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All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Microstructure and Chemical Composition of Al2O3-, Cr2O3- and MgO-rich Refractories Exposed to Plastic Ashes

Plastics are widely integrated with today’s lifestyle due to their low cost, durability, lightweight, water resistance, and flexibility. However, tremendous plastic waste cause severe threats to the environment. Thus, sustainable recycling of plastic waste is critical, where plastic waste gasification technology with carbon management becomes one of the most effective recycling methods. We simulate the gasification process by exposing the Al2O3-, Cr2O3- and MgO-rich refractories to synthetic plastic ashes at 1500 ℃ for 50 h. A comprehensive study on the microstructure and chemical composition change before/after exposure is conducted using scanning electron microscopy. Meanwhile, the differences among these three refractories after exposure are revealed for quantifying the performance in plastic ashes. Discussion of the results will establish an understanding of the influence of plastic ashes on the microstructure, composition, and phase of different types of refractories, providing insights into designing new refractory materials for future recycling of plastic waste.

Fang, Xiaotian↗
DOE OSTI2013

Pulsed Magnetic Welding for Advanced Core and Cladding Steel

To investigate a solid-state joining method, pulsed magnetic welding (PMW), for welding the advanced core and cladding steels to be used in Generation IV systems, with a specific application for fuel pin end-plug welding. As another alternative solid state welding technique, pulsed magnetic welding (PMW) has not been extensively explored on the advanced steels. The resultant weld can be free from microstructure defects (pores, non-metallic inclusions, segregation of alloying elements). More specifically, the following objectives are to be achieved: 1. To design a suitable welding apparatus fixture, and optimize welding parameters for repeatable and acceptable joining of the fuel pin end-plug. The welding will be evaluated using tensile tests for lap joint weldments and helium leak tests for the fuel pin end-plug; 2 Investigate the microstructural and mechanical properties changes in PMW weldments of proposed advanced core and cladding alloys; 3. Simulate the irradiation effects on the PWM weldments using ion irradiation.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗
NASA NTRS2014

Electron Beam Freeform Fabrication of Titanium Alloy Gradient Structures

Historically, the structural optimization of aerospace components has been done through geometric methods. A monolithic material is chosen based on the best compromise between the competing design limiting criteria. Then the structure is geometrically optimized to give the best overall performance using the single material chosen. Functionally graded materials offer the potential to further improve structural efficiency by allowing the material composition and/or microstructural features to spatially vary within a single structure. Thus, local properties could be tailored to the local design limiting criteria. Additive manufacturing techniques enable the fabrication of such graded materials and structures. This paper presents the results of a graded material study using two titanium alloys processed using electron beam freeform fabrication, an additive manufacturing process. The results show that the two alloys uniformly mix at various ratios and the resultant static tensile properties of the mixed alloys behave according to rule-of-mixtures. Additionally, the crack growth behavior across an abrupt change from one alloy to the other shows no discontinuity and the crack smoothly transitions from one crack growth regime into another.

Brice, Craig A.↗
DOE OSTI2014

Catalyst by Design

The development of new catalytic materials is still dominated by trial and error methods. Although it has been successful, the empirical development of catalytic materials is time consuming and expensive with no guarantee of success. In our laboratories, we are developing a comprehensive catalysts by design that involves state-of-the-art first principle density functional theory calculations, experimental design of catalyst sites, and sub- ngstr m resolution imaging with an aberration-corrected electron microscope to characterize the microstructure. In this chapter, we focus on supported platinum cluster catalyst systems which are one of the most important industrial catalysts and attempt to demonstrate the feasibility of the catalyst by design concept.

catalysis↗
DOE OSTI2018

Enhancing workability in sheet production of high silicon content electrical steel through large shear deformation

