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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 415 records · Page 23

Design of additively manufactured methanol conversion reactor for high throughput production

Additively manufactured methanol conversion reactor was designed and fabricated for high throughput fuel production while capturing carbon dioxide. Here, the reactor designed is part of large effort in integrating electrolyzer and catalytic reactor system. Processing in fabricating the steel, titanium, and nickel alloy reactors were optimized to improve the catalyst deposition process and reaction efficiency. Microstructure of the additively manufactured reactors were characterized. General design is utilized to improve the performance of the reactor while exploring the benefit of freeform in additive manufacturing.

08 HYDROGEN↗

In Situ Investigation of Chemomechanical Effects in Thiophosphate Solid Electrolytes

Solid-state batteries can suffer from catastrophic failure at high current densities due to solid electrolyte fracture, interface decomposition, or lithium filament growth. Failure is linked to chemomechanical material transformations that can manifest during electrochemical cycling. We systematically investigate how solid electrolyte microstructure and interfacial decomposition (e.g., interphase) affect failure mechanisms in lithium thiophosphates (Li3PS4, LPS) electrolytes. Kinetically metastable interphases are engineered with iodine doping, and microstructural control is achieved using milling and annealing processing techniques. In situ transmission electron microscopy reveals iodine diffusion to the interphase, and upon electrochemical cycling, pores are formed in the interphase region. In situ synchrotron tomography reveals that interphase pore formation drives edge fracture events, which are the origin of through-plane fracture failure. Fractures in thiophosphate electrolytes actively grow toward regions of higher porosity and are affected by heterogeneity in microstructure (e.g., porosity factor). This report provides fundamental design guidelines for high-performance solid-state batteries.

25 ENERGY STORAGE↗

Oil-Pressure Based Apparatus for In-Situ High-Energy Synchrotron X-Ray Diffraction Studies During Biaxial Deformation

Background: Understanding biaxial loading response at the microstructural level is crucial in helping better design sheet manufacturing processes and calibrate/validate material deformation models. Objective: The objective of this work was to develop a low-cost testing apparatus to probe, with sufficient spatial resolution, the micro-mechanical response of a sheet material in-situ under biaxial loading conditions. Methods: The testing apparatus fabricated as a part of this study operates in a similar fashion to a standard bulge test and uses oil pressure to generate biaxial loading conditions. This biaxial testing apparatus was operated within a synchrotron beamline to characterize the mechanical response of a flash-processed steel sheet using in-situ high-energy X-ray diffraction (XRD) measurements. Further, the GSAS-II package was utilized to develop a workflow for the analysis of the large volume of diffraction data acquired. The workflow was then used to extract the peak position, width, and integrated intensity of the XRD peaks corresponding to the major body-centered cubic phase. Results: The equi-biaxial nature of the loading in the measured area was independently corroborated using experimental (XRD) and simulation (finite element analysis) methods. Furthermore, we discuss the evolution of elastic strain in the major body-centered cubic phase as a function of applied oil pressure and location on the steel sheet. Conclusions: A key advantage of the biaxial apparatus fabricated in this synchrotron study is demonstrated using the results obtained for the flash-processed steel sheet – i.e., mapping the lattice plane-dependent response to biaxial loading for a relatively large sample area in a spatially resolved manner.

36 MATERIALS SCIENCE↗

Scaling Laws of Exciton Recombination Kinetics in Low Dimensional Halide Perovskite Nanostructures

Carrier recombination is a crucial process governing the optical properties of a semiconductor. Although various theoretical approaches have been utilized to describe carrier behaviors, a quantitative understanding of the impact of defects and interfaces in low dimensional semiconductor systems is still elusive. Here, we develop a model system consisting of chemically tunable, highly luminescent halide perovskite nanocrystals to illustrate the role of carrier diffusion and material dimensionality on the carrier recombination kinetics and luminescence efficiency. Our advanced synthetic methods provide a well-controlled colloidal system consisting of nanocrystals with different aspect ratios, halide compositions, and surface conditions. Using this system, we reveal the scaling laws of photoluminescence quantum yield and radiative lifetime with respect to the aspect ratio of nanocrystals. The scaling laws derived herein are not only a phenomenological observation but proved a powerful tool disentangling the carrier dynamics of microscopic systems in a quantitative and interpretable manner. The investigation of our model system and theoretical formulation bring to light the dimensionality, as a hidden constraint on carrier dynamics, and identify the diffusion length as an important parameter that distinguishes nanoscale and macroscale carrier behaviors. Furthermore, the conceptual distinction in carrier dynamics in different dimensionality regimes informs new design rules for optical devices where complex microstructures are involved.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Insights into Plastic Localization by Crystallographic Slip from Emerging Experimental and Numerical Approaches

Advanced experimental and numerical approaches are being developed to capture the localization of plasticity at the nanometer scale as a function of the multiscale and heterogeneous microstructure present in metallic materials. These innovative approaches promise new avenues to understand microstructural effects on mechanical properties, accelerate alloy design, and enable more accurate mechanical property prediction. This article provides an overview of emerging approaches with a focus on the localization of plasticity by crystallographic slip. New insights into the mechanisms and mechanics of strain localization are addressed. The consequences of the localization of plasticity by deformation slip for mechanical properties of metallic materials are also detailed.

