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DOE OSTI2023

Machine Learning Enabled Sensor Fusion for In-Situ Defect Detection in Laser Powder Bed Fusion

Laser Powder Bed Fusion (L-PBF) Additive Manufacturing (AM) is among the metal 3D printing technologies most broadly adopted by the manufacturing industry. The current industry qualification paradigm for critical-application L-PBF parts relies heavily on expensive non-destructive inspection techniques such as X-Ray Computed Tomography (XCT), which significantly limits the use-cases of L-PBF. In situ monitoring of the process promises a less expensive alternative to ex situ testing, but existing sensor technologies and data analysis techniques struggle to detect sub-surface flaws (e.g., porosity and cracking) on production-scale L-PBF printers. RTX Technologies Research Center (RTRC) has licensed ORNL’s Peregrine software package – a printer- and camera-agnostic data analytics tool designed specifically for detecting process anomalies using in situ data collected during powder bed printing. The goal of this project was to feed temporally rich, multi-modal sensor data, including visible light, integrated near infrared (NIR), and spatially mapped co-axial melt pool thermal emission data into Peregrine to enable detection of subsurface flaws. XCT data was used as ground truth training data to allow Peregrine’s deep learning algorithms to recognize anomalies in these complex data streams in both test artifacts and industrially relevant geometries. Completion of this program has seen the successful implementation of multi-modal, multi-layer sensor data footprints for training of machine learning models in Peregrine. Flaws detected in XCT data have been successfully detected directly from this in situ data footprint, and initial analyses of the in situ probability-of-detection has been conducted, showing performance levels commensurate with traditional non-destructive evaluation (NDE) methods. The in situ monitoring methodology was then applied to an industrially relevant component that was using post-build NDE, highlighting the utility of the proposed method for hard-to-inspect AM components. As a direct result of this program, two journal manuscripts [1], [2] have been published in Additive Manufacturing, with additional manuscripts planned following program completion.

36 MATERIALS SCIENCE↗

DOE OSTI2025

In-Situ Process Monitoring Evaluation and Demonstration using Advanced Characterization with Laser Powder Bed Systems

Oak Ridge National Laboratory’s (ORNL) Manufacturing Demonstration Facility (MDF) worked with EOS Group to evaluate the current in-situ sensor capabilities of an EOS M290 Laser Powder Bed Fusion machine. The M290 was fitted with a 1 Mega-Pixel (MP) grayscale visible-light camera and a 5 MP temporally integrated (TI) near-infrared (NIR) camera. One print from stainless steel (SS) 316 and two from Inconel 625 (IN625) were performed where data including in-situ imaging and a machine log file were captured. These data were subsequently analyzed using a Dynamic Multi-Scale Segmentation Convolutional Neural Network (DMSCNN) trained on user defined classes and correlated to as-printed flaws, in the form of porosity, discovered in X-Ray Computed Tomography (XCT). In Phase I, two indications were detected in-situ and spatially correlated to stochastic lack-of-fusion flaws discovered using XCT. In Phase II, using these links from in-situ signatures to XCT flaw populations, a second neural network (NN) was trained to create a Voxelized Property Prediction Model (VPPM) to predict porosity percentages within the part using only features garnered from the in-situ data from two IN625 complex geometries. The VPPM was able to accurately predict porosity values for IN625 parts with an R 2 value of 0.764.

36 MATERIALS SCIENCE↗

DOE OSTI2025

In-Situ Process Monitoring Evaluation and Demonstration using Advanced Characterization with Laser Powder Bed Systems