Enhanced workability, as characterized by the magnitude and heterogeneity of accommodated plastic strains during sheet processing, is demonstrated in high Si content Fe-Si alloys containing 4 and 6.5 wt% Si using two single-step, simple-shear deformation techniques – peeling and large strain extrusion machining (LSEM). The model Fe-Si material system was selected for its intrinsically poor material workability, and well-known applications potential in next-generation electric machines. In a comparative study of the deformation characteristics of the shear processes with conventional rolling, two distinct manifestations of workability are observed. For rolling, the relatively diffuse and unconfined deformation zone geometry leads to cracking at low strains, with sheet structures characterized by extensive deformation twinning and banding. Workpiece pre-heating is required to improve the workability in rolling. In contrast, peeling and LSEM produce continuous sheet at large plastic strains without cracking, the result of more confined deformation geometries that enhances the workability. Peeling, however, results in heterogeneous, shear-banded microstructures, pointing to a second type of workability issue – flow localization – that limits sheet processing. This shear banding is to a large extent facilitated by unrestricted flow at the sheet surface, unavoidable in peeling. With additional confinement of this free surface deformation and appropriately designed deformation zone geometry, LSEM is shown to suppress shear banding, resulting in continuous sheet with homogeneous microstructure. Thus LSEM is shown to produce the greatest enhancement in process workability for producing sheet. In conclusion, these workability findings are explained and discussed based on differences in process mechanics and deformation zone geometry.

36 MATERIALS SCIENCE↗
NASA NTRS1987

A 2000-hour cyclic endurance test of a laboratory model multipropellant resistojet

The technological readiness of a long-life multipropellant resistojet for space station auxiliary propulsion is demonstrated. A laboratory model resistojet made from grain-stabilized platinum served as a test bed to evaluate the design characteristics, fabrication methods, and operating strategies for an engineering model multipropellant resistojet developed under contract by the Rocketdyne Division of Rockwell International and Technion Incorporated. The laboratory model thruster was subjected to a 2000-hr, 2400-thermal-cycle endurance test using carbon dioxide propellant. Maximum thruster temperatures were approximately 1400 C. The post-test analyses of the laboratory model thruster included an investigation of component microstructures. Significant observations from the laboratory model thruster are discussed as they relate to the design of the engineering model thruster.

Morren, W. Earl↗
NASA NTRS1987

2000-hour cyclic endurance test of a laboratory model multipropellant resistojet

The technological readiness of a long-life multipropellant resistojet for space station auxiliary propulsion is demonstrated. A laboratory model resistojet made from grain-stabilized platinum served as a test bed to evaluate the design characteristics, fabrication methods, and operating strategies for an engineering model multipropellant resistojet developed under contract by the Rocketdyne Division of Rockwell International and Technion Incorporated. The laboratory model thruster was subjected to a 2000-hr, 2400-thermal-cycle endurance test using carbon dioxide propellant. Maximum thruster temperatures were approximately 1400 C. The post-test analyses of the laboratory model thruster included an investigation of component microstructures. Significant observations from the laboratory model thruster are discussed as they relate to the design of the engineering model thruster.

Morren, W. Earl↗
DOE OSTI2022

ExaAM: Metal additive manufacturing simulation at the fidelity of the microstructure

Additive manufacturing (AM), or 3D printing, of metals is transforming the fabrication of components, in part by dramatically expanding the design space, allowing optimization of shape and topology. However, although the physical processes involved in AM are similar to those of welding, a field with decades of experimental, modeling, simulation, and characterization experience, qualification of AM parts remains a challenge. The availability of exascale computational systems, particularly when combined with data-driven approaches such as machine learning, enables topology and shape optimization as well as accelerated qualification by providing process-aware, locally accurate microstructure and mechanical property models. We describe the physics components comprising the Exascale Additive Manufacturing simulation environment and report progress using highly resolved melt pool simulations to inform part-scale finite element thermomechanics simulations, drive microstructure evolution, and determine constitutive mechanical property relationships based on those microstructures using polycrystal plasticity. We report on implementation of these components for exascale computing architectures, as well as the multi-stage simulation workflow that provides a unique high-fidelity model of process–structure–property relationships for AM parts. In addition, we discuss verification and validation through collaboration with efforts such as AM-Bench, a set of benchmark test problems under development by a team led by the National Institute of Standards and Technology.