36 MATERIALS SCIENCE↗

Factors Controlling Stress Rupture of Fiber-Reinforced Ceramic Composites

The successful application of fiber-reinforced ceramic matrix composites (CMC) depends strongly on maximizing material rupture life over a wide range of temperatures and applied stresses. The objective of this paper is to examine the various intrinsic and extrinsic factors that control the high-temperature stress rupture of CMC for stresses below and above those required for cracking of the 0 C plies (Regions I and II, respectively). Using creep-rupture results for a variety of ceramic fibers and rupture data for CMC reinforced by these fibers, it is shown that in those cases where the matrix carries little structural load, CMC rupture conditions can be predicted very well from the fiber behavior measured under the appropriate test environment. As such, one can then examine the intrinsic characteristics of the fibers in order to develop design guidelines for selecting fibers and fiber microstructures in order to maximize CMC rupture life. For those cases where the fiber interfacial coatings are unstable in the test environment, CMC lives are generally worse than those predicted by fiber behavior alone. For those cases where the matrix can support structural load, CMC life can even be greater provided matrix creep behavior is properly controlled. Thus the achievement of long CMC rupture life requires understanding and optimizing the behavior of all constituents in the proper manner.

DiCarlo, J. A.↗

High-Performance Scanning Acousto-Ultrasonic System

A high-performance scanning acousto-ultrasonic system, now undergoing development, is designed to afford enhanced capabilities for imaging microstructural features, including flaws, inside plate specimens of materials. The system is expected to be especially helpful in analyzing defects that contribute to failures in polymer- and ceramic-matrix composite materials, which are difficult to characterize by conventional scanning ultrasonic techniques and other conventional nondestructive testing techniques. Selected aspects of the acousto-ultrasonic method have been described in several NASA Tech Briefs articles in recent years. Summarizing briefly: The acousto-ultrasonic method involves the use of an apparatus like the one depicted in the figure (or an apparatus of similar functionality). Pulses are excited at one location on a surface of a plate specimen by use of a broadband transmitting ultrasonic transducer. The stress waves associated with these pulses propagate along the specimen to a receiving transducer at a different location on the same surface. Along the way, the stress waves interact with the microstructure and flaws present between the transducers. The received signal is analyzed to evaluate the microstructure and flaws. The specific variant of the acousto-ultrasonic method implemented in the present developmental system goes beyond the basic principle described above to include the following major additional features: Computer-controlled motorized translation stages are used to automatically position the transducers at specified locations. Scanning is performed in the sense that the measurement, data-acquisition, and data-analysis processes are repeated at different specified transducer locations in an array that spans the specimen surface (or a specified portion of the surface). A pneumatic actuator with a load cell is used to apply a controlled contact force. In analyzing the measurement data for each pair of transducer locations in the scan, the total (multimode) acousto-ultrasonic response of the specimen is utilized. The analysis is performed by custom software that extracts parameters of signals in the time and frequency domains. The computer hardware and software provide both real-time and postscan processing and display options. For example, oscilloscope displays of waveforms and power spectral densities are available in real time. Images can be computed while scanning continues. Signals can be digitally preprocessed and/or post-processed by filtering, windowing, time-segmenting, and running-waveform-averaging algorithms. In addition, the software affords options for off-line simulation of the waveform-data-acquisition and scanning processes. In tests, the system has been shown to be capable of characterizing microstructural changes and defects in SiC/SiC and C/SiC ceramic-matrix composites. Delaminations, variations in density, microstructural changes attributable to infiltration by silicon, and crack-space indications (defined in the next sentence) have been revealed in images formed from several time- and frequency-domain parameters of scanning acousto-ultrasonic signals. The crack-space indications were image features that were not revealed by other nondestructive testing methods and are so named because they turned out to mark locations where cracking eventually occurred.

Roth, Don↗

Step-by-step growth of complex oxide microstructures

The synthesis of complex and hybrid oxide microstructures is of fundamental interest and practical applications. However, the design and synthesis of such structures is a challenging task. We developed a solution phase process to synthesize complex silica and silica titania hybrid microstructures by exploiting the emulsion droplet based shape control and step by step growth. The strategy is robust and can be extended to make complex hybrid structures made of two or more materials while each having its own shape.

