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DOE OSTI2026

Advancing Battery Manufacturing: Synchrotron Characterization for Industry

Large-scale battery manufacturing requires understanding the fundamental principles of materials and interfaces and relies on advanced techniques for detailed interrogation. Despite advancements in the industrial scale production and their associated quality control tools, challenges such as electrode heterogeneity, internal defects, and largescale material waste (e.g., scrap) can hamper manufacturing. Synchrotron X-ray characterization techniques offer spatial, temporal, and chemical resolution that can provide diagnostic insights for metrology across various manufacturing steps. This review examines the use of synchrotron tools to advance understanding of key steps in the battery manufacturing process. Recent examples demonstrate how synchrotron methods resolve manufacturing challenges and uncover degradation pathways that are otherwise inaccessible. Future directions for advancing battery manufacturing emphasize collaboration between academia and industry through the use of synchrotron X-ray techniques.

Batteries↗

NASA NTRS2006

Calibration Issues and Operating System Requirements for Electron-Probe Microanalysis

Instrument purchase requirements and dialogue with manufacturers have established hardware parameters for alignment, stability, and reproducibility, which have helped improve the precision and accuracy of electron microprobe analysis (EPMA). The development of correction algorithms and the accurate solution to quantitative analysis problems requires the minimization of systematic errors and relies on internally consistent data sets. Improved hardware and computer systems have resulted in better automation of vacuum systems, stage and wavelength-dispersive spectrometer (WDS) mechanisms, and x-ray detector systems which have improved instrument stability and precision. Improved software now allows extended automated runs involving diverse setups and better integrates digital imaging and quantitative analysis. However, instrumental performance is not regularly maintained, as WDS are aligned and calibrated during installation but few laboratories appear to check and maintain this calibration. In particular, detector deadtime (DT) data is typically assumed rather than measured, due primarily to the difficulty and inconvenience of the measurement process. This is a source of fundamental systematic error in many microprobe laboratories and is unknown to the analyst, as the magnitude of DT correction is not listed in output by microprobe operating systems. The analyst must remain vigilant to deviations in instrumental alignment and calibration, and microprobe system software must conveniently verify the necessary parameters. Microanalysis of mission critical materials requires an ongoing demonstration of instrumental calibration. Possible approaches to improvements in instrument calibration, quality control, and accuracy will be discussed. Development of a set of core requirements based on discussions with users, researchers, and manufacturers can yield documents that improve and unify the methods by which instruments can be calibrated. These results can be used to continue improvements of EPMA.

Carpenter, P.↗

NASA NTRS2006

Role of Process Control in Improving Space Vehicle Safety A Space Shuttle External Tank Example

Developing a safe and reliable space vehicle requires good design and good manufacturing, or in other words "design it right and build it right". A great design can be hard to build or manufacture mainly due to difficulties related to quality. Specifically, process control can be a challenge. As a result, the system suffers from low quality which leads to low reliability and high system risk. The Space Shuttle has experienced some of those cases, but has overcome these difficulties through extensive redesign efforts and process enhancements. One example is the design of the hot gas temperature sensor on the Space Shuttle Main Engine (SSME), which resulted in failure of the sensor in flight and led to a redesign of the sensor. The most recent example is the Space Shuttle External Tank (ET) Thermal Protection System (TPS) reliability issues that contributed to the Columbia accident. As a result, extensive redesign and process enhancement activities have been performed over the last two years to minimize the sensitivities and difficulties of the manual TPS application process.

Safie, Fayssal M.↗

NASA NTRS1998

Evaluation of Chemical Coating Processes for AXAF

The need existed at MSFC for the development and fabrication of radioisotope calibration sources of cadmium 109 and iron 55 isotopes. This was in urgent response to the AXA-F program. Several issues persisted in creating manufacturing difficulties for the supplier. In order to meet the MSFC requirements very stringent control needed to be maintained for the coating quality, specific activity and thickness. Due to the difficulties in providing the precisely controlled devices for testing, the delivery of the sources was seriously delayed. It became imperative that these fabrication issues be resolved to avoid further delays in this AXA-F observatory key component. The objectives are: 1) Research and provide expert advice on coating materials and procedures. 2) Research and recommend solutions to problems that have been experienced with the coating process. 3) Provide recommendations on the selection and preparation of substrates. 4) Provide consultation on the actual coating process including the results of the qualification and acceptance test programs. 5) Perform independent tests at UAH or MSFC as necessary.