3D printing↗
DOE OSTI2020

Enabling high rate capability, low internal resistance, and excellent cyclability for vanadium redox flow batteries utilizing ultrafast laser-structured graphite felt

The electrochemical performance of vanadium redox flow batteries (VRFBs) was enhanced via laser-patterned graphite felt (GF) electrodes. The laser-structured GF electrodes engineered via preparing a series of well-ordered microscopic channel structures with an average width of 200 μm, creating a three-dimensional carbon framework. The ultrafast laser patterning increased the porosity by 10%, as compared to pristine electrode. The analysis of the overpotential distribution using electrochemical impedance spectroscopy revealed that the electrode polarization involving charge transfer and diffusion resistance is strongly alleviated with the aid of carbon micro-perforation. The advanced design of laser-structured GF electrode also exhibits high rate capability, low internal resistance, and excellent cyclability. The improved performance was attributed to the synergistic effect involving (i) high electrochemically active surface area for rapid electrochemical reactions (i.e., V(II)/V(III) and V(IV)/V(V) redox couples) and (ii) excellent transport properties for facile electron/ion/species transport. The micro-scale channels created with the laser-ablation technique act as capillary structures and enabled homogeneous and rapid wetting of GF electrodes as formulated with the classical Washburn equation. The VRFB equipped with the laser-structured GF electrodes delivered a high discharge capacity with exceptional capacity retention upon extended cycling (>84.9%). In conclusion, accordingly, the design of laser-structured electrode paves the pathway towards finely tuning the electrode internal microstructure for improved cyclability, durability, and capacity retention in various electrochemical energy storage/conversion devices (e.g. all-vanadium redox flow batteries).

25 ENERGY STORAGE↗
NASA NTRS2015

Ultra High Temperature (UHT) SiC Fiber (Phase 2)

Silicon-carbide fiber-reinforced silicon-carbide ceramic matrix composites (SiCSiC CMC) are emerginglightweight re-usable structural materials not only for hot section components in gas turbine engines, but also for controlsurfaces and leading edges of reusable hypersonic vehicles as well as for nuclear propulsion and reactor components. Ithas been shown that when these CMC are employed in engine hot-section components, the higher the upper usetemperature (UUT) of the SiC fiber, the more performance benefits are accrued, such as higher operating temperatures,reduced component cooling air, reduced fuel consumption, and reduced emissions. The first generation of SiCSiC CMC with a temperature capability of 2200-2400F are on the verge of being introduced into the hot-section components ofcommercial and military gas turbine engines.Today the SiC fiber type currently recognized as the worlds best in terms ofthermo-mechanical performance is the Sylramic-iBN fiber. This fiber was previously developed by the PI at NASA GRC using patented processes to improve the high-cost commercial Sylramic fiber, which in turn was derived from anotherlow-cost low-performance commercial fiber. Although the Sylramic-iBN fiber shows state-of-the art creep and rupture resistance for use temperatures above 2550oF, NASA has shown by fundamental creep studies and model developmentthat its microstructure and creep resistance could theoretically be significantly improved to produce an Ultra HighTemperature (UHT) SiC fiber.This Phase II Seedling Fund effort has been focused on the key objective of effectively repeating the similar processes used for producing the Sylramic-iBN fiber using a design of experiments approach to first understand the cause of the less than optimum Sylramic-iBN microstructure and then attempting to develop processconditions that eliminate or minimize these key microstructural issues. In so doing, it is predicted that that theseadvanced process could result in an UHT SiC fiber with 20 times more creep resistance than the Sylramic-iBN fiber,which in turn would allow SiCSiC CMC to operate up to 2700oF and above, thereby further enhancing the performancebenefits of SiCSiC components in aero-propulsion engines. It was also envisioned that the fiber processes developedduring Phase II efforts would not only reduce production costs for the UHT fiber by using low-cost precursor fibers andcombined processes, but also allow the UHT fibers to be directly produced in preforms of the precursor fibers, possibly atthe facilities of the CMC fabricator.

