Engineering Papers⌕ Search

SEARCH · Engineering Papers

Results for “microstructure characterization”

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.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 307 records · Page 17

Joining of Thermoset Carbon Fiber Reinforced Polymer and AZ31 Magnesium Alloy Sheet Via Friction Stir Interlocking

A new technique called friction stir interlocking (FSI) was applied for lap-joining of AZ31 magnesium sheet and thermoset carbon fiber reinforced polymer (TS-CFRP) sheet. Instead of directly joining AZ31 and TS-CFRP, a series of magnesium interlocks were used to friction stir weld with AZ31 sheet to enable joining with TS-CFRP. Microstructural characterization of joint cross sections showed that a tool rotation rate of 800 rpm produced incomplete mixing of magnesium interlocks and the top AZ31 sheet, while 1200 rpm achieved sufficient material mixing to avoid unwelded regions. Mechanical property characterization showed that AZ31/TS-CFRP dissimilar joints failed through the magnesium interlock shanks during lap shear tensile testing, with a maximum normalized joint strength reaching ~100 MPa.

Wang, Tianhao↗

Understanding Oxide–Metal Interactions During Hot Isostatic Pressing to Diffusion Bond Aluminum Alloy 6061 Plates

The interaction between Mg, Si, and Al 2 O 3 during hot isostatic pressing diffusion bonding of aluminum alloy 6061 (AA6061) plates was investigated through thermodynamic calculations and experimental microstructural characterization. Thermodynamic calculations as functions of temperature, pressure, and composition revealed that the interaction among Mg, Si, and Al 2 O 3 yields Mg 2 Si and either MgO + Al or MgAl 2 O 4 + Al, facilitating the reduction of Al 2 O 3 and allowing Al/Al metallic bonds to form. Total pressure variation had a negligible influence on the oxygen partial pressure, and consequently, the reaction product formation. Oxygen partial pressure variation as a function of temperature and initial amount of Al 2 O 3 determined the formation of either MgO or MgAl 2 O 4 . Experimental Hot Isostatic Pressure (HIP) bonding at 723 K and 833 K under a constant pressure of 1017 atm documented the cooling rate-dependent formation of β–Mg 2 Si precipitates. High-resolution transmission electron microscopy imaging and selected area electron diffraction patterns verified the formation of β–Mg 2 Si and MgO at the interface but did not detect MgAl 2 O 4 . In conclusion, findings from this study clarify the role of thermochemical interactions in oxide disruption and bonding mechanisms during HIP diffusion bonding of AA6061 and provide guidance for optimizing joining processes for monolithic nuclear fuel assemblies.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Creep Behavior and Phase Equilibria in Model Precipitate Strengthened Alumina-Forming Austenitic Alloys

Abstract Creep-rupture behavior and microstructural response in alumina-forming austenitic (AFA) alloys with two different precipitation strengthening mechanisms, “Laves-phase + M 23 C 6 carbide” and “coherent L1 2 γ′-Ni 3 (Al,Ti),” were explored as “model” cases of multi-phase, multi-scale heat-resistant AFA alloys for 650–750°C use. These alloys will be used to guide and verify computational alloy design and life-prediction modeling under an on-going eXtremeMAT project through the Office of Fossil Energy and Carbon Management, US Department of Energy. Computational thermodynamics were used to design and predict the amounts of strengthening and deteriorating secondary phases at 750°C. Creep-rupture lives of the alloys tested at 750°C and 100 MPa were in a range of 4000–9000 h, and the microstructure at the gage/grip after creep-rupture testing was compared with isothermally aged alloys for 1500 h, as well as the calculated phases. Detailed microstructure characterization includes phase identification, volume fraction measurement, and compositional analysis, which were correlated with the creep-rupture properties. High-temperature oxidation resistance was also screened and compared with commercial, chromia-forming heat-resistant steels. These model alloys also provide the basis for further design and optimization of next generation AFA alloys with improved creep resistance.

