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DOE OSTI2025

Estimating the State of Charge in Lithium Primary Batteries: Recent Advances and Critical Insights

Lithium primary batteries (LPBs) remain essential in critical applications such as military, aerospace, medical and emergency devices, and portable electronics. Their superior energy density over lithium-ion batteries offers a significant advantage for long-duration use. Therefore, accurate estimation of the state of charge (SoC) is essential for ensuring the reliable and safe operation of these batteries. While extensive research has been conducted on SoC estimation techniques for lithium-ion secondary batteries, LPBs present unique challenges that complicate accurate SoC estimation. Moreover, research on nondestructive testing techniques for SoC estimation in LPBs is significantly lacking. In this review article, it is aimed to provide a comprehensive overview of recent advancements in SoC estimation for LPBs and generates new insights and directions for future research. Herein, existing methods are discussed and their effectiveness and mechanisms are identified, and areas for further optimization are outlined. More theoretical/experimental efforts to advance SoC detection in LPBs is recommended due to challenges identified with existing techniques.

25 ENERGY STORAGE↗

DOE OSTI2024

In-Process Monitoring and Structural Health Monitoring of Large-Scale Additive Manufacturing Using Acoustic Emission Technique

ORNL collaborated with MISTRAS Group, Inc. to investigate acoustic emission (AE) as a structural health monitoring (SHM) method for large-scale additive manufacturing (AM). Large-scale AM is being adapted as method of producing large structures in a short lead time and cost-effective way. With the growing advancement in AM techniques and application, machine monitoring and part qualification is highly needed. There has been leading research focused on the manufacturing, feedstock material but minimum research on the SHM, defect detection, and nondestructive evaluation (NDE) for AM. Scanning large structure using conventional nondestructive testing (NDT) techniques, such as ultrasound or X-ray, and searching for potential defects can be very time consuming, challenging and cost prohibitive. AE is a passive technique that can be used to monitor and locate defect progression in large structure by distributing group of sensors around the part. This project utilized AE technique and system manufactured/designed by MISTRAS Group to monitor large-scale AM equipment (i.e. Big Area Additive Manufacturing (BAAM) system located at the Oak Ridge National Laboratory – Manufacturing Demonstration Facility (ORNL-MDF) and the printed parts it produces. The AE system provided valuable insight on defect development/progression during and post-printing process.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Demonstrating resonant ultrasound spectroscopy as a viable technique to characterize thermally conditioned high explosive materials

We present results of resonant ultrasound spectroscopy (RUS) measurements applied to granular high explosive materials at different bulk pressing densities and degree of thermal conditioning. The material chosen in this study is a ubiquitously used explosive material known as pentaerythritol tetranitrate (PETN), which is used commercially in civil and defense applications both as a binderized plastic bonded explosive material and an unbinderized neat material. However, changes in granular PETN bulk elastic properties due to thermal conditioning, which could have implications for better understanding environmental aging-related effects, have not been well studied even though it is believed that elasticity may play an important role in explosive material initiation mechanisms. Furthermore, monitoring elastic property changes in granular explosive pressings has not yet been demonstrated using RUS, which is an appealing non-destructive characterization tool that requires only dry point contact with the explosive material. To this end, we report the first study using RUS to quantify the elastic properties of binderized and neat PETN pressings as well as to quantify changes in elastic properties as a function of both thermal conditioning and bulk pressing density. Elastic stiffness coefficients, sometimes more commonly referred to as elastic constants, calculated from the RUS measurements on the different PETN-based materials show a significant increase for the post-conditioned samples compared to the pre-conditioned samples. This trend of increasing elastic properties with thermal conditioning was consistent for different density pressings, different thermal exposure conditions, and even different neat PETN pressings of differing average crystal sizes and/or specific surface areas.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Quantitative uranium elemental reconstruction using spectral x-ray radiography

X-ray radiography offers the ability to noninvasively inspect the internal structure and material composition of objects. Dual-energy radiography allows material discrimination but is limited in quantitative material measurements due to the broad nature of the interrogating x-ray spectrum. Spectral radiography detectors provide an observation of not just the number of x rays that are transmitted through a sample but also the spectrum. Here, experimental validations of a method to use spectral x-ray radiography to accurately quantify the uranium mass in a powder are presented. An accurate system response model was developed, which includes a model of the incident x-ray source spectrum and a pixel-wise detector response that describes how the transmitted x rays were observed. Further, a calibration to account for the effect of partial x-ray attenuation was developed. As a result, the method is demonstrated to be capable of estimating the uranium mass in a variety of uranium oxide powders to a bias of –0.01±0.62%.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