36 MATERIALS SCIENCE↗

NASA NTRS2017

X-Ray Computed Tomography: The First Step in Mars Sample Return Processing

The Mars 2020 rover mission will collect and cache samples from the martian surface for possible retrieval and subsequent return to Earth. If the samples are returned, that mission would likely present an opportunity to analyze returned Mars samples within a geologic context on Mars. In addition, it may provide definitive information about the existence of past or present life on Mars. Mars sample return presents unique challenges for the collection, containment, transport, curation and processing of samples [1] Foremost in the processing of returned samples are the closely paired considerations of life detection and Planetary Protection. In order to achieve Mars Sample Return (MSR) science goals, reliable analyses will depend on overcoming some challenging signal/noise-related issues where sparse martian organic compounds must be reliably analyzed against the contamination background. While reliable analyses will depend on initial clean acquisition and robust documentation of all aspects of developing and managing the cache [2], there needs to be a reliable sample handling and analysis procedure that accounts for a variety of materials which may or may not contain evidence of past or present martian life. A recent report [3] suggests that a defined set of measurements should be made to effectively inform both science and Planetary Protection, when applied in the context of the two competing null hypotheses: 1) that there is no detectable life in the samples; or 2) that there is martian life in the samples. The defined measurements would include a phased approach that would be accepted by the community to preserve the bulk of the material, but provide unambiguous science data that can be used and interpreted by various disciplines. Fore-most is the concern that the initial steps would ensure the pristine nature of the samples. Preliminary, non-invasive techniques such as computed X-ray tomography (XCT) have been suggested as the first method to interrogate and characterize the cached samples without altering the materials [1,2]. A recent report [4] indicates that XCT may minimally alter samples for some techniques, and work is needed to quantify these effects, maximizing science return from XCT initial analysis while minimizing effects.

Welzenbach, L. C.↗

NASA NTRS2018

Calculating the Modal Mineralogy of Aubrite Meteorites Using X-Ray Computed Tomography

The aubrites are a group of differentiated meteorites that formed in extremely reducing conditions, with oxygen fugacities (ƒO2) ranging from ~2 to ~6 log units below the Iron-Wüstite buffer. At these extreme conditions, elements that are lithophile (silica-loving) on Earth can behave as chalcophiles (sulfur-loving) or siderophiles (metal-loving), and FeO-poor silicates and exotic sulfides can form. Elemental partitioning among minerals at these conditions are still not well understood, thus studying aubrites could help better constrain elemental behavior. Only 30 aubrites exist; however, they display various textures, which can be difficult to identify in small samples. Identifying composite clasts can help in understanding the igneous history of the aubrite parent bodies. In order to distinguish different minerals and textures in larger samples, we use X-ray computed tomography (XCT), which is a useful, non-destructive analysis that can produce a 3D representation of a meteorite's textures, structures, and modal mineralogy. This study investigates the Norton County aubrite using XCT. Norton County is a fragmental impact breccia aubrite, and was an observed fall with a main mass of 1.1 tons. This large amount of material offers an opportunity to investigate a great volume of reduced, aubritic sample and study a more diverse variety of clasts. Here we report XCT results of two samples of Norton County (NC 15417) in order to constrain the 3D modal mineralogy of silicates, sulfides, and metals, and to identify unique clasts within the matrix.

Wilbur, Zoe↗

NASA NTRS2019

A New Look at Aubrites: Investigating 3D Modal Mineralogy with X-Ray Computed Tomography

The aubrites (approximately 30 known meteorites) are a unique group of differentiated meteorites that formed on asteroids with oxygen fugacities (ƒO2) from approximately 2 to approximately 6 log units below the iron-wustite buffer. At these highly reduced conditions, elements deviate from the geochemical behavior exhibited at terrestrial ƒO2, forming FeO-poor silicates and exotic sulfides. While previous studies have described the petrology and 2D modal abundances of aubrites, this work investigates the 3D modal mineralogies of silicate, metal, and sulfide phases in aubrite samples, which are then compared to the available 2D data. In addition to 3D modal mineralogies, we have examined the geochemistry of fourteen aubrites, including mineral major-element compositions, bulk-rock compositions, and oxygen isotopic compositions to understand their formation and evolution at extreme ƒO2 conditions. We utilize X-ray computed tomography (XCT) to non-destructively analyze the distribution and abundances of mineral phases in aubrites and locate composite clasts of sulfide grains for future analytical study. In order to better constrain elemental behavior under reduced conditions, we specifically target minerals phases that comprise moderately volatile elements (i.e. oldhamite [CaS], caswellsilverite [NaCrS2] and djerfisherite [K6Na(Fe,Cu,Ni)25S26Cl]) as it has been shown that their geochemical behavior changes as a function of ƒO2. Currently, we have produced 3D scans of the Norton County aubrite. The results of the XCT data have allowed for the determination of the abundances of silicate groundmass (i.e., enstatite, forsterite, albite, and diopside), light (based on electron density) sulfides (i.e. alabandite [MnS] and daubréelite [FeCr2S4]), heavy (based on electron density) sulfides (i.e., troilite [FeS]), and Fe,Ni metal by segmenting a density histogram in Volume Graphics Studio software. XCT scans of additional aubrites are underway. By combining the 3D representation of the exotic phases found in aubrites with existing 2D characterizations, we are able to better determine modal abundances. By integrating 3D and 2D modal abundances and geochemistry, we can ultimately better constrain aubrite petrogenesis and elemental partitioning under reduced conditions. Furthermore, application of this new 3D approach offers the opportunity to identify and select clasts for future study prior to cutting the sample, which will minimize sample loss of this precious material.