36 MATERIALS SCIENCE↗

Novel self-assembled two-dimensional layered oxide structure incorporated with Au nanoinclusions towards multifunctionalities

Two-dimensional (2D) layered oxides have recently attracted wide attention owing to the strong coupling among charges, spins, lattice, and strain, which allows great flexibility and opportunities in structure designs as well as multifunctionality exploration. In parallel, plasmonic hybrid nanostructures exhibit exotic localized surface plasmon resonance (LSPR) providing a broad range of applications in nanophotonic devices and sensors. A hybrid material platform combining the unique multifunctional 2D layered oxides and plasmonic nanostructures brings optical tuning into the new level. Here, a novel self-assembled Bi 2 MoO 6 (BMO) 2D layered oxide incorporated with plasmonic Au nanoinclusions has been demonstrated via one-step pulsed laser deposition (PLD) technique. Comprehensive microstructural characterizations, including scanning transmission electron microscopy (STEM), differential phase contrast imaging (DPC), and STEM tomography, have demonstrated the high epitaxial quality and particle-in-matrix morphology of the BMO-Au nanocomposite film. DPC-STEM imaging clarifies the magnetic domain structures of BMO matrix. Three different BMO structures including layered supercell (LSC) and superlattices have been revealed which is attributed to the variable strain states throughout the BMO-Au film. Owing to the combination of plasmonic Au and layered structure of BMO, the nanocomposite film exhibits a typical LSPR in visible wavelength region and strong anisotropy in terms of its optical and ferromagnetic properties. This study opens a new avenue for developing novel 2D layered complex oxides incorporated with plasmonic metal or semiconductor phases showing great potential for applications in multifunctional nanoelectronics devices.

36 MATERIALS SCIENCE↗

Mass production of high-performance single atomic FeNC electrocatalysts via sequenced ultrasonic atomization and pyrolysis process

Mass production of highly efficient, durable, and inexpensive single atomic catalysts is currently the major challenge associated with the oxygen reduction reaction (ORR) for fuel cells. In this study, we develop a general strategy that uses a simple ultrasonic atomization coupling with pyrolysis and calcination process to synthesize single atomic FeNC catalysts (FeNC SACs) at large scale. The microstructure characterizations confirm that the active centers root in the single atomic Fe sites chelating to the four-fold pyridinic N atoms. The identified specific Fe active sites with the variable valence states facilitate the transfer of electrons, endowing the FeNC SACs with excellent electrochemical ORR activity. The FeNC SACs were used as cathode catalysts in a homemade Zn-air battery, giving an open-circuit voltage (OCV) of 1.43 V, which is substantially higher than that of commercial Pt/C catalysts. This study provides a simple approach to the synthesis of single atomic catalysts at large scale.

36 MATERIALS SCIENCE↗

Crystallographic orientation and spatially resolved damage in a dispersion-hardened Al alloy

The in-situ neutron diffraction technique, in combination with both the full-field crystal elasto-viscoplastic finite element model and microstructural characterization, was used to study the deformation-induced damage anisotropy in a commercial Al alloy, subjected to uniaxial tensile and cyclic loading. The simulations capture well the crystallographic-orientation-dependent lattice strain behavior. The hard grains, e.g. those orientated with the <111> and <422> orientations parallel with the uniaxial loading direction (LD), feature large Taylor factors and seem more prone to form damage-related band structures. Their effective elastic moduli decrease with the accumulation of damage, which are different from the soft grains orientated with the <200> orientation along the LD. Correlation between the distribution of voids and that of the residual lattice strain developed after failure may exist. The maximum tensile type residual lattice strain observed after failure may be resulted from the band structure formed in the hardest <111> grains. It was revealed that the band structure triggered by the hard particles could be one of sources of damage. In addition, while the specimen was obviously damaged, a fast stress relief was evidenced after unloading from the tension, especially at the beginning of unloading. Our present investigations provide a novel method for exploring the damage mechanisms of polycrystalline materials during plastic deformation.

36 MATERIALS SCIENCE↗

Microstructure and high temperature tensile properties of 316L fabricated by laser powder-bed fusion

316L stainless steel fabricated by laser powder-bed fusion (LPBF) has attracted significant attention due to a unique combination of strength and ductility at room temperature. Understanding of high temperature tensile properties of LPBF fabricated 316L is, however, limited. In the present investigation, tensile testing was conducted at 20–700ºC on LPBF 316L in as printed condition and after annealing for 5 h at 500–800ºC. Room temperature data confirmed the excellent ductility of the LPBF-processed 316L steel due to the cellular structure with high dislocation density. However, a significant decrease in ductility was observed at temperatures above 200ºC. These results are consistent with a change of deformation mechanisms observed in wrought 316L, with twinning playing a key role at room temperature. Finally, microstructure characterization and tensile testing revealed that the cellular structure is stable up to 500ºC, but a decrease of yield strength was observed at temperatures above 600ºC likely due to a decrease in dislocation density via annealing.

