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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 487 records · Page 27

Thermal Nondestructive Characterization of Corrosion in Boiler Tubes by Application fo a Moving Line Heat Source

Wall thinning in utility boiler waterwall tubing is a significant inspection concern for boiler operators. Historically, conventional ultrasonics has been used lor inspection of these tubes. This technique has proved to be very labor intensive and slow. This has resulted in a "spot check" approach to inspections, making thickness measurements over a relatively small percentage of the total boiler wall area. NASA Langley Research Center has developed a thermal NDE technique designed to image and quantitatively characterize the amount of material thinning present in steel tubing. The technique involves the movement of a thermal line source across the outer surface of the tubing followed by an infrared imager at a fixed distance behind the line source. Quantitative images of the material loss due to corrosion are reconstructed from measurements of the induced surface temperature variations. This paper will present a discussion of the development of the thermal imaging system as well as the techniques used to reconstruct images of flaws. The application of the thermal line source, coupled with this analysis technique, represents a significant improvement in the inspection speed for large structures such as boiler waterwalls while still providing high-resolution thickness measurements. A theoretical basis for the technique will be presented thus demonstrating the quantitative nature of the technique. Further, results of laboratory experiments on flat Panel specimens with fabricated material loss regions will be presented.

Cramer, K. Elliott↗

Use of Graph Theory and Neural Networks for Microstructural Classification

Recent advances in materials data analytics have provided new avenues for determining process-structure-property (PSP) linkages in a variety of materials. Machine learning techniques including few-shot learning have increased the efficiency of classifying microscopy images for the purposes of material characterization. Modifications in segmentation also show potential in improving the accuracy of our current pyCHIP classifier. Replacing previous encoders trained on ImageNet with those trained on microscopy images like MicroNet has initially shown better performance at classifying images of irradiated samples. Additionally, different normalization approaches were tested to show no discernable effect on classification. The Louvain method for community detection is analyzed on a set of irradiated samples with different parameters to determine which proved beneficial under what circumstances. We suggest that microscopy experiments be automated in the future using a combination of these techniques to enable high-throughput analyses.

36 MATERIALS SCIENCE↗

High strain-rate strength response of single crystal tantalum through in-situ hole closure imaging experiments

The properties of crystalline materials often depend on directionality and operating conditions. Specifically, the strength of materials can depend anisotropically on crystal direction and the loading condition. To probe these effects, a preliminary series of high strain-rate (> 105/s) strength plate-impact hole closure experiments were performed on high purity single crystal Tantalum cubes. The orientation of the single crystals with respect to impact/loading were varied to provide data to inform crystal plasticity modeling efforts. The experiments consist of in-situ high-resolution X-ray radiographic imaging of the hole collapse under dynamic compression conditions to infer the material strength via its resistance to closure at increasing levels of plastic strain. The experiments are compared against hydrocode simulation predictions. Here, a comparison with simple elastic perfectly plastic strength model predictions is presented to elucidate the response of the different crystal orientations at high strain-rate and large plastic strains.

36 MATERIALS SCIENCE↗

Development of Multimodal Few-Shot Analytics for Electron Micrographs

Recent advances in materials data analytics have provided new avenues for determining process-structure-property (PSP) linkages in a variety of materials. Machine learning techniques including few-shot learning have increased the efficiency of classifying microscopy images for the purposes of material characterization. Attempts at creating a multimodal approach can provide further improvements to current models and help extract more salient features from data. In this vein, raw spectrum data was taken to provide an additional modality to our current pyCHIP classifier. Modifications in segmentation also show potential in improving the accuracy of the pyCHIP classifier. Classifier output was analyzed using network graphs and unsupervised clustering algorithms such as spectral clustering to detect better segmentation methods than the current “chipping” approach. We suggest that the chip selection process can be automated in the future using a combination of these techniques to enable high-throughput analyses.

36 MATERIALS SCIENCE↗

Development and Application of In Situ Nanocharacterization to Photocatalytic Materials for Solar Fuel Generation

Photocatalytic materials offer an attractive approach for converting solar energy into chemical energy but the performance of the current generation of materials is insufficient to make a technology viable. To address this deficiency, it is necessary to develop a fundamental atomic level understanding of the functioning of such materials so that strategies can be developed to improve performance. This project was undertaken to explore the fundamental structure and properties of photocatalytic materials using atomic resolution imaging and spectroscopy techniques available on advanced transmission electron microscopy. Specifically, there is a need to develop an understanding of how atomic structures/defects and nanoparticle configurations regulate electronic, optical, and catalytic properties to facilitate the design of next generation photocatalysts for solar fuel production. The work focused on fundamental materials information that can be gained from advanced transmission electron microscopy study on novel and existing photocatalytic systems with an emphasis on the hydrogen evolution reaction (HER). Throughout the project, new instrumentation and microscopy characterization tools were developed. Two focus areas were: developing in situ TEM methods and advanced electron energy-loss spectroscopic for nanoscale analysis of catalysts. The work spanned a period of 12 years and for convenience, the report is divided into four phases, approximately corresponding to the four funding periods of the program. Most of the significant results are reported in archival journal publications.

