep properties of LPBF 304L ODS alloy were evaluated at a temperature of 700 °C under three applied stresses of 70, 85, and 100 MPa yielding a stress exponent (n) of ~7.7; the minimum creep rate at 100 MPa was found to be about two orders of magnitude lower than found in the literature for wrought 304L stainless steel.

36 MATERIALS SCIENCE↗