DOE OSTI2024

3D Reconstruction of a High-Energy Diffraction Microscopy Sample Using Multi-modal Serial Sectioning with High-Precision EBSD and Surface Profilometry

High-energy diffraction microscopy (HEDM) combined with in situ mechanical testing is a powerful nondestructive technique for tracking the evolving microstructure within polycrystalline materials during deformation. This technique relies on a sophisticated analysis of X-ray diffraction patterns to produce a three-dimensional reconstruction of grains and other microstructural features within the interrogated volume. However, it is known that HEDM can fail to identify certain microstructural features, particularly smaller grains or twinned regions. Characterization of the identical sample volume using high-resolution surface-specific techniques, particularly electron backscatter diffraction (EBSD), can not only provide additional microstructure information about the interrogated volume but also highlight opportunities for improvement of the HEDM reconstruction algorithms. In this study, a sample fabricated from undeformed “low solvus, high refractory” nickel-based superalloy was scanned using HEDM. The volume interrogated by HEDM was then carefully characterized using a combination of surface-specific techniques, including epi-illumination optical microscopy, zero-tilt secondary and backscattered electron imaging, scanning white light interferometry, and high-precision EBSD. Custom data fusion protocols were developed to integrate and align the microstructure maps captured by these surface-specific techniques and HEDM. The raw and processed data from HEDM and serial sectioning have been made available via the Materials Data Facility (MDF) at https://doi.org/10.18126/4y0p-v604 for further investigation.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Material Identification From Radiographs Without Energy Resolution

We propose a method for performing material identification from radiographs without energy-resolved measurements. Material identification has a wide variety of applications, including in biomedical imaging, nondestructive testing, and security. While existing techniques for radiographic material identification make use of dual energy sources, energy-resolving detectors, or additional (e.g., neutron) measurements, such setups are not always practical— requiring additional hardware and complicating imaging. We tackle material identification without energy resolution, allowing standard X-ray systems to provide material identification information without requiring additional hardware. Assuming a setting where the geometry of each object in the scene is known and the materials come from a known set of possible materials, we pose the problem as a combinatorial optimization with a loss function that accounts for the presence of scatter and an unknown gain and propose a branch and bound algorithm to efficiently solve it. We present experiments on both synthetic data and real, experimental data with relevance to security applications— thick, dense objects imaged with MeV X-rays. We show that material identification can be efficient and accurate, for example, in a scene with three shells (two copper, one aluminum), our algorithm ran in six minutes on a consumer-level laptop and identified the correct materials as being among the top 10 best matches out of 8,000 possibilities.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Internal defect detection and characterization of samarium-cobalt sintered magnets by ultrasonic testing technique

Excessive quantities of samarium-cobalt (Sm-Co) magnet material are being scrapped needlessly due to a lack of understanding of inhomogeneity distribution and unacceptable internal defects. If there is a way to identify, locate, characterize and when needed separate the defective portions of magnet material, utilization can be increased and product quality improved. Further, the magnets’ magnetic and mechanical performance can be improved by reducing the occurrence of internal defects. This paper reports on a cost-effective and efficient nondestructive evaluation method based on an ultrasonic testing (UT) technique applied for detecting and characterizing internal defects in Sm-Co sintered magnets. Applying the UT technique will allow users to comprehensively analyze internal defects, such as inclusions, porosity, microcracks, and other structural irregularities, check for homogeneity and anomalous regions and give the locations of these internal anomalies and defects within the Sm-Co sintered magnets. The UT technique can also be applied to other rare-earth permanent magnets, such as sintered or die-upset neodymium-iron-boron (Nd-Fe-B) magnets. The UT technique can effectively guide quality control and acceptable product selection, in addition to optimizing the magnet alloy design and production processes. Therefore, it can facilitate the improvement of magnet manufacturing efficiency and machinability, reduce scrap, prolong service life, increase the use of what would be post-production waste, and enhance product reuse and recycling at end-of-life disposition.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Sparse-Data Deep Learning Strategies for Radiographic Non-Destructive Testing