36 MATERIALS SCIENCE↗

Predicting phase transformation kinetics during metal additive manufacturing using non-isothermal Johnson-Mehl-Avrami models: Application to Inconel 718 and Ti-6Al-4V

Here, a computational model was developed to predict solid-state phase transformation kinetics within mechanical parts during metal additive manufacturing processes. This model is a modified version of the Johnson-Mehl-Avrami model for non-isothermal phase transformations that can be applied to various material systems undergoing solid-state phase transformations. Using the thermal history of an additive manufacturing fabricated mechanical part, along with the necessary thermodynamic data and kinetic information as inputs, the model outputs the history of phase fraction evolution during the build process. The model was applied to an Inconel 718 part built by powder bed fusion and a Ti-6Al-4V part built by directed energy deposition. Microstructure characterization and mechanical testing were performed for the validation of the model.

36 MATERIALS SCIENCE↗

Interpretation of wide-angle x-ray diffraction patterns from mesophase pitch-based carbon fibers – a simulation and experimental study

Carbon fiber is a critical material in a wide range of industries, where it is highly valued for its high specific strength/stiffness, excellent wear resistance, efficient electrical and thermal transport properties, chemical resistance, and low coefficient of thermal expansion. The properties of a specific carbon fiber are closely tied to its structural characteristics at all length scales. Here, in this work, we applied wide-angle x-ray diffraction to a set of heat-treated mesophase pitch-based carbon fibers, with the goal of elucidating the crystalline structures as a function of fiber orientation. To assist with analysis and interpretation of the experimental data, we employed diffraction pattern simulations using the scalar and vector forms of the Debye scattering equation to determine the influence of basal plane orientation, crystalline ordering (turbostratic-graphitic), and basal plane asymmetry on the diffraction patterns. The results presented here suggest that growth of the transverse crystallites in mesophase pitch-based carbon fiber is fixed until graphitization temperatures are reached. The work completed here provides a framework for the analysis of carbon fiber and other oriented carbon-based materials via diffraction.

36 MATERIALS SCIENCE↗

Ce post-treatment for increased corrosion resistance of AA2024-T3 anodized in tartaric-sulfuric acid

Here, the effect of a post-treatment for short time in 50 mM Ce(NO 3 ) 3 solution, with or without H 2 O 2 , on the corrosion of AA2024-T3 anodized in tartaric-sulfuric acid was investigated. Electrochemical (EIS, polarization curves) and corrosion (immersion) tests showed improved performance for samples post-treated at 50 °C in the H 2 O 2 containing solution. Microstructural characterization (SEM, STEM, GDOES) evidenced the presence of Ce oxyhydroxides both at the surface and within the pores of the anodized layer, and their preferential interaction with defective sites both at micro and nanoscale. Important amounts of Ce-species were found near corrosion products, indicating active corrosion protection by Ce ions.

36 MATERIALS SCIENCE↗

Bridging microscale to macroscale mechanical property measurements of FeCrAl alloys by crystal plasticity modeling

FeCrAl alloys are candidates for accident tolerant fuel cladding of light water reactors. In this work, a microstructure- and temperature-dependent crystal plasticity model is employed to bridge microscale to macroscale mechanical property measurements of FeCrAl alloys. With the visco-plastic self-consistent (VPSC) polycrystal plasticity framework, a mechanism-based single crystal plasticity (MSCP) model adopts the Arrhenius type rate equation to describe the dependence of the critical resolved shear stress for dislocation slips on their temperature-dependent intrinsic frictional resistance and the microstructure-dependent irradiation hardening. The intrinsic frictional resistance associated with {110}<111> and {112}<111> slip systems were measured by in-situ micromechanical testing on unirradiated/irradiated samples at 25-500 °C. The irradiation hardening is estimated by the Bacon-Kocks-Scattergood (BKS) model with density and size of radiation-induced defects measured from microstructural characterization. Several features associated with thermo-mechanical behavior of unirradiated/irradiated polycrystalline FeCrAl alloys are captured. High density of deformation-induced dislocations and radiation-induced defects results in obvious hardening at room temperature, which is weakened at high temperature, and facilitates damage evolution during deformation. Moreover, both high temperature and radiation-induced defects, which facilitate dislocation multiplication, trigger large hardening rate. Finally, the proposed method together with application of accelerator-based ion irradiation technique is a surrogate approach to simulate neutron damage, improving the efficiency associated with evaluation of mechanical properties of FeCrAl alloys exposed to temperature, stress and radiation conditions.