Wilbur, Zoe↗

NASA NTRS2019

Using X-Ray Computed Tomography as a Tool for Preliminary Examination Tool of Current and Future Extraterrestrial Sample Return Missions

The Astromaterials Acquisition and Curation Office at the Johnson Space Center is the past, present, and future home of all of NASA’s astromaterials sample collections. The primary goals of the curation office are to maintain the long-term integrity of the samples and ensure that the samples are distributed for scientific study in a fair, timely, and responsible manner, thus maximizing the return on each sample. Part of the curation process is planning for the future. To this end, we perform fundamental research in advanced curation initiatives to better prepared for future sample return missions. Advanced Curation is tasked with developing procedures, technology, and data sets necessary for curating new sample collections, or getting new results from existing sample collections. As part of these advanced curation efforts, we have installed and are operating a Nikon XTH 320 X-ray Computed Tomography(XCT) system in the JSC curation office with four interchangeable X-ray sources, a large-area detector, and a heavy-duty stage. These instrument characteristics allow us exceptional flexibility to analyze a wide range of sample sizes, from sub-mm soil particles to rocks >10 cm in diameter. The penetrative nature of the XCT scans allows for astromaterials samples to be analyzed within sealed low-density containers (e.g., Teflon bags), preserving the pristinity of the samples. We have begun scanning of the Apollo and Antarctic Meteorite sample suites in order to non-destructively map out lithic clasts (and other features) within the samples. The data from these scans will be made available to scientists via the JSC curation website and the Astromaterials Curation Newsletter. We anticipate sample requests from these “new” lithic clasts identified in these “old” samples. We also anticipate that XCT analyses like these would be useful for future sample return missions, like the OSIRIS REx mission, as well as future sample return missions.

Zeigler, Ryan↗

NASA NTRS2020

Using X-Ray Computed Tomography to Image Apollo Drive Tube 73002

The Apollo missions collected 382 kg of rock, regolith, and core samples from six locations on the nearside of the Moon. Today, just over 84% by mass of the Apollo collection remains in pristine condition within the curation facility at Johnson Space Center. Most Apollo samples have been well characterized, however there are several types of samples that have remained wholly or largely unstudied since their return, and/or that have been curated under special conditions. These sample types are: (1) unopened samples sealed under vacuum on the Moon; (2) unopened (but unsealed) drive tubes; (3) Apollo 17 samples frozen shortly after their return; and (4) Apollo 15 samples opened and stored in a helium atmosphere since their return. Last summer, NASA solicited proposals for the Apollo Next Generation Sample Analysis Program (ANGSA), and 9 teams were selected to study: (1) unsealed, unopened drive tube 73002; (2) sealed, unopened drive tube 73001 (paired with 73002); and (3) a subset of the frozen and He-purged samples [1]. The first sample opened as part of the ANGSA program was drive tube 73002. This is a 30 cm long, 4 cm diameter drive tube collected on a landslide deposit near Lara Crater at the Apollo 17 landing site. It was part of a 60 cm long double drive tube collected, and the bottom half of the tube (73001) was sealed under vacuum on the Moon [2]. Prior to opening sample 73002, the sample was imaged with a high resolution Xray Computed Tomography (XCT) scan of the entire tube. Additional XCT scans have been made of “large” clasts removed from the core as part of the dissection process [3]. Here we present a first look at the XCT data from 73002, and talk about the utility of the scans as part of the curation process, including the potential for future science returns from the high resolutions scans.