Engelhaupt, Darell↗

NASA NTRS1997

Evaluation of Chemical Coating Processes for AXAF

The need existed at MSFC for the development and fabrication of radioisotope calibration sources of cadmium 109 and iron 55 isotopes. This was in urgent response to the AXAF program. Several issues persisted in creating manufacturing difficulties for the supplier. In order to meet the MSFC requirements very stringent control needed to be maintained for the coating quality, specific activity and thickness. Due to the difficulties in providing the precisely controlled devices for testing, the delivery of the sources was seriously delayed. It became imperative that these fabrication issues be resolved to avoid further delays in this AXAF observatory key component.

Engelhaupt, Darell E.↗

NASA NTRS2018

Effectiveness of Surface Treatment Techniques for Composite Bonding with Different Contamination Levels

Various surface treatment techniques have been developed to promote adhesive bond performance for composite structural components in aerospace applications. The condition of the pre-bond surface is critical to achieving desirable bond quality. Contamination on bonding surfaces is well recognized as a major threat to ultimate bond performance. Variation in contamination level has brought additional challenges into manufacturing process control. High fidelity surface treatment techniques are required for effective removal of contaminants over a wide range of contamination levels. In this study, a common contaminant, i.e. silicone mold release, was introduced to pre-bond composite surfaces with different concentrations. Plasma and laser surface treatment techniques were performed and their effectiveness in restoring and enhancing desirable bond quality was investigated. Surface characterization techniques, including water contact angle goniometry, Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy, were conducted to assess the condition of contaminated surfaces and the improvement induced by plasma and laser surface treatments. Failure modes from a customized double cantilever beam test were investigated before and after surface treatments. Fundamental mechanisms of plasma and laser surface treatments on the composite bonding surfaces were also investigated.

Fang, Xiaomei↗

NASA NTRS2015

Thermal Model Development for an X-Ray Mirror Assembly

Space-based x-ray optics require stringent thermal environmental control to achieve the desired image quality. Future x-ray telescopes will employ hundreds of nearly cylindrical, thin mirror shells to maximize effective area, with each shell built from small azimuthal segment pairs for manufacturability. Thermal issues with these thin optics are inevitable because the mirrors must have a near unobstructed view of space while maintaining near uniform 20 C temperature to avoid thermal deformations. NASA Goddard has been investigating the thermal characteristics of a future x-ray telescope with an image requirement of 5 arc-seconds and only 1 arc-second focusing error allocated for thermal distortion. The telescope employs 135 effective mirror shells formed from 7320 individual mirror segments mounted in three rings of 18, 30, and 36 modules each. Thermal requirements demand a complex thermal control system and detailed thermal modeling to verify performance. This presentation introduces innovative modeling efforts used for the conceptual design of the mirror assembly and presents results demonstrating potential feasibility of the thermal requirements.

x ray optics↗

NASA NTRS1973

Fabrication and Improvement of Lmsc's All-silica RSI

The LI-1500 and LI-900 all silica RSI materials have made the transition from laboratory to manufacturing operation. Improvements in both quality and reproducibility have been achieved. The LI-1500 material has displayed superior reliability in evaluations conducted at various facilities. The dependable performance of the material is attributed to the adherence to the stringent requirements of the numerous material, process, and product control evaluations and inspection points performed during manufacture.

Beasley, R. M.↗

NASA NTRS1992

High-speed civil transport flight- and propulsion-control technological issues

Technology advances required in the flight and propulsion control system disciplines to develop a high speed civil transport (HSCT) are identified. The mission and requirements of the transport and major flight and propulsion control technology issues are discussed. Each issue is ranked and, for each issue, a plan for technology readiness is given. Certain features are unique and dominate control system design. These features include the high temperature environment, large flexible aircraft, control-configured empennage, minimizing control margins, and high availability and excellent maintainability. The failure to resolve most high-priority issues can prevent the transport from achieving its goals. The flow-time for hardware may require stimulus, since market forces may be insufficient to ensure timely production. Flight and propulsion control technology will contribute to takeoff gross weight reduction. Similar technology advances are necessary also to ensure flight safety for the transport. The certification basis of the HSCT must be negotiated between airplane manufacturers and government regulators. Efficient, quality design of the transport will require an integrated set of design tools that support the entire engineering design team.