SiC Ceramic Fiber↗
DOE OSTI2021

Development of Corrosion- and Erosion-Resistant Coatings for Advanced Ultra-Supercritical Materials

This final report summarized the research efforts and major findings of the Phase I Project “Development of Corrosion- and Erosion-Resistant Coatings for Advanced Ultra-Supercritical Materials”, for the period of October 1, 2019 – Sept. 30, 2021. This project is a collaborative endeavor between Tennessee Tech University, Purdue University, Oak Ridge National Laboratory, Siemens Corporation, and Eastern Plating, LLC, aiming at improving the durability and lifetime of high-pressure (HP) steam turbine blades in advanced ultra-supercritical (A-USC) coal-fired power plants through the development of corrosion/erosion-resistant coatings manufactured via a low-cost electrolytic codeposition process. While Tribaloy alloy T-400C was identified by the U.S. A-USC Materials Consortium as a promising coating composition, further composition optimization is needed to enhance its corrosion and erosion resistance for protecting the A-USC Ni-base turbine components. An integrated computational and experimental approach was employed to optimize coating composition/microstructure and processing parameters. In order to identify candidate coating compositions that could offer balanced properties, thermodynamic calculations were performed to explore the γ+Laves composition space in the Co-Ni-Cr-Mo-Si system with different alloying additions at 600-800 °C. Guided by the calculation results, experimental assessment of selected alloys led to the development of a new generation of Tribaloy compositions with the optimal levels of Cr, Mo and Si, reactive element (e.g., 0.4-0.6 wt.% Y) and other alloying additions. The low-cost and non-line-of-sight electro-codeposition process was employed to deposit a Ni(Co)-CrMoSiY composite coating on commercial Haynes 282 (H282) Ni-base alloy. A diffusion treatment was subsequently applied to convert the composite to the Tribaloy-type coating. Both the codeposition parameters and heat treatment conditions were varied to achieve the desired coating composition, microstructure and phase constituents. In addition, since additive manufacturing (AM) may be an alternative cost-saving option for potential A-USC turbine repair, laser direct deposition was explored to fabricate the H282 alloy with minimal defects. The electro-codeposited Tribaloy coating was also applied to the AM H282 substrate to demonstrate the viability of the coating process in improving the surface finish of AM alloys. Both high-temperature oxidation performance and solid particle erosion (SPE) resistance of model alloys and electro-codeposited coatings were evaluated. About 25 model alloys with various Cr/Mo ratios and reactive element levels, as well as partial substitution of Mo with Nb were evaluated with regard to their oxidation resistance in both air and pure steam at 760-800°C. Compositions based on Ni(Co)-20Cr-18Mo-2.6Si-0.6Y (wt.%) showed significantly improved oxidation resistance over the baseline T400-C. Based on the alloy development results, three generations of new Tribaloy coatings (Gen-1, Gen-2, and Gen-3) with various Mo/Cr contents and Y levels were prepared via electro-codeposition and their microstructure/performance were evaluated. Outstanding air and steam oxidation resistance was achieved for the Gen-2 and Gen-3 coatings. Furthermore, while the SPE resistance of the coatings depended on many factors such as temperature, environment, erodent, velocity and impact angle, the coated samples exhibited similar or better SPE resistance compared to the H282 substrate when magnetite was used as erodent (which is a realistic erodent in A-USC steam turbines). The new Tribaloy coatings also had good long-term compatibility with the H282 alloy substrate. The two large-sized rotating barrels were designed, constructed, and employed to coat dummy HP blades. Uniform coating thickness and microstructure were achieved at various blade locations. Also, a preliminary techno-economic analysis of the proposed coating process was conducted to quantify the cost-effectiveness and to assess the commercial viability of the corrosion- and erosion-resistant coatings. It is estimated that a cost reduction of ~30% could be achieved with the electro-codeposition coating process over the state-of-the-art high velocity oxygen fuel (HVOF) thermal spray. Compared to the leading Tribaloy coating technologies such as HVOF and plasma transfer alloying, electro-codeposition based process has advantages such as low-cost process equipment, uniform deposition even for complex shapes, low levels of contaminants/porosities, reduction of powder waste, and potentially better surface finish and longer turbine service life. The Phase 1 study has demonstrated that it is feasible to develop an electro-codeposited Tribaloy coating with balanced corrosion and erosion properties, even though additional research efforts such as further coating process scale-up and longer-term performance evaluation under realistic A-USC conditions are clearly needed.