Zeigler, R. A.↗

NASA NTRS2020

Applicability and Utility of the Astromaterials X-Ray Computed Tomography Laboratory at Johnson Space Center

The Astromaterials Acquisition and Curation Office at NASA’s Johnson Space Center is responsible for curating all of NASA’s astromaterial sample collections (i.e. Apollo samples, Luna Samples, Antarctic Meteorites, Cosmic Dust Particles, Microparticle Impact Collection, Genesis solar wind atoms, Stardust comet Wild-2 particles, Stardust interstellar particles, and Hayabusa asteroid Itokawa particles) [1-3]. To assist in sample curation and distribution, JSC Curation has recently installed an X-ray computed tomography (XCT) scanner to visualize and characterize samples in 3D. [3] describes the instrumental set-up and the utility of XCT to astromaterials curation. Here we describe some of the current and future projects and illustrate the usefulness of XCT in studying astromaterials.

Eckley, S. A.↗

NASA NTRSDate not supplied

Using X-Ray Computed Tomography to Image Apollo Drive Tube 73002

The Apollo missions collected 382 kg of rock, regolith, and core samples from six locations on the nearside of the Moon. Today, just over 84% by mass of the Apollo collection remains in pristine condition within the curation facility at Johnson Space Center. Most Apollo samples have been well characterized, however there are several types of samples that have remained wholly or largely unstudied since their return, and/or that have been curated under special conditions. These sample types are: (1) unopened samples sealed under vacuum on the Moon; (2) unopened (but unsealed) drive tubes; (3) Apollo 17 samples frozen shortly after their return; and (4) Apollo 15 samples opened and stored in a helium atmosphere since their return. NASA solicited proposals for the Apollo Next Generation Sample Analysis Program (ANGSA), and 9 teams were selected to study: (1) unsealed, unopened drive tube 73002; (2) sealed, unopened drive tube 73001 (paired with 73002); and (3) a subset of the frozen and He-purged samples [1]. The first sample opened as part of the ANGSA program was drive tube 73002. This was originally a ~30 cm long, 4 cm diameter drive tube collected on a landslide deposit near Lara Crater at the Apollo 17 landing site. It was part of a ~60 cm long double drive tube collected, and the bottom half of the tube (73001) was sealed under vacuum on the Moon [2]. Prior to opening sample 73002, the sample was imaged with a high resolution X-ray Computed Tomography (XCT) scan of the entire tube. Additional XCT scans have been made of “large” clasts removed from the core as part of the dissection process [3]. Here we present the whole tube and close-up XCT data from 73002, and talk about the utility of the scans as part of the curation process, including the potential for future science returns from the high resolutions scans.

R A Zeigler↗

DOE OSTI2025

Impacts of Biomass Feedstock Pre-Processing on Heat and Mass Transfer During Pyrolysis Using X-Ray Computed Tomography and Multiscale Modeling

Knowledge of the transport properties of biomass particles such as porosity, tortuosity, and permeability is paramount for high-fidelity modeling of biomass pyrolysis due to the heat and mass transfer limitations imposed by particle microstructure. X-ray computed tomography (XCT) is a non-destructive imaging method that enables full 3D reconstructions of the biomass particle microstructure with high resolution, permitting direct calculation of porosity, tortuosity, and permeability from real particle geometries. In this study, XCT imaging revealed the 3D microstructures of particles and chars from pyrolytic conversion of cylindrically cut or milled/pelletized loblolly pine samples. The porosity, tortuosity, and permeability were calculated directly from the XCT geometries via open-source microstructural analysis tool MATBOX+TauFactor (https://github.com/NREL/MATBOX_Microstructure_analysis_toolbox) and computational fluid dynamics (CFD) simulations using our solver, Mesoflow (https://github.com/NREL/mesoflow). These properties were used in a reactor scale model developed in COMSOL of the single particle reactor at NREL to investigate the impact of feedstock pre-processing on biomass conversion during pyrolysis with rigorous experimental validation.

biomass↗

DOE OSTI2026

Process-driven roadmap for depositing super duplex stainless steel via wire Arc additive manufacturing