Ray, J. K.↗

DOE OSTI2025

The AMACStar ASIC for the HL-LHC ATLAS ITk Strip detector: design, verification, testing, and quality assurance

For the high-luminosity upgrade to the LHC (HL-LHC), the ATLAS detector at CERN requires an all-new inner detector, the Inner Tracker (ITk). The ITk Strip subdetector is made up of silicon modules, which include three types of radiation-hard ASICs. One of these is the Autonomous Monitor and Control (AMAC). The AMAC is manufactured by Global Foundries using 130 nm CMOS8RF DM technology and is approximately 3 by 5 mm in size. This ASIC autonomously monitors the temperatures, voltages, and currents in the module components while controlling critical values in order to prevent these quantities from reaching dangerous levels. The final design, AMACStar, was verified, tested, and ensured to perform all necessary functions. A quality control procedure using an in-house probe station set-up was developed in order to ensure that every individual chip on each wafer of AMACStars required by the ITk Strip project met performance requirements. The average per wafer yield of usable AMACStars is 92.33%, exceeding the design-specific 90% yield estimated for project costing. This estimate was based on actual yields for similar designs in this process.

Analogue electronic circuits↗

DOE OSTI2022

Defect and satellite characteristics of additive manufacturing metal powders

Metal additive manufacturing (AM) requires high-quality metal powders to three-dimensionally (3D) print metallic components with complex and customizable geometries. The lack of quantification of AM metal powders creates quality control challenges for 3D printed components, increases the uncertainty of printing reliability and net cost of inspected and certified printed components, and reduces the recyclability of used powders. However, critical characteristics of AM metal powders that are decisive factors for the 3D printing process, such as internal porosity, contamination, and satellite feature, remain ambiguous. In this work, we developed a novel approach to 3D quantify key characteristics of AM metal powders down to individual particles by using high-resolution synchrotron x-ray computed tomography. Empowered by the penetrative capability of high-energy x-ray, internal porosity and contamination within as-atomized metal powders from high-entropy alloys to nickel-based superalloys were evaluated. Additionally, the newly-developed dispersion method enables the homogeneous separation of individual particles, and consequently, results in the implementation of 3D particle shape analysis. To resolve a major challenge of identification and quantification of satellite-feature particles in as-atomized AM metal powders, the satellite features were quantitated by modeling and analyzing the shape parameter of local thickness variance. Furthermore, the 3D analytical methods of particle assessment in this study can be applied to other materials systems like rock, food, and pharmaceutical particles, and provide insights for process optimization across powder metallurgy, concrete, food and pharmaceutical manufacturing, and AM industries.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Quality Control of Additively Manufactured Metallic Structures with Machine Learning of Thermography Images

Additive manufacturing (AM) of high-strength metals is currently based on the laser powder bed fusion (LPBF) process, which can introduce internal material flaws, such as pores and anisotropy. Quality control (QC) requires nondestructive evaluation of actual AM structures. Flash thermography is a potentially promising QC technique because it is scalable to arbitrary structure size. However, the detection sensitivity of this method is limited by noise. We investigate separation of signal from noise in thermography images using several machine learning (ML) methods, including new spatial–temporal blind source separation and spatial–temporal sparse dictionary learning methods. Performance of the ML methods is benchmarked using thermography data obtained from imaging stainless steel 316L and Inconel 718 specimens produced by the LPBF method with imprinted calibrated porosity defects. The ML methods are ranked by F-score and execution runtime. Finally, the ML methods with higher accuracy require a longer runtime. However, this runtime is sufficiently short to perform QC within a realistic time frame.

36 MATERIALS SCIENCE↗

NASA NTRS1975

Flexible joints for thrust vector control

Flexible joints have been used to achieve thrust vector control over a wide range of sizes of nozzles and have been demonstrated successfully in bench tests and static firings, and are operational on two motors. From these many joints the problems of flexible joints have been defined as establishment of the movable nozzle envelope, definition of the actuation power requirements, definition of the mechanical properties of joint materials, adhesive bonding, test methods, and quality control. These data and problem solutions are contained in a large number of reports. Data relating to joint configuration, design requirements, materials selection, joint design, structural analysis, manufacture, and testing are summarized.

