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At least 451 records · Page 25

Automated Guided-Wave Scanning Developed to Characterize Materials and Detect Defects

The Nondestructive Evaluation (NDE) Group of the Optical Instrumentation Technology Branch at the NASA Glenn Research Center has developed a scanning system that uses guided waves to characterize materials and detect defects. The technique uses two ultrasonic transducers to interrogate the condition of a material. The sending transducer introduces an ultrasonic pulse at a point on the surface of the specimen, and the receiving transducer detects the signal after it has passed through the material. The aim of the method is to correlate certain parameters in both the time and frequency domains of the detected waveform to characteristics of the material between the two transducers. The scanning system is shown. The waveform parameters of interest include the attenuation due to internal damping, waveform shape parameters, and frequency shifts due to material changes. For the most part, guided waves are used to gauge the damage state and defect growth of materials subjected to various mechanical or environmental loads. The technique has been applied to polymer matrix composites, ceramic matrix composites, and metal matrix composites as well as metallic alloys. Historically, guided wave analysis has been a point-by-point, manual technique with waveforms collected at discrete locations and postprocessed. Data collection and analysis of this type limits the amount of detail that can be obtained. Also, the manual movement of the sensors is prone to user error and is time consuming. The development of an automated guided-wave scanning system has allowed the method to be applied to a wide variety of materials in a consistent, repeatable manner. Experimental studies have been conducted to determine the repeatability of the system as well as compare the results obtained using more traditional NDE methods. The following screen capture shows guided-wave scan results for a ceramic matrix composite plate, including images for each of nine calculated parameters. The system can display up to 18 different wave parameters. Multiple scans of the test specimen demonstrated excellent repeatability in the measurement of all the guided-wave parameters, far exceeding the traditional point-by-point technique. In addition, the scan was able to detect a subsurface defect that was confirmed using flash thermography This technology is being further refined to provide a more robust and efficient software environment. Future hardware upgrades will allow for multiple receiving transducers and the ability to scan more complex surfaces. This work supports composite materials development and testing under the Ultra-Efficient Engine Technology (UEET) Project, but it also will be applied to other material systems under development for a wide range of applications.

Martin, Richard E.↗

Nanomechanical Characterization of Additive Manufactured GRCop-42 Alloy Developed by Directed Energy Deposition Methods

Propulsion applications such as combustion chambers and nozzles for liquid rocket engines require the use of unique materials with superior mechanical and thermal properties. GRCop-42(Cu-4 wt.% Cr-2 wt.% Nb) is one such candidate material developed by NASA and is now being manufactured using additive manufacturing (AM) techniques. AM offers a unique processing environment different from traditional metal fabrication processes. This study characterized the mechanical and structural properties of as-deposited and heat-treated GRCop-42manufactured with Blown Powder Directed Energy Deposition (BPD)based on preliminary testing. The materials were characterized using several techniques including surface profiling by laser microscopy, mechanical stiffness by instrumented indentation, crystal structure, residual stress measurements using XRD and residual XRD, and chemical composition and microstructural evaluation using SEM with EBSD. The results of the study are compared using the BPD techniques for samples in the as-deposited and heat-treated conditions.

GRCop-42↗

Structural Materials and Fuels for Space Power Plants

A fission reactor combined with Stirling convertor power generation is one promising candidate in on-going Fission Surface Power (FSP) studies for future lunar and Martian bases. There are many challenges for designing and qualifying space-rated nuclear power plants. In order to have an affordable and sustainable program, NASA and DOE designers want to build upon the extensive foundation in nuclear fuels and structural materials. This talk will outline the current Fission Surface Power program and outline baseline design options for a lunar power plant with an emphasis on materials challenges. NASA first organized an Affordable Fission Surface Power System Study Team to establish a reference design that could be scrutinized for technical and fiscal feasibility. Previous papers and presentations have discussed this study process in detail. Considerations for the reference design included that no significant nuclear technology, fuels, or material development were required for near term use. The desire was to build upon terrestrial-derived reactor technology including conventional fuels and materials. Here we will present an overview of the reference design, Figure 1, and examine the materials choices. The system definition included analysis and recommendations for power level and life, plant configuration, shielding approach, reactor type, and power conversion type. It is important to note that this is just one concept undergoing refinement. The design team, however, understands that materials selection and improvement must be an integral part of the system development.