Radiography is an imaging technique used in a variety of applications, such as medical diagnosis, airport security, and nondestructive testing. We present a deep learning system for extracting information from radiographic images. We perform various prediction tasks using our system, including material classification and regression on the dimensions of a given object that is being radiographed. Our system is designed to address the sparse-data issue for radiographic nondestructive testing applications. It uses a radiographic simulation tool for synthetic data augmentation, and it uses transfer learning with a pre-trained convolutional neural network model. Using this system, our preliminary results indicate that the object geometry regression task saw an improvement of 70% in the R-squared value when using a multi-regime model. In addition, we increase the performance of the object material classification tasks by utilizing data from different imaging systems. In particular, using neutron imaging improved the material classification accuracy by 20% when compared to x-ray imaging.

convolutional neural networks↗

DOE OSTI2024

Long-Term Performance of Ag/AgCl Reference Electrodes for Corrosion Potential Monitoring in Radioactive Tank Waste at the Hanford Site

This work studied the exposure effects of radioactive tank waste on the long-term performance of single junction Ag/AgCl reference electrodes for corrosion potential monitoring at the Hanford Site. Electrodes from three manufacturers with very different designs were studied using open-circuit potential and electrochemical impedance measurements in radioactive tank waste. Post-test analyses were conducted on some failed electrodes using destructive and nondestructive techniques. The intrusion of the aggressive and radioactive chemicals in tank waste through the porous frit materials was the primary mechanism that led to the clogging of frit, physical and chemical degradation of AgCl bonded to Ag wire, and alteration of the internal electrolyte. Radiolytic chemical species such as H2O2 and HNO3 may have also induced the degradation of the Ag wire. The extent of electrode degradation and failure probability highly depended on the electrode design and environmental conditions. Chemicals in tank waste had stronger effects than radiation on the long-term performance of the Ag/AgCl reference electrodes.

Materials Science↗

DOE OSTI2023

An Assessment of Machine Learning Applied to Ultrasonic Nondestructive Evaluation

In the United States, the nuclear industry performs inservice inspection (ISI) through nondestructive examination (NDE) methods in accordance with guidelines specified in the American Society of Mechanical Engineers (ASME) Boiler and Pressure Vessel Code (BPVC), Section XI, Rules for Inservice Inspection of Nuclear Power Plant Components. Ultrasonic nondestructive testing and evaluation (NDT&E) is one of the more commonly used techniques for inspecting Class 1 structural components in nuclear power systems. As the number of qualified NDE inspectors declines, the nuclear industry is looking to take advantage of advances in automation to enhance inspection capabilities. Advances in computational power, cloud-based computing, and machine learning algorithms make automated data analysis possible. Machine learning (ML) has shown huge potential in automated data analyses for ultrasonic NDE in the context of weld inspections.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2024

Guest Editorial for Nondestructive Testing and Evaluation (NDT&E) Special Section

Nondestructive testing and evaluation (NDT&E) are interdisciplinary fields that require a significant amount of interconnection between fundamental physics, measurement techniques, data processing, decision making, and reporting to have a significant impact on industry. NDT&E practitioners are challenged to keep up with the fast-paced evolution of materials, structures, processing, and manufacturing technologies. The development of engineered materials, complex structures and composites, and novel forming techniques require NDT&E to rapidly evolve to meet the needs of industry.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2023

Laboratory Instrument Software Controlled Spread Spectrum Time Domain Reflectometry for Electrical Cable Testing