20 FOSSIL-FUELED POWER PLANTS↗
NASA NTRS2003

Robust Joining and Assembly of Ceramic Matrix Composites for High Temperature Applications

Advanced ceramic matrix composites (CMCs) are under active consideration for use in a wide variety of high temperature applications within the aerospace, energy, and nuclear industries. The engineering designs of CMC components require fabrication and manufacturing of large and complex shaped parts of various thicknesses. In many instances, it is more economical to build up complex shapes by joining simple geometrical shapes. Thus, joining and attachment have been recognized as enabling technologies for successful utilization of ceramic components in various demanding applications. In this presentation, various challenges and opportunities in design, fabrication, and testing of high temperature joints in ceramic matrix composites will be presented. A wide variety of ceramic composites, in different shapes and sizes, have been joined using an affordable, robust ceramic joining technology (ARCJoinT). Microstructure and mechanical properties of joints in melt infiltrated and CVI Sic matrix composites will be reported. Various joint design philosophies and design issues in joining of composites will be discussed.

Singh, Mrityunjay↗
DOE OSTI2025

SEM/EBSD Characterization of Baffle-Former Bolts Designated for High Energy X-ray Microscopy Studies at the Advanced Photon Source

This report documents the microstructural and surface characterization of two high-fluence baffle-former bolts (BFBs) harvested from a commercial pressurized water reactor (PWR) after nearly four decades of service. These bolts experienced extreme conditions including high neutron fluence, elevated temperatures, corrosive primary water, and sustained mechanical loads, all of which contribute to degradation mechanisms such as irradiation-assisted stress corrosion cracking (IASCC). Using scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD), the study assessed bulk and near-surface microstructures, grain boundary characteristics, and in-service oxide layers. The results revealed significant differences between bolts exposed to 41 dpa and 29 dpa, including differences in recrystallization extent, deformation structures, and oxidation morphology. These findings establish critical baseline data for integration with advanced synchrotron-based high-energy X-ray microscopy (HEXM) and computational crystal plasticity models. Ultimately, the work supports improved mechanistic understanding and predictive capability regarding the long-term performance of reactor core internal components.

Lach, Tim [Oak Ridge National Laboratory (ORNL), O↗
DOE OSTI2018

Effect of Eu/Ca ratio on the crystalline phase, morphology and luminescent properties of Ca2-1.5xEux(MoO4)2 (0 ≤ x ≤ 4/3) ceramics phosphors

Highlights: • Novel Ca{sub 2-1.5x}Eu{sub x}(MoO{sub 4}){sub 2} red phosphors have been proposed and fabricated. • The correlations between the microstructure and PL have been investigated. • This work may provide a guidance to design for molybdate phosphors. - Abstract: A series of Ca{sub 2-1.5x}Eu{sub x}(MoO{sub 4}){sub 2} (0 ≤ x ≤ 4/3) phosphors have been fabricated by a traditional solid-state reaction. The correlations between the crystal structure, luminescent properties and surface morphologies with the chemical composition of the as-fabricated Ca{sub 2-1.5x}Eu{sub x}(MoO{sub 4}){sub 2} crystals have been investigated in detail. The results show that the Ca{sub 2-1.5x}Eu{sub x}(MoO{sub 4}){sub 2} (0 ≤ x ≤ 1.3) phosphors possess tetragonal phase, whereas the obtained Ca{sub 2-1.5x}Eu{sub x}(MoO{sub 4}){sub 2} (x = 4/3) (i.e. Eu{sub 2}(MoO{sub 4}){sub 3}) phosphor exhibits monoclinic phase. The morphologies of crystals change gradually from quasi sphericity to tetragonal bipyramid owing to the preferential growth along c-axis induced by Eu{sup 3+} ions. The photoluminescence spectra reveal that the intensities of the characteristic emission and excitation peaks initially increase and then decrease with increasing x, given the maximum at x = 1/3. Our results indicate that the difference in the charge, electronegativity, as well as ionic radius between Ca{sup 2+} ions and Eu{sup 3+} ions lead to the variation of crystal symmetry, crystal phase, surface morphologies and luminescence of the final Ca{sub 2-1.5x}Eu{sub x}(MoO{sub 4}){sub 2} crystals.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2020