Bowman, Cheryl↗

Synthetic Accessibility and Sodium Ion Conductivity of the Na8–x A x P2O9 (NAP) High-Temperature Sodium Superionic Conductor Framework

Advancement of solid-state electrolytes (SSEs) for all solid-state batteries typically focuses on modification of a known structural framework to improve conductivity, e.g., cation substitution for an immobile ion or varying the concentration of the mobile ions. Novel frameworks can be disruptive by enabling fast ion conduction aided by different structure and diffusion mechanisms, thereby unlocking optimal conductors with different properties. Herein, we perform a high-throughput survey of a structural framework for sodium ion conduction, Na8–x A x P2O9 (NAP), to understand the family’s thermodynamic stability, synthesizability, and ionic conduction. We show that the parent phase Na4TiP2O9 (NTP) undergoes a structural distortion (with accompanying conductivity transition) due to unstable phonons arising from pseudo-Jahn–Teller mode in the 1D titanium chains. Screening compounds in which Ti is substituted by other metals computationally reveal a number of candidates that are predicted to be low in formation energy and have high predicted ionic conductivities. High-throughput experimental and subsequent methodology optimization trials deliver one new compound, Na4SnP2O9 (NSP). X-ray diffraction (XRD), microscopy, and spectroscopy characterization indicate that the room-temperature structure of NSP is similar to the high-temperature, orthorhombic NTP phase but with some small unresolved structural differences. These uncharacterized structural details are speculated to limit the ion conductivity. Temperature-dependent XRD and electrochemical impedance spectroscopy indicate multiple coupled conductivity–structure transitions at a high temperature. We demonstrate the challenges with synthesis development and a priori identification of promising SSE phases as a major bottleneck in new (energy) materials development.

Chemical reactions↗

Understanding Formation of Irradiation-Induced Defects through 4D-STEM, Electron Tomography, and WBDF-STEM

A major challenge in advancing nuclear materials for next-generation fission and proposed fusion reactors is to comprehensively understand the formation of irradiation-induced defects. Here it is essential to correlate the evolution of irradiation-induced defects and the degradation of mechanical properties, as they collectively dictate the material's lifespan and ensure nuclear safety. Scanning transmission electron microscopy (STEM) based techniques have emerged as indispensable tools for irradiation-induced defect characterization, offering high spatial resolution imaging and chemical analysis, such as electron energy loss spectroscopy (EELS) and energy dispersive X-ray spectroscopy (EDXS). These techniques have been effectively used to obtain an atomic-scale view of the defect structure. Recent advances in electron microscopy, particularly in 4D-STEM, offer detailed insight into microstructural evolution by capturing full 2D diffraction patterns at every pixel position. Using high-speed direct electron detectors, this technology generates a four-dimensional dataset, overcoming the limitations of traditional STEM imaging.

36 MATERIALS SCIENCE↗

Morphologically-Directed Raman Spectroscopy as an Analytical Method for Subvisible Particle Characterization in Therapeutic Protein Product Quality

Abstract Subvisible particles (SVPs) are a critical quality attribute of injectable therapeutic proteins (TPs) that needs to be controlled due to potential risks associated with drug product quality. The current compendial methods routinely used to analyze SVPs for lot release provide information on particle size and count. However, chemical identification of individual particles is also important to address root-cause analysis. Herein, we introduce Morphologically-Directed Raman Spectroscopy (MDRS) for SVP characterization of TPs. The following particles were used for method development: (1) polystyrene microspheres, a traditional standard used in industry; (2) photolithographic (SU-8); and (3) ethylene tetrafluoroethylene (ETFE) particles, candidate reference materials developed by NIST. In our study, MDRS rendered high-resolution images for the ETFE particles (> 90%) ranging from 19 to 100 μm in size, covering most of SVP range, and generated comparable morphology data to flow imaging microscopy. Our method was applied to characterize particles formed in stressed TPs and was able to chemically identify individual particles using Raman spectroscopy. MDRS was able to compare morphology and transparency properties of proteinaceous particles with reference materials. The data suggests MDRS may complement the current TPs SVP analysis system and product quality characterization workflow throughout development and commercial lifecycle.