This research discusses development of a software-controlled laboratory instrument based spread spectrum time domain reflectometry system (SSTDR). This constitutes one task within PNNL’s Light Water Sustainability Program (LWRS) whose mission includes advancing nondestructive examination (NDE) techniques for off-line and on-line in-situ cable condition monitoring. In 2022, PNNL evaluated SSTDR for detection and characterization of a number of cable anomalies (Glass et al. 2022). The review included comparison of SSTDR to Frequency Domain Reflectometry (FDR) techniques which have enjoyed encouraging feedback and are starting to be used in nuclear power plants for periodic cable condition monitoring of cable systems as part of the plant’s overall cable aging management program. The FDR test introduces a broad-band chirp onto the cable at the cable end then listens for any reflection from a change of impedance along the cable caused by a damaged conductor or insulation, splices, contact with moisture, or other cable anomalies. The signal is captured in the frequency domain then transformed back to the time domain using an inverse Fourier transform (IFT). Based on the velocity of propagation, the impedance response signal is plotted against distance along the cable. Peak locations along the X-axis indicate the distance along the cable where a portion of the signal has been reflected back to the instrument as a result of a cable anomaly. The FDR test is considered the gold standard of reflectometry however it does require the cable to be de-energized to perform the test. The LIVEWIRE commercial SSTDR produces a similar plot to the FDR however all processing is in the time domain. A pseudo-random noise code (PN code) is input onto the cable conductor and the instrument listens for any reflected response from cable anomalies. The SSTDR processes the signal as an autocorrelation comparing the input PN code to any reflected signal detected. The autocorrelation analysis for thermal aging, water and water ingress detection, ground fault and phase-to-phase fault detection at various locations along the cable and with the cable attached and detached from a motor load, and on both energized and un-energized conditions were performed. These results were contrasted to Frequency Domain Reflectometry (FDR) measurements of the un-energized cable. Results were encouraging but indicated more work was warranted – particularly with the SSTDR, it seemed that the insulation damage would likely be better evaluated with multiple bandwidth cable tests particularly including larger bandwidths than were possible with the current commercial instrument. The commercial instrument’s bandwidth was set at 6, 12, 24, and 48MHz but note that SSTDR and FDR definitions of bandwidth trend similarly but are not the same. The FDR response could be more broadly adjusted, and the bandwidth of 100 to 500 MHz produced the best responses. FDR responses to anomalies were clearer than SSTDR responses and indications were that a broader bandwidth SSTDR may lead to improved SSTDR detection capability. This project used a laboratory instrument based SSTDR (primarily using an Arbitrary Waveform Generator (AWG) and a digital oscilloscope plus Python in-house software) that allowed software adjustment of the SSTDR bandwidth, window functions applied to the exciting Pseudo-random Noise (PN) code plus and other aspects of the SSTDR signal processing. Hereafter, this will be referred to as the PNNL SSTDR. Evaluating specific performance of the PNNL SSTDR is left to a separate report. This report documents hardware and software development to produce the SSTDR cable test system.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

DOE OSTI2025

Evaluation and Development of Phase Array Ultrasonic Testing (PAUT) System for Additively Manufactured Parts

This research focuses on the application of advanced ultrasonic testing techniques developed by The Phased Array Company (TPAC) for inspecting defects in additive manufacturing (AM) parts. Traditionally, X-ray computed tomography is the standard for inspecting AM components. Although, the long inspection and analysis time, along with relatively high cost make implementation difficult. Thus, an alternative nondestructive evaluation (NDE) approach is necessary to support quality assurance efforts within the field of AM. TPAC is recognized as a leader in ultrasonic testing innovation, deploying sophisticated algorithms such as Total Focusing Method (TFM) and Phased Wave Imaging (PWI) for ultrasonic data processing and interpretation. This work will explore how the TFM and PWI algorithms can assist defect detection within polymer AM parts. The AM field is seeking novel NDE methods to provide support within quality control and assurance efforts. Advanced ultrasonics inspection have the potential to fulfill this need.

99 GENERAL AND MISCELLANEOUS↗

DOE OSTI2025

Evaluation and Development of Phase Array Ultrasonic Testing (PAUT) System for Additively Manufactured Parts

36 MATERIALS SCIENCE↗

DOE OSTI2026

Ultrasound Characterization of Plastic Bonded Explosives With Varied Binder Content and Density

Advanced explosive formulations and methods of production require rapid characterization for both processes and materials. Here, we present results for ultrasound characterization of a plastic bonded explosive (PBX) formulation as a function of binder weight percent and pressing density using through-transmission sound speed measurements. The explosive in this study was composed of 1,3,5-triamino-2,4,6-trinitrobenzene (TATB) combined with the fluoropolymer binder Kynar Ultraflex B. Binder content ranged from 2.6 wt.% to 11.5 wt.% with associated explosive formulation densities from 1.69 g/cc to 1.89 g/cc. We find linear and nonlinear changes in longitudinal and shear sound speeds, peak frequencies, and measured elastic properties for the different PBX formulations. These measured changes can differentiate the tested formulations, highlighting the potential for ultrasound as a nondestructive characterization method for newly-formulated PBXs. We also demonstrate through-transmission measurements using different coupling media and present results from an ultrasound technique called resonant ultrasound spectroscopy (RUS). Both transmission and RUS approaches may allow for rapid and even automated characterization of PBX components suitable for high-throughput manufacturing operations.