36 MATERIALS SCIENCE↗

High hardness and oxidation-resistant Cr-containing medium entropy ZrTaW diboride

This study reports the successful synthesis of a Cr-containing (Zr 0.30 Ta 0.34 Cr 0.06 W 0.30 )B 2 medium-entropy boride (MEB) via an in-situ reactive borothermal reduction route from oxide precursors. High-energy ball milling was employed to homogenize the precursor mixture prior to reactive densification. X-ray diffraction confirmed the formation of a predominantly AlB₂-type hexagonal diboride structure together with a secondary (W X , M 1-X )B monoboride phase. Microstructural characterization revealed compositional heterogeneity and localized W-rich regions associated with the secondary phase. The synthesized medium-entropy boride exhibited enhanced mechanical properties, which are attributed to lattice distortion and solid-solution strengthening effects. Thermogravimetric analysis revealed complex multistage oxidation behavior, and the oxidation resistance was compared with conventional ultra-high-temperature diborides. The results demonstrate the strong relationship between oxide-derived processing, compositional complexity, phase evolution, and oxidation behavior, highlighting the potential of medium-entropy borides for high-temperature structural applications

36 MATERIALS SCIENCE↗

Characterization of fusion welded ceramics in the SiC-ZrB 2 -ZrC system

Various SiC-ZrB 2 -ZrC ceramics were joined by fusion welding to determine the maximum silicon carbide content that could be joined. Commercial powders were hot pressed, machined, and preheated to 1450 °C before joining with a tungsten inert gas welding torch at 160–200 A. Resulting welds were cross-sectioned and analyzed to determine which compositions were weldable and to characterize microstructural evolution in welded samples. As compositions approached the ternary eutectic, the welds had smaller SiC grains and exhibited better weldability. Penetration depth of welds was controlled by a combination of current input and welding speed. Here, the ternary eutectic in the system was found at 36.9 ± 1.3 vol% SiC, 42.7 ± 1.5 vol% ZrB 2 , and 20.4 ± 1.9 vol% ZrC and its melting temperature was 2330 ± 23 °C. A ternary phase diagram for the SiC-ZrB 2 -ZrC was constructed and proposed via microstructural analysis of arc melted pellets on binary joins between each binary eutectic and the ternary eutectic in the system.

36 MATERIALS SCIENCE↗

Evaluating the bond strength and fracture mechanisms of cold-sprayed zinc coating on AZ91 magnesium substrate via a combined experimental and computational approach

Magnesium (Mg) alloys are ideal candidates for automotive applications due to their high strength to weight ratio, castability, recyclability etc., however, they lack corrosion and oxidation resistance. Solid-state deposition techniques, such as cold spray, have been demonstrated to enhance their corrosion resistance as it relies on the severe plastic deformation of powder particles upon impact with the substrate to form a metallurgical bond with the substrate and within the coating. At cold sprayed interfaces, a heterogeneous microstructure is formed that includes some porosity, oxides and intermetallics which can significantly affect coating performance. Thus, establishing a direct correlation between the interface microstructure and its properties can aid in designing optimal cold spray parameters. In this study, we investigated the microstructure and mechanical properties of a zinc (Zn) coating deposited on a high pressure die cast (HPDC) AZ91 Mg substrate via high resolution scanning transmission electron microscopy, in situ micro-tensile testing, and finite element method (FEM) modeling. Micro-tensile pillars fabricated using the plasma focused ion beam (PFIB) successfully isolates the coating-substrate interface within the gauge length. The average bond strength of Zn-Mg interface was determined to be ∼140 MPa with failure occurring partially at the interface and mostly into the coatings. A detailed microstructural characterization revealed evidence of a strong metallurgical bonding at the Zn-Mg interface and formation of the C14 MgZn 2 laves phase interlayer resulting in a mixed mode of fracture during the micro-tensile experiments. FEM modeling reveals the stress distribution along the interfaces and suggests that a MgZn 2 layer thickness between 200–400 nm is optimum to increase the bond strength and minimize the triaxiality. Such a site-specific interfacial analysis with correlative computational modeling provides crucial insight into the overall performance of cold spray interfaces.