Science & Technology - Other Topics↗

Lessons learned from the development and implementation of a workforce training curriculum for advanced controls for high performance HVAC systems

Over the past decade, academic research on advanced controls has slowly transitioned into new software platforms, giving rise to various companies developing and deploying these innovative products, including solutions for light commercial HVAC systems. However, the current workforce remains widely unprepared to install, maintain and operate these systems, particularly complex software-based control platforms, as most workforce training programs still focus on traditional building automation for large commercial buildings. This paper presents the development and piloting of curriculum for three key types of professionals: ● Technicians (trade-level): installing and maintaining modern high-performance HVAC systems and controls ● Programmers (undergrad-level): developing and implementing advanced controls ● Engineers and energy professionals (undergrad/grad-level): managing and evaluating system performance We share details of the material developed including training videos, open-source software, instruction manuals. We also present the results of a pilot implementation of the training materials with real students.

Casillas, Armando↗

Development, fabrication and test of a high purity silica heat shield

A highly reflective hyperpure ( 25 ppm ion impurities) slip cast fused silica heat shield material developed for planetary entry probes was successfully scaled up. Process development activities for slip casting large parts included green strength improvements, casting slip preparation, aggregate casting, strength, reflectance, and subscale fabrication. Successful fabrication of a one-half scale Saturn probe (shape and size) heat shield was accomplished while maintaining the silica high purity and reflectance through the scale-up process. However, stress analysis of this original aggregate slip cast material indicated a small margin of safety (MS. = +4%) using a factor of safety of 1.25. An alternate hyperpure material formulation to increase the strength and toughness for a greater safety margin was evaluated. The alternate material incorporates short hyperpure silica fibers into the casting slip. The best formulation evaluated has a 50% by weight fiber addition resulting in an 80% increase in flexural strength and a 170% increase in toughness over the original aggregate slip cast materials with comparable reflectance.

Rusert, E. L.↗

Advanced Solid Rocket Motor nozzle development status

This paper presents a status update of the design and development of an improved nozzle for the Advanced Solid Rocket Motor (ASRM). The ASRM nozzle incorporates advanced state-of-the-art design features and materials which contribute to enhanced safety, reliability, performance, and producibility for the space shuttle boosters. During 1992 the nozzle design progressed through a successful Preliminary Design Review (PDR). An improved ablative material development program also culminated in the selection of new standard and low density carbon cloth phenolic prepreg offering reduced variability and improved process attributes. A subscale motor test series to evaluate new materials and design features was also completed. An overview update of the matured design characteristics, supporting analysis, key development-program results and program status and plans is reported.

Kearney, W. J.↗

Area-based composition predictions of materials fabricated using simultaneous wire-powder-directed energy deposition

Functionally graded materials are an emergent method for designing components with programmable site-specific material properties. These materials are typically fabricated using metal additive manufacturing tools by simultaneously feeding multiple wire and/or powder feedstocks at various rates to achieve spatial composition change. The wire-powder-directed energy deposition (WP-DED) technique is of particular interest for many functionally graded material applications by balancing the low raw materials cost of wire with the high resolution of powder. However, feeding wire and powder are inherently different processes since all extruded wire enters the melt pool, while much of the blown powder is scattered, which makes determining the composition of the build challenging. In this study, we devise a simple area-based measurement method for estimating the composition of WP-DED structures. WP-DED single beads are printed using 309L stainless steel wire and commercially pure Fe powder at five wire feed rates (0.5, 0.75, 1.00, 1.25, 1.50 mm/mm) and five powder feed rates (2, 4, 6, 8, 10 rpm). Characteristic defects including interface gaps and macrosegregation (lack of mixing) tendencies are examined. High powder feed rates (8, 10 rpm) result in interface gaps at all wire feed rates, but smooth deposition and complete mixing is achieved at low powder feed rates, particularly with lower wire feed rates as well. The area-based composition measurement method is within ±20% of energy dispersive x-ray spectroscopy measurements for all samples, showing its effectiveness as a rapid composition estimate for WP-DED materials development.