36 MATERIALS SCIENCE↗

Irradiation creep measurement and microstructural analysis of chromium nitride–coated zirconium alloy using pressurized tubes

Environmental barrier coatings for Zr-based materials are currently under development to reduce oxidation and embrittlement in light-water reactors. Chromium nitride is one such candidate for this application, particularly as accident-tolerant fuel cladding. However, quantifying the impact of coatings on the irradiation-induced creep of zircaloy (Zry) is critical as this mechanism often exceeds thermal creep rates under light-water reactor operating conditions and can be a limiting design characteristic. Additionally, examining irradiation effects in the microstructure at the coating interface is key to understanding the compatibility of the material system. Here, to accelerate the experimental measurement of irradiation creep and microstructure evolution in CrN-Zry, compact, pressurized creep tubes were fabricated and irradiated in the High Flux Isotope Reactor (HFIR) at Oak Ridge National Laboratory. Miniature, thin-walled rodlets fabricated from annealed Zr-Sn barstock were coated with CrN using physical vapor deposition (PVD) to nominal thicknesses of 4 and 8 μm. Coated and uncoated rodlet specimens were internally pressurized and welded, generating nominal circumferential hoop stresses of 0, 90, or 180 MPa under 300°C irradiation conditions. Twelve specimens were measured diametrically prior to irradiation using a low-cost, automated, contactless laser profilometer developed for this work. Specimens were irradiated in sealed capsules for one 25-day HFIR cycle, accumulating approximately 1.8 $\times$ 10 21 n/cm 2 fast fluence (E n > 10 MeV). The irradiated samples were retrieved and remeasured using the same profilometry system in a shielded hot cell facility. Irradiation creep between specimens was compared using standard statistical tests and showed that both thicknesses of CrN coating had a negligible effect on the irradiation creep strain of the Zry material. Microstructure characterization of pre- and post-irradiated CrN-Zry specimens showed minimal changes due to irradiation but did show a substantial O-rich region at the Zry-CrN interface.

36 MATERIALS SCIENCE↗

Making & Breaking the Rules for DED Design

Design for Additive Manufacturing (DfAM) is widely used to describe design activities and guidelines employed in the creation of Additively Manufactured (AM) parts. Basic design rules for widely adopted processes like Powder Bed Fusion (PBF) are relatively understood including material performance, part size constraints, self-supporting angles, overhangs, wall thicknesses, and feature resolution. Complexity is often inherent with PBF using organically inspired solutions through generative design and topology optimization software to create designs that often cannot be realized via traditional manufacturing processes. The design rules for Directed Energy Deposition (DED) are less well known, and, in some cases, the lack of understanding is likely inhibiting broader application of the various DED processes. This presentation covers key design rules for DED fusion processes and elucidates opportunities like multi-material deposition and build approaches ranging from basic features to complex large-scale parts. Complementary to the opportunistic characteristics of DfAM for DED, Manufacture for AM (MfAM) encompasses the restrictive aspects of the manufacturing lifecycle with limitations due to bead width and wall thickness, self-supporting angles, surface texture, microstructural evolution, and residual stresses. AM enabled part design must always consider the entire value chain starting with incoming feedstock (e.g. plate, wire, or powder) and progressing through the printing process, post-processing (e.g. machining, inspection), and final system assembly. Key considerations, like the tradeoffs between feature resolution and build rate, for process and part selection and economic assessments will be discussed as DED is often traded against other AM processes. After highlighting typical DED design rules, we will also show how some of those rules can be broken via use cases and part designs that span the full spectrum of DED processes with examples of various DED part designs.

Additive Manufacturing↗

Additively manufactured novel Al-Cu-Sc-Zr alloy: Microstructure and mechanical properties

An in-depth understanding of microstructure and resultant properties is paramount in the design of a novel alloy system, especially for additive manufacturing (AM). The present investigation aims to characterize a prototypical AM Al alloy with great potential for structural applications. An Al-1.5Cu-0.8Sc-0.4Zr alloy designed using integrated computational material engineering was printed using the laser powder bed fusion AM process. This novel alloy shows promising combination of strength and ductility in as-built and peak-aged conditions. This improvement in the tensile properties is attributed to the presence of both coherent L1 2 Al 3 Sc/Al 3 (Sc,Zr) precipitates and Cu-rich regions. The microstructures were studied via extensive microscopy at different length scales using X-ray microscopy, scanning electron microscopy, and transmission electron microscopy. Fractography revealed that the columnar grain boundaries in as-built condition allow easy slip transfer as compared to the equiaxed grains, with the apex of the melt pool acting as the crack nucleation site. Furthermore, the peak aged condition resulted in improved strength while marginally sacrificing ductility due to precipitates decorating dislocations, grain boundaries and melt pool boundaries thus acting as obstacles to slip transfer.