Engineering↗

DOE OSTI2024

Accurate Ultrasonic Thickness Measurement for Arbitrary Time-Variant Thermal Profile

Ultrasonic thickness measurement of mechanical structures is one of the most popular and commonly used nondestructive methods for various kinds of process control and corrosion monitoring. With ultrasonic propagation speed being temperature-dependent, the thickness measurement can be performed reliably only when the thermal profile is completely known. Most conventional techniques assume the temperature of the test structure is uniform and at room temperature across its thickness. Such assumptions may lead to large errors in the thickness measurement, especially when there are significant temperature variations across the thickness. State-of-the-art techniques use external temperature measurements or implement iterative methods to compensate for the unknown thermal profiles. However, such techniques produce unsatisfactory results when the heat distribution is complex or varies rapidly with time. In this work, we propose a two-sensors technique, using both compressive and shear excitations, with a non-iterative rapid data processing method for accurate thickness measurement under arbitrary time-variant thermal profile. The independent behavior of shear and compressive waves is used to formulate a real-time thickness estimation technique. The developed technique is experimentally validated on a steel plate with fixed acoustic sensors. Test results show that the error in thickness estimation can be reduced by up to 98% compared to conventional thickness gauging methods.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Mounted Accelerometer Frequency Response of Adhesive Products and Aluminum Frame Quick Mounts

An accelerometer mounting technique has large implications on the frequency range and accuracy of the measurement, with stiffness and the mass relative to the monitored structure as the primary concerns. The International Organization for Standardization (ISO) gives an extensive list in 5348:2021, detailing mounting methods, and provides recommendations for testing mounts that are not specifically defined. In the nuclear industry on the laboratory scale, there is a need for vibration measurements for predictive maintenance and process monitoring that are nondestructive and capable of working in high-temperature environments. Commercial adhesive products with easy application and removal were tested as nondestructive methods, while quick mounts to a commonly used aluminum frame were tested as nondestructive and have potential applicability in high-temperature environments. The sinusoidal excitation method was used, measuring frequencies from 50 Hz to 10 kHz in one-third octave band intervals, utilizing three accelerometers and comparing the results to those obtained with the stud-mounting method. Using the lowest ±3 dB threshold across each accelerometer, foam dots and poster strips were not successful, and foam tapes were accurate up to 2000 Hz, hose clamps and zip ties up to 800 Hz, and a custom 3D printed mount up to 1000 Hz. Knowing the limitations of each mounting technique allows for accurate measurements within the appropriate range.

47 - OTHER INSTRUMENTATION↗

DOE OSTI2024

Anti-reflection coating with mullite and Duroid for large-diameter cryogenic sapphire and alumina optics

We developed a broadband two-layer anti-reflection (AR) coating for use on a sapphire half-wave plate (HWP) and an alumina infrared (IR) filter for the cosmic microwave background (CMB) polarimetry. Measuring the faint CMB B-mode signals requires maximizing the number of photons reaching the detectors and minimizing spurious polarization due to reflection with an off-axis incident angle. Sapphire and alumina have high refractive indices of 3.1 and are highly reflective without an AR coating. This paper presents the design, fabrication, quality control, and measured performance of an AR coating using thermally sprayed mullite and Duroid 5880LZ. This technology enables large optical elements with diameters of 600 mm. We also present a thermography-based nondestructive quality control technique, which is key to assuring good adhesion and preventing delamination when thermal cycling. We demonstrate the average reflectance of about 2.6% (0.9%) for two observing bands centered at 90/150 (220/280) GHz. At room temperature, the average transmittance of a 105 mm square test sample at 220/280 GHz is 83%, and it will increase to 90% at 100 K, attributed to reduced absorption losses. Therefore, our developed layering technique has proved effective for 220/280 GHz applications, particularly in addressing dielectric loss concerns. This AR coating technology has been deployed in the cryogenic HWP and IR filters of the Simons Array and the Simons observatory experiments and applies to future experiments such as CMB-S4.

Sakaguri, Kana (ORCID:0000000156678118)↗