36 MATERIALS SCIENCE↗

Technology Advancements for Channel Wall Nozzle Manufacturing In Liquid Rocket Engines

A regeneratively-cooled or dump-cooled nozzle is a critical component for expansion of hot gases to enable high temperature and performance in liquid rocket engines systems. Regeneratively-cooled channel wall nozzles are a design solution used across the propulsion industry as a simplified method to fabricate the nozzle structure with internal coolant passages. The scale and complexity of the channel wall nozzle (CWN) design can be challenging to fabricate which results in extended lead times and higher costs. Some of these challenges include: 1) Unique and high temperature materials, 2) Tight tolerances on large parts during manufacturing and assembly to contain high pressure propellants, 3) Thin-walled features to maintain adequate wall temperatures, and 4) Unique manufacturing process operations and complex tooling. The United States (U.S.) National Aeronautics and Space Administration (NASA) and U.S. specialty manufacturing vendors are maturing modern fabrication techniques to reduce complexity and decrease costs associated with channel wall nozzle manufacturing technology. Additive Manufacturing (AM) is one of the key technology advancements under evaluation for channel wall nozzles. Much of additive manufacturing for propulsion components has focused on laser powder bed fusion (L-PBF), but the scale is not yet feasible for application to large scale nozzles. NASA is evolving directed energy deposition (DED) techniques for nozzles including arc-based deposition, blown powder deposition, and Laser Wire Direct Closeout (LWDC). There are different approaches being considered for fabrication of the nozzle, and each of these DED processes offer unique process steps for rapid fabrication. The arc-based and blown powder deposition techniques are used for the forming of the CWN liner. A variety of materials are being demonstrated including Inconel 625, Haynes 230, JBK-75, and NASA HR-1. The blown powder DED process is also being demonstrated for forming an integral channel nozzle in a single operation in similar materials. The LWDC process is a method for closing out the channels within the liner and forming the structural jacket using a localized laser wire deposition technique. Identical materials mentioned above have been used for this process in addition to bimetallic closeout (C-18150–SS347, and C-18150–Inconel 625). NASA has completed process development, material characterization, and hot-fire testing on a variety of these channel wall nozzle fabrication technique. This publication presents an overview of the various channel wall nozzle manufacturing processes and materials under evaluation including results from the hot-fire testing. Future development and technology focus areas is also discussed relative to channel wall nozzle manufacturing.

Additive manufacturing↗

Holistic comparison of environmental barrier coating material candidates through design of a figure of merit

The first figure of merit for environmental barrier coating (EBC) materials was designed through a ranking system for material properties pertaining to established EBC failure modes in service. Seven past, present, and novel EBC candidate materials were used in the figure of merit design: SiO 2 , Ba 0.75 Sr 0.25 Al 2 Si 2 O 8 (BSAS), HfSiO 4 , Yb 2 Si 2 O 7 , Yb 2 SiO 5 , Yb 2 O 3 , and YbPO 4 . Utilizing compiled data from the literature, the presented figure of merit verified Yb 2 Si 2 O 7 as the state-of-the-art candidate with optimal EBC properties and inferred that YbPO 4 should be considered as a potentially viable EBC material candidate. Further, the figure of merit allows for a holistic comparison of EBC candidates and informs experimental and computational search efforts for next-generation complex EBCs. Clear knowledge gaps found through this work include CaO–MgO–Al 2 O 3 –SiO 2 (CMAS)-resistant coatings, EBC lifetimes before delamination, and oxidant diffusion rates in relevant EBC microstructures. It was shown that while some materials show promise for solving a single key failure mode for EBCs (i.e., CMAS reactivity), a community-wide goal should be placed on materials development to achieve acceptable resistance against all major failure modes, which are interconnected. Novel compositionally complex EBC materials, in addition to layered EBC architectures, show promise for the optimization of material properties for long-lifetime EBCs in combustion environments.