Bond strength↗

Interfacial characteristics of P91 steel - Inconel 740H bimetallic structure fabricated using wire-arc additive manufacturing

Although bimetallic structures can offer unique solutions to engineering problems with varying functionality, joining two dissimilar alloys using additive manufacturing involves challenges such as cracking and segregation. In this work, bimetallic structures of Inconel 740H superalloy and P91 steel are processed using wire-arc additive manufacturing (WAAM) for the first time. P91 steel is directly deposited over 740H with a cooling time of 20 minutes in between the two depositions. During microstructure characterization, a large gradient zone with coarse grains spanning for ~2200 μm is observed. Moreover, the microhardness of the gradient zone is the least in comparison with the P91 and 740H deposits. No deleterious phase formation is found; however, intergranular cracks are observed along the gradient zone. In order to deduce the reason for cracking, non-equilibrium solidification simulations are performed for the mixed compositions of P91 and 740H in the gradient zone. Here, the reasons for crack formation in the gradient zone are the sudden change in the volumetric coefficient of thermal expansion due to the formation of MC carbides as well as the development of local strains from the thermal residual stresses. Therefore, altering the deposition sequence and introducing gradient layers with mixed composition between the P91 and 740H deposits will be beneficial in achieving defect-free builds. Through the integration of experiments and simulation, this work gains valuable insights into the processability of dissimilar alloy manufacturing using the WAAM technique.

20 FOSSIL-FUELED POWER PLANTS↗

Radiation response of FeCrAl-coated Zircaloy-4

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.

36 MATERIALS SCIENCE↗

Thermal conductivity measurement of the interaction layer between UMo and Al produced by high-energy heavy ion irradiation

In this work, we report the first direct thermal conductivity measurement results for Al-UMo interaction layer (IL), which is typically observed in UMo/Al dispersion fuel plates under irradiation. The investigated IL was formed by irradiating Al coated UMo substrate using 80 MeV iodine ions at 180 degrees C up to 3.03 x 10 17 ions/cm 2 fluence. Microstructural characterization indicated that the induced IL is amorphous with an approximately (U 0.8 ,Mo 0.2 )Al 5.3 stoichiometry, which is similar to that formed under in-pile irradiation. Focused ion beam (FIB) was used to prepare nine specimens of various lengths from the IL that could be suspended across a microfabricated device for thermal conductivity measurement. The measured thermal conductivity values of the IL were significantly lower than the values for both the original UMo fuel and the Al. The successful measurement of the Al-UMo IL provides valuable information for the development and qualification of UMo/Al dispersion fuels for research and test reactor conversion applications, and further demonstrates the promising capabilities of utilizing the suspended bridge method in nuclear fuel research.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Postirradiation examination from separate effects irradiation testing of uranium nitride kernels and coated particles

An overview of postirradiation examination results for uranium nitride kernels and uranium nitride coated particles irradiated in the High Flux Isotope Reactor are presented. This is the first postirradiation examination of the MiniFuel irradiation vehicle that was recently developed to rapidly accumulate burnup during separate effects irradiation testing. In general, the burnup and fuel temperatures measured postirradiation were consistent with the design calculations. The burnup measured by mass spectrometry ranged from 5.9 to 10 MWd/kgU and was achieved after only 68 effective full-power days of irradiation. The dilatometric evaluation of passive silicon carbide thermometry indicated that the fuel was irradiated at temperatures ranging from 410 to 460 °C. Because the irradiation temperatures and burnup were low, the UN kernels showed minimal fission gas release that was within the range of the expected recoil (athermal) release. While it is possible to measure fuel swelling using x-ray computed tomography, the observed swelling was too small to quantify in this case. Extensive microstructural characterization of the irradiated fuel was performed in this study, and no significant irradiation induced changes were observed.

36 MATERIALS SCIENCE↗