MEUMAPPS (Microstructure Evolution Using Massively Parallel Phase-field Simulations)

The software “MEUMAPPS” is a h high-performance computing code used to simulate microstructure evolution associated with diffusional solid-state transformations in structural alloys. Understanding microstructure evolution during thermo-mechanical processing of structural alloys is the first step towards designing and processing alloys for specific applications by meeting property requirements demanded by the application. In this instance, the code is an important component in predicting processing-structure linkages during additive manufacturing of structural alloys as a function of processing parameters and alloy composition used in an additive manufacturing process. The code provides a detailed three-dimensional distribution of different types of phases / constituents and their morphologies, as well as the compositions of these phases that make up the microstructure. The microstructure is simulated by solving the governing partial differential equations using a Fourier Spectral Method.

Radhakrishnan, Balasubram↗
DOE OSTI2017

Rafting and elastoplastic deformation of superalloys studied by neutron diffraction

The rafting of monocrystalline Ni- and Co-based superalloys has been studied by neutron diffractometry. Lattice parameter misfit values and the difference in phase stiffnesses at room temperature, 650 °C, and 900 °C are presented. These microstructural parameters should assist in refining computer models that aim to predict precipitate evolution in superalloys and aid future alloy design. The nature of rafting is shown experimentally to be dependent upon the lattice parameter misfit. The 900 °C yield strength of the γ-phase of the Co-based superalloy with a rafted microstructure occurs at ~100 MPa, when loaded at a low strain rate.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Integrated Multiscale Model for Design of Robust 3D Solid-state Lithium Batteries

In FY23, we successfully established the multiscale modeling framework for probing the effects of materials microstructure on cell performance of 3D solid-state batteries. The framework covers physicochemical processes co-evolving at the atomistic and microstructure scales. Our simulations revealed the mechanism of initial interfacial degradation, formation of secondary phases, and the structure-property relationship for ion transport and mechanical stability at the interface. In addition, we also established the microstructure-performance relationships by performing sensitivity tests of various microstructure features and extracting their impact on cell performance during charge-discharge cycles. We have successfully applied our multiscale, multiphysics modeling capability to common electrode and electrolyte materials that are of interests to VTO and the experimental teams within the US-Germany collaboration. The insights we obtained from these simulations provide valuable design principles to optimize materials properties for advanced 3D solid-state batteries.

25 ENERGY STORAGE↗
DOE OSTI2013

Yield asymmetry design of magnesium alloys by integrated computational materials engineering

Deformation asymmetry of magnesium alloys is an important factor on machine design in the automobile industry. Represented by the ratio of compressive yield stress (CYS) against tensile yield stress (TYS), deformation asymmetry is strongly related to texture and grain size. A polycrystalline viscoplasticity model, modified intermediate Φ-model, is used to predict the deformation behavior of magnesium alloys with different grain sizes. Validated with experimental results, integrated computational materials engineering is applied to find out the route in achieving desired asymmetry via thermomechanical processing. For example, CYS/TYS in rolled texture is smaller than 1 under different loading directions. In other textures, such as extruded texture, CYS/TYS is large along the normal direction. Starting from rolled texture, asymmetry will increase to close to 1 along the rolling direction after being compressed to a strain of 0.2. Our modified Φ-model also shows that grain refinement increases CYS/TYS. Along with texture control, grain refinement also can optimize the yield asymmetry. After the grain size decreases to a critical value, CYS/TYS reaches to 1 because CYS increases much faster than TYS. By tailoring the microstructure using texture control and grain refinement, it is achievable to optimize yield asymmetry in wrought magnesium alloys.

36 MATERIALS SCIENCE↗