36 MATERIALS SCIENCE↗

Nanoindentation’s imprint on an advanced society: Toward application conditions at the extremes

Abstract As society strives for a more sustainable future, key technologies depend on advanced materials development. Nanoindentation enables highly localized nanoscale measurement of mechanical properties, crucial for optimizing the performance of functional materials. Coupled with chemical charging, variable temperatures, or high deformation speeds, it offers insights into pressing materials science challenges necessary for sustainable energy transitions. This article explores the role of nanoindentation in advancing vital next-generation technologies. Graphical abstract

36 MATERIALS SCIENCE↗

Metalorganic chemical vapor deposition of ZnGeN 2 films on GaN: effects of cation stoichiometry on surface morphology and crystallinity

Novel optoelectronic device designs based on the heterostructures of III-N and II-IV-N 2 are promising to advance device performance significantly. For example, by utilizing InGaN-ZnGeN 2 quantum well (QW) structures instead of pure InGaN, the band structure engineering in the QW active region can lead to improved electron-hole wavefunction overlap, and thus enhance the radiative efficiency for photon generation. These novel heterostructures have great potential to address the current challenge of low quantum efficiency in InGaN QW based light emitting diodes emitting in green and beyond. The materials development of ZnGeN 2 is still at an early stage as compared to the much matured GaN material system. In an ideal octet rule preserving ordered structure of ZnGeN 2 , every N atom is coordinated by exactly two Zn and two Ge atoms. However, local violation of octet rule can be caused by non-ideal coordination of N by the cations. The disordered structure is thermodynamically less favorable but can still be achieved, for example, in kinetics-limited growth regime. The ordered ZnGeN 2 has a bandgap very close to that of GaN (~3.4 eV) and a lattice mismatch of <0.1% with GaN. Interestingly, the valence band of ZnGeN 2 has been predicted to be ~1 eV above that of GaN, which has inspired novel designs for high efficiency light emitters. In this work, we investigated the metalorganic chemical vapor deposition (MOCVD) of ZnGeN 2 films on GaN/c-sapphire templates. Diethylzinc (DEZn), germane (GeH4) and ammonia were used as the precursors for Zn, Ge and N, respectively. A systematic study was conducted to investigate the cation stoichiometry as a function of growth temperature (TG), total reactor pressure (P) and DEZn/GeH 4 molar flow rate ratio (RII/IV). Under the investigated growth window, the Zn/(Zn+Ge) composition in the films, determined from energy dispersive X-ray spectroscopy, decreased monotonically with increase in TG but increased with increase in P and RII/IV. Atom probe tomography data did not indicate the presence of any secondary phases such as Zn 3 N 2 or Ge 3 N 4 . The surface morphology and crystallinity of the grown films had strong correlation with the Zn/(Zn+Ge) composition. The scanning electron microscopy images showed that the near-stoichiometric films have planar surfaces whereas Zn-rich films had crystallites on their surface and the Zn-poor films had faceted surface. Scanning transmission electron microscopy (STEM) imaging revealed that the Zn-rich and Zn-poor films have columnar and filament-like morphology, respectively, whereas the near-stoichiometric films have continuous film-like cross-sectional morphology. TEM nano-diffraction patterns as well as X-ray diffraction 2θ-ω scan profiles indicate that the near stoichiometric films are single crystalline. Nano-diffraction pattern of the stoichiometric films resembled that of a disordered ZnGeN 2 structure. Room temperature Raman spectra of near-stoichiometric films showed only the phonon density of states like features of a cation disordered ZnGeN 2 . Cathodoluminescence and photoluminescence spectra measured at different temperatures had similar features with peak emission wavelength at ~ 2 eV. In conclusion, the stoichiometry of ZnGeN 2 films can be widely tuned by tuning the MOCVD growth parameters. The surface morphology and the crystallinity of the films were found to have strong correlation with the Zn/(Zn+Ge) composition. The stoichiometric ZnGeN 2 films grown on GaN were demonstrated with uniform surface morphology and high crystalline quality. The results from this work will provide pathway to implement ZnGeN 2 in device structures.

Karim, Md Rezaul↗

Characterization of Additively Manufactured Tungsten Heavy Alloy Material (CRADA Final Report)

LLNL and Aerojet Rocketdyne, Inc. (AR), using earlier collaborative work in powder bed printing of other materials, have been collaboratively pursuing the additive manufacture of tungsten heavy alloy (WHA) material since 2014. The goal of the project was to establish the ability to produce the LLNL developed material at the AR production facility. When accomplished, AR would produce an agreed array of test samples to technically characterize the material properties via testing. AR would conduct a portion of that testing and provide those results to LLNL. The goal of this work was to perform a trial transfer of LLNL’s WHA technology to AR

36 MATERIALS SCIENCE↗

The LARSYS Educational Package: Instructor's Notes for Use with the Data 100

The LARSYS Educational Package is a set of instructional materials developed to train people to analyze remotely sensed multispectral data using LARSYS, a computer software system. The materials included in this volume have been designed to assist LARSYS instructors as they guide students through the LARSYS Educational Package. All of the materials have been updated from the previous version to reflect the use of a Data 100 Remote Terminal.