Here, this study systematically investigates the effects of shielding gas, bead spacing, weld mode, and travel speed on the phase balance, porosity, and hardness of wire arc additively manufactured (WAAM) super duplex stainless steel (ER2594). Robotic WAAM was employed to fabricate multilayer walls under systematically varied process conditions, followed by phase transformation simulations, X-ray computed tomography (XCT), electron backscatter diffraction (EBSD), and microhardness evaluation. Thermodynamic simulations predicted rapid cooling of AM process can suppress the potential formation of deleterious precipitates which was later validated via cross-sectional microstructure analyses of printed samples. XCT revealed porosity levels below 0.2% for all deposits, with reduced travel speed significantly lowering defect volume. Microstructural analyses revealed the evolution of various austenite precipitates, including grain boundary austenite (GBA), Widmanstätten austenite (WA), and intergranular austenite (IGA), sequentially upon cooling of the ferrite phase. Among all process parameters, weld transfer mode exhibited the strongest influence on phase balance; pulsed mode promoted higher ferrite retention (~ 36%) compared to RapidX mode. No consistent relationship between stabilized phase fraction and captured microhardness was observed. This work provides critical insights for optimizing WAAM parameters to control phase balance and mechanical performance, which is essential for producing high-integrity super duplex stainless-steel components for nuclear and marine applications.

Grain orientation↗

DOE OSTI2025

Formation of Composite SiC/SiC Joints by Embedded Wire Chemical Vapor Deposition

The joining of ceramic monoliths or composites to date has primarily been limited to the formation of brittle monolithic joints using heterogeneous (dissimilar) materials, similar to brazing in metals. The development of a damage-tolerant joint layer by SiC fiber reinforcements is demonstrated here. Tube workpieces made of SiC fiber-SiC matrix composite are joined using a nonwoven SiC fiber mat densified by embedded wire chemical vapor deposition (EWCVD), creating a fiber-reinforced weld-like joint by homogeneous joining. EWCVD uses a localized heating method to target deposition and growth to the joint region specifically, while minimizing thermal damage to the surrounding composite tube material. X-ray computed tomography (XCT) is used to nondestructively characterize as-made joints for relative density, adhesion, and composition. In situ XCT analysis during mechanical testing revealed crack deflections in the bonding layer, which indicates a toughening mechanism typical of ceramic matrix composite phase. Gas permeation testing of these proof-of-concept composite joints identified relatively high leak rates in comparison to fully coated SiC/SiC composite tube workpieces. In conclusion, the novelty of the composite joining method and current technology challenges, including gas permeability, are discussed in comparison with traditional ceramic joints and materials.

SiC↗

DOE OSTI2023

Nondestructively Visualizing and Understanding the Mechano-Electro-chemical Origins of “Soft Short” and “Creeping” in All-Solid-State Batteries

All-solid-state Li-metal batteries (ASLMBs) represent a significant breakthrough in the quest to overcome limitations associated with traditional Li-ion batteries, particularly in energy density and safety aspects. However, widespread implementation is stymied due to a lack of profound understanding of the complex mechano-electro-chemical behavior of Li metal in the ASLMBs. Herein, operando neutron imaging and X-ray computed tomography (XCT) are leveraged to nondestructively visualize Li behaviors within ASLMBs. This approach offers real-time observations of Li evolutions, both pre- and post- occurrence of a “soft short”. The coordination of 2D neutron radiography and 3D neutron tomography enables charting of the terrain of Li metal deformation operando. Concurrently, XCT offers a 3D insight into the internal structure of the battery following a “soft short”. Despite the manifestation of a “soft short”, the persistence of Faradaic processes is observed. To study the elusive “soft short”, phase field modeling is coupled with electrochemistry and solid mechanics theory. The research unravels how external pressure curbs dendrite growth, potentially leading to dendrite fractures and thus uncovering the origins of both “soft” and “hard” shorts in ASLMBs. Furthermore, by harnessing finite element modeling, it dive deeper into the mechanical deformation and the fluidity of Li metal.

25 ENERGY STORAGE↗

DOE OSTI2021

Identifying build orientation of 3D-printed materials using convolutional neural networks

The advent of additive manufacturing (AM) processes brought with it intense research into various materials and manufacturing processes. At the same time, the need for validation of material properties, as well as study and forecasting of aging, has arisen. Modern imaging techniques, like X-ray computed tomography (XCT), are a convenient vehicle for such studies; however, the large datasets they produce require novel analysis techniques to efficiently extract critical information. Here, we present our work on developing a 3D extension of the ResNet architecture to distinguish between two build orientations of tensile bars produced by AM. Using only information from XCT, our method achieves a 99.3% correct classification at a misidentification of 1%.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Scalable in situ non-destructive evaluation of additively manufactured components using process monitoring, sensor fusion, and machine learning