36 MATERIALS SCIENCE↗

Controlling homogenization length scales and microstructure in additively manufactured Ti-Ta functionally graded materials

Materials with smooth compositional gradients or functionally grade materials (FGMs) produced via additive manufacturing (AM), enables joining dissimilar materials and optimizing multiple properties in advanced engineering applications. However, as-printed AM microstructures exhibit micro-segregation and solidification defects which, when combined with controlling macroscale gradient properties, complicates necessary post-processing. Here, we use CALPHAD-informed diffusion modelling to design post-processing heat treatments for lightweight to refractory FGMs. Ti-Ta (0 to 85 at. % Ta) FGMs were fabricated using laser-based directed energy deposition AM. Post-processing heat treatments at 1000° C and 1500° C were designed to promote homogenization across specific length scales and experimentally validated. Investigation of chemical segregation and microstructures demonstrated that the length scale of homogenization is controlled as a function of time, temperature, and local composition. Ta-rich regions exhibited incomplete homogenization compared to Ti-rich layers. Unmelted Ta particles were found to completely dissolve at 1500 °C. By controlling cooling rate (200 °C/min), martensitic structures were produced between 14–36 at. % Ta, consistent with martensite-start temperatures calculations, while furnace cooling (2 °C/min) produced α+β morphologies. This work establishes a validated predictive framework for designing post-processing to tailor microstructure and chemical architecture in AM FGMs, facilitating their deployment in demanding environments.

Materials science↗

Multi deep learning-based stochastic microstructure reconstruction and high-fidelity micromechanics simulation of time-dependent ceramic matrix composite response

A multi deep learning-based framework is developed for efficient, automated microstructure reconstruction and generation of stochastic representative volume elements (SRVEs) with periodic boundary conditions (PBCs) for accurate modeling of ceramic matrix composite (CMC) response. The methodology comprises a convolutional neural network coupled with regression layers to act as a vanilla regression network for semantic segmentation of the microstructure, allowing accurate characterization of the phases and their distributions at the microscale. Scanning electron microscope and confocal microscope are used to obtain C/SiNC and SiC/SiNC CMCs micrographs for vanilla regression testing. Microstructure variability in terms of fiber volume fraction and porosity are quantified through the output regression layer, ensuring accurate representation of material variability in SRVE construction. Generative adversarial network (GAN) and its variants are designed to produce high-fidelity SRVE, spanning CMCs microstructure variability space. A circular padding algorithm is developed to generate SRVEs with PBCs during training of GANs. The accuracy of the generated SRVEs is established through micromechanics simulations, where an efficient formulation of the high-fidelity generalized methods of cells (HFGMC) approach is used to compute the effective mechanical properties. Furthermore, an iterative algorithm is implemented in the HFGMC solver to simulate time-dependent deformation of SiC/SiNC subjected to creep loading conditions.

36 MATERIALS SCIENCE↗

A Bezier Curve Informed Melt Pool Geometry to Model Additive Manufacturing Microstructures Using SPPARKS

Additive manufacturing is a transformative technology with the potential to manufacture designs which traditional subtractive machining methods cannot. Additive manufacturing offers fast builds at near final desired geometry; however, material properties and variability from part to part remain a challenge for certification and qualification of metallic components. AM induced metallic microstructures are spatially heterogeneous and highly process dependent. Engineering properties such as strength and toughness are significantly affected by microstructure morphologies resulting from the manufacturing process Linking process parameters to microstructures and ultimately to the dynamic response of AM materials is critical to certifying and qualifying AM built parts and components and improving the performance of AM materials. The AM fabrication process is characterized by building parts layer by layer using a selective laser melt process guided by a computer. A laser selectively scans and melts metal according to a designated geometry. As the laser scans, metal melts, fuses, and solidifies forming the final geometry in a layerwise fashion. As the laser heat source moves away, the metal cools and solidifies forming metallic microstructures. This work describes a microstructure modeling application implemented in the SPPARKS kinetic Monte Carlo computational framework for simulating the resulting microstructures. The application uses Bzier curves and surfaces to model the melt pool surface and spatial temperature profile induced by moving the laser heat source; it simulates the melting and fusing of metal at the laser hot spot and microstructure formation and evolution when the laser moves away. The geometry of the melt pool is quite flexible and we explore effects of variances in model parameters on simulated microstructures.

36 MATERIALS SCIENCE↗