Lindenlaub, J. C.↗

Rough-Wall Turbulent Heat Transfer Experiments in Hypersonic Free Flight

Experiments are being conducted in the NASA Ames Hypervelocity Free Flight Aerodynamic Facility to quantify the effects on turbulent convective heat transfer of surface roughness representative of a new class of 3D woven thermal protection system mRough-wall turbulent heat transfer measurements were obtained on ballistic-range models in hypersonic flight in the NASA Ames Hypervelocity Free Flight Aerodynamic Facility. Each model had three different surface textures on segments of the conic frustum: smooth wall, sand roughness, and a pattern roughness, thus providing smooth-wall and sand-roughness reference data for each test. The pattern roughness was representative of a woven thermal protection system material developed by NASA's Heatshield for Extreme Entry Environment Technology project. The tests were conducted at launch speeds of 3.2 km/s in air at 0.15 atm. Roughness Reynolds numbers, k+, ranged for 12 to 70 for the sand roughness, and as high as 200 for the pattern roughness. Boundary-layer parameters required for calculating k+ were evaluated using computational fluid dynamics simulations. The effects of pattern roughness are generally characterized by an equivalent sand roughness determined with a correlation developed from experimental data obtained on specifically-designed roughness patterns that do not necessarily resemble real TPS materials. Two sand roughness correlations were examined: Dirling and van Rij, et al. Both gave good agreement with the measured heat-flux augmentation for the two larger pattern roughness heights tested, but not for the smallest height tested. It has yet to be determined whether this difference is due to limitations in the experimental approach, or due to limits in the correlations used. Future experiments are planned that will include roughness patterns more like those used in developing the equivalent sand roughness correlations.aterials being developed by NASA's Heatshield for Extreme Entry Environment Technology (HEEET) project. Data were simultaneously obtained on sand-grain roughened surfaces and smooth surfaces, which can be compared with previously obtained data. Results are presented in this extended abstract for one roughness pattern. The full paper will include results from three roughness patterns representing virgin HEEET, nominal turbulent ablated HEEET, and twice the roughness of nominal turbulent ablated HEEET. Results will be used to compare with commonly used equivalent sand grain roughness correlations.

pattern roughness↗

Measuring 3D Profilometry of SAVY-4000 Nuclear Material Storage Containers: Novacam TubeInspect Capabilities Report

The SAVY-4000 container series is a general-purpose interim storage container for nuclear materials, developed and maintained by Los Alamos National Laboratory (LANL). It is the first vented, general-use nuclear material container to be demonstrated as meeting the requirements outlined in DOE M 441.1-1, the Nuclear Material Packaging Manual. Due to the challenging radiation, thermal, and corrosive storage conditions that the SAVY containers must endure, continuous surveillance techniques are employed to ensure the containers meet all safety standards and specifications. These inspections are typically performed by human operators, who check for issues such as corrosion, O-ring deterioration, corrosion, filter integrity, and potential manufacturing defects. However, human inspections alone are not sufficient, and automated inspection technologies, such as the ATIS system, as well as other automated systems are also utilized. The MicroCam TubeInspect, developed by Novacam Technologies Inc., is designed to address the challenges of understanding how manufacturing variations in the SAVY-4000 container series may affect performance. It is a 3D profilometry measurement system that enables detailed analysis of surface features, including defects, surface roughness, and manufacturing variations. This advanced tool significantly enhances rapid surveillance techniques for both pristine and used containers. In this study, container properties such as surface roughness, thickness, and geometric attributes like circularity are measured for SAVY-4000 containers. Artificially corroded or dented containers are examined to demonstrate the MicroCam's ability to quantify defects. A sensitivity analysis is also conducted, comparing the MicroCam results to those obtained using more precise instruments such as confocal microscopy. This comparison aims to provide valuable insights into container quality, durability, and potential improvements in manufacturing processes.

42 ENGINEERING↗