Laser Powder Bed Fusion (L-PBF) Additive Manufacturing (AM) is among the metal 3D printing technologies most broadly adopted by the manufacturing industry. However, the current industry qualification paradigm for critical-application L-PBF parts relies heavily on expensive non-destructive inspection techniques, which significantly limits the use-cases of L-PBF. In situ monitoring of the process promises a less expensive alternative to ex situ testing, but existing sensor technologies and data analysis techniques struggle to detect sub-surface flaws (e.g., porosity and cracking) on production-scale L-PBF printers. In this work, an in situ NDE (INDE) system was engineered to detect subsurface flaws detected in X-Ray Computed Tomography (XCT) directly from process monitoring data. A multilayer, multimodal data input allowed the INDE system to detect numerous subsurface flaws in the size range of 200–1000µm using a novel human-in-the-loop annotation procedure. Furthermore, a framework was established for generating probability-of-detection (POD) and probability-of-false-alarm (PFA) curves compliant with NDE standards by systematically comparing instances of detected subsurface flaws to post-build XCT data. Here, we also introduce for the first time in the AM in situ sensing literature the a 90/95 – the flaw size corresponding to a 90% detection rate on the lower 95% confidence interval of the POD curve. The INDE system successfully demonstrated POD capabilities commensurate with traditional NDE methods. Traditional ML performance metrics were also shown to be inadequate for assessing the ability of the INDE system’s flaw detection performance. It is the hope of the authors that future studies will adopt the POD and PFA approach outlined here to provide better insight into the utility of process monitoring for AM.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Qualitative and quantitative analysis of neutron irradiation effects in SiC/SiC composites using X-ray computed tomography

Silicon carbide fiber-reinforced silicon carbide matrix (SiC/SiC) composites are candidate materials for cladding of light water reactor (LWR) fuels. Loss of fission product gas retention due to the formation of microcrack networks is considered a potential failure mechanism for SiC/SiC-cladded fuels. In this work, a variety of SiC/SiC composite tubes were irradiated with and without an LWR-relevant radial heat flux in the High Flux Isotope Reactor, followed by detailed characterization with X-ray computed tomography (XCT). This first set of XCT data for neutron-irradiated samples confirmed that the internal stresses arising from a combination of temperature gradients and irradiation-induced swelling act as the primary driver for cracking. Consequently, while the observed cracking patterns varied depending on the tube architectures, the sharp edges of relatively large pores were found to be the common stress concentrator. These findings are useful to help improve the design and manufacturing of SiC/SiC fuel claddings for reduced failure probability.

42 ENGINEERING↗

DOE OSTI2025

Fabrication of porous transport electrodes: Development of quantitative approach for quality control

This work focuses on porous transport electrodes (PTEs), which integrate the anodic catalyst with the adjacent Ti porous transport layer (PTL). Challenges in catalyst deposition on PTLs, particularly at low loadings, motivated this study to evaluate various fabrication methods and characterization approaches. This work investigated Pt-treated PTLs coated with Ir-based catalysts using several common methods, including airbrush coating, rod coating, ultrasonic spray coating, electrodeposition, and sputter deposition, with catalyst loadings ranging from 2.9 to 0.1 mg/cm 2 , providing the opportunity for comparisons across a large set of samples produced by different methods. Two widely accessible characterization techniques: X-ray computed tomography (XCT) and scanning electron microscopy energy dispersive X-ray spectroscopy (SEM-EDS) were explored. Initial evaluation of selected samples with XCT provided qualitative insights into catalyst distribution, however comprehensive quantitative analysis was limited. SEM-EDS enabled detailed information on the catalyst distribution both qualitatively and quantitatively using two metrics. Atomic and surface area % ratios of Pt:Ir and Ti:Ir revealed trends in catalyst loading and losses into the PTL pores, as well as evaluating the homogeneity of catalyst coatings. The analysis demonstrated that ultrasonic spray coating, electrodeposition, and sputter coating produced the most homogeneous coatings, with minimal catalyst losses observed for electrodeposition and sputter coating. By adapting common techniques with novel, standardized methodologies, this work establishes a universally applicable framework for cross-study comparison of PTEs. The SEM-EDS approach provides a practical, accessible tool for PTE characterization and contributes a reference dataset supporting both research development and rapid quality control.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