Woodberry, R. F. H.↗

NASA NTRS2007

Materials Safety - Not just Flammability and Toxic Offgassing

For many years, the safety community has focused on a limited subset of materials and processes requirements as key to safety: Materials flammability, Toxic offgassing, Propellant compatibility, Oxygen compatibility, and Stress-corrosion cracking. All these items are important, but the exclusive focus on these items neglects many other items that are equally important to materials safety. Examples include (but are not limited to): 1. Materials process control -- proper qualification and execution of manufacturing processes such as structural adhesive bonding, welding, and forging are crucial to materials safety. Limitation of discussions on materials process control to an arbitrary subset of processes, known as "critical processes" is a mistake, because any process where the quality of the product cannot be verified by inspection can potentially result in unsafe hardware 2 Materials structural design allowables -- development of valid design allowables when none exist in the literature requires extensive testing of multiple lots of materials and is extremely expensive. But, without valid allowables, structural analysis cannot verify structural safety 3. Corrosion control -- All forms of corrosion, not just stress corrosion, can affect structural integrity of hardware 4. Contamination control during ground processing -- contamination control is critical to manufacturing processes such as adhesive bonding and also to elimination foreign objects and debris (FOD) that are hazardous to the crew of manned spacecraft in microgravity environments. 5. Fasteners -- Fastener design, the use of verifiable secondary locking features, and proper verification of fastener torque are essential for proper structural performance This presentation discusses some of these key factors and the importance of considering them in ensuring the safety of space hardware.

Pedley, Michael D.↗

NASA NTRS1993

Principles of gas phase processing of ceramics during combustion

In recent years, ceramic materials have found applications in an increasingly wider range of industrial processes, where their unique mechanical, electrical and optical properties are exploited. Ceramics are especially useful for applications in high temperature, corrosive environments, which impose particularly stringent requirements on mechanical reliability. One approach to provide such materials is the manufacture of submicron (and more recently nanometer scale) particles, which may subsequently be sintered to produce a material with extremely high mechanical integrity. However, high quality ceramic materials can only be obtained if particles of known size, polydispersity, shape and chemical purity can be produced consistently, under well controlled conditions. These requirements are the fundamental driving force for the renewed interest in studying particle formation and growth of such materials.

Zachariah, Michael R.↗

NASA NTRSDate not supplied

Closed-Loop Control of Laser Surface Treatment via Laser Induced Breakdown Spectroscopy

Current composite manufacturing rates need to be improved to meet the projected demand of on-demand mobility (ODM) and commercial aircraft transports. Some processes in the composite manufacturing chain require touch labor such as manual sanding of surfaces prior to bonding and installing thousands of mechanical fasteners in bonded primary structures to achieve Federal Aviation Administration (FAA) certification. The consequences are insufficient repeatability in bond quality resulting in increased manufacturing time. The FAA has indicated that robust process control is one potential means of certifying bondlines in primary structure. This work describes an integrated closed-loop control system between a laser machining system and laser induced breakdown spectroscopy (LIBS) instrumentation as a means of assuring bond performance and achieving certified composite bondlines. Preliminary results from in-situ treatment and inspection are presented. Results indicate that LIBS inspection and laser treatment can be conducted simultaneously to achieve high quality, reliable adhesive bonds.

Rodolfo Ledesma↗

NASA NTRSDate not supplied

Closed-Loop Control of Laser Surface Treatment via Laser Induced Breakdown Spectroscopy

Rodolfo Ledesma↗

NASA NTRS2007

Supportability Technologies for Future Exploration Missions

Future long-duration human exploration missions will be challenged by resupply limitations and mass and volume constraints. Consequently, it will be essential that the logistics footprint required to support these missions be minimized and that capabilities be provided to make them highly autonomous from a logistics perspective. Strategies to achieve these objectives include broad implementation of commonality and standardization at all hardware levels and across all systems, repair of failed hardware at the lowest possible hardware level, and manufacture of structural and mechanical replacement components as needed. Repair at the lowest hardware levels will require the availability of compact, portable systems for diagnosis of failures in electronic systems and verification of system functionality following repair. Rework systems will be required that enable the removal and replacement of microelectronic components with minimal human intervention to minimize skill requirements and training demand for crews. Materials used in the assembly of electronic systems (e.g. solders, fluxes, conformal coatings) must be compatible with the available repair methods and the spacecraft environment. Manufacturing of replacement parts for structural and mechanical applications will require additive manufacturing systems that can generate near-net-shape parts from the range of engineering alloys employed in the spacecraft structure and in the parts utilized in other surface systems. These additive manufacturing processes will need to be supported by real-time non-destructive evaluation during layer-additive processing for on-the-fly quality control. This will provide capabilities for quality control and may serve as an input for closed-loop process control. Additionally, non-destructive methods should be available for material property determination. These nondestructive evaluation processes should be incorporated with the additive manufacturing process - providing an in-process capability to ensure that material deposited during layer-additive processing meets required material property criteria.

Watson, Kevin↗