36 MATERIALS SCIENCE↗

Dark-field X-ray microscopy with structured illumination for three-dimensional imaging

Dark-field X-ray microscopy is a lens-based technique that enables real-space imaging of heterogeneous micro- and meso-scale ordered materials. However, achieving accurate three-dimensional (3D) reconstruction often requires meticulous sample alignment or rastering, requiring complex rotational setups and extended acquisition times. To address these challenges, we introduce a structured illumination technique optimized for 3D imaging of ordered materials at sub-micrometer length scales. Our approach employs a coded aperture to spatially modulate the incident X-ray beam, enabling 3D structural reconstruction from images captured at various aperture positions. Unlike current 3D imaging approaches, which often rely on rotational or rastering methods, our technique uses scanning X-ray silhouettes of the coded aperture for depth resolution along the diffraction axis. This eliminates the need for sample rotation or rastering, resulting in a highly stable and efficient imaging modality. We validated the efficacy of this approach through experimental imaging of an isolated twin domain within a bulk single crystal of an iron pnictide using a dark-field X-ray microscope. This advancement aligns with the enhanced brightness upgrades of modern synchrotron radiation facilities, unlocking new possibilities for high-resolution imaging of ordered materials.

47 OTHER INSTRUMENTATION↗

A comparison of conventional and advanced ultrasonic inspection techniques in the characterization of TMC materials

Results obtained with a conventional ultrasonic inspection technique as well as those obtained with more advanced ultrasonic NDE methods in the characterization of an 8-ply quasi-isotropic titanium matrix composite (TMC) specimen are presented. Images obtained from a conventional ultrasonic inspection of TMC material are compared with those obtained using more sophisticated ultrasonic inspection methods. It is suggested that the latter techniques are able to provide quantitative images of TMC material. They are able to reveal the same potential defect indications while simultaneously providing more quantitative information concerning the material's inherent properties. Band-limited signal loss and slope-of-attenuation images provide quantitative data on the inherent material characteristics and defects in TMC.

Holland, Mark R.↗

Advanced Characterization of Thin Film Solar Cells

Polycrystalline thin-film solar cells have reached a levelized cost of energy that is competitive with all other sources of electricity. The technology has significantly improved in recent years, with laboratory cell efficiencies for cadmium telluride (CdTe), perovskites, and copper indium gallium diselenide (CIGS) each exceeding 22 percent. Both CdTe and CIGS solar panels are now produced at the gigawatt scale. However, there are ongoing challenges, including the continued need to improve performance and stability while reducing cost. Advancing polycrystalline solar cell technology demands an in-depth understanding of efficiency, scaling, and degradation mechanisms, which requires sophisticated characterization methods. These methods will enable reseachers and manufacturers to improve future solar modules and systems. This work provides researchers with a concise overview of the status of thin-film solar cell technology and characterization. Chapters describe material systems and their properties and then provide an in-depth look at relevant characterization methods and the learning facilitated by each of these. Following an introductory chapter, the book provides systematic and thorough coverage of the following topics: trends to improve CdTe solar cell performance; Cu(In,Ga)Se2 and related materials; perovskite solar cells; photovoltaic device modelling; luminescence and thermal imaging of thin-film photovoltaic materials, devices, and modules; application of spatially resolved spectroscopy characterization techniques on Cu2ZnSnSe4 solar cells; time-resolved photoluminescence characterization of polycrystalline thin-film solar cells; fundamentals of electrical material and device spectroscopies applied to thin-film polycrystalline chalcogenide solar cells; nanometer-scale characterization of thin-film solar cells by atomic force microscopy-based electrical probes; scanning transmission electron microscopy characterization of solar cells; photoelectron spectroscopy methods in solar cell research; time-of-flight secondary-ion mass spectrometry and atom probe tomography; and solid-state nuclear magnetic resonance characterization for photovoltaic applications. The final chapter provides an overview and describes future prospects.

41 EE - Solar Energy Technologies Office (EE-4S)↗

Bridging the Gap Between Microscale Modeling and Additive Manufacturing for TPS

An overview of the now open-source NASA ARC software PuMA will be provided. On top of the well-documented ability to import and compute material properties from micro-CT images, PuMA has the ability to design microstructures and compute/predict material properties such as: porosity, permeability, tortuosity, thermal and electrical conductivity, tensile strength, etc. Therefore, a whole new range of capabilities is available, and provides users with the ability to build TPS materials (both fibrous and woven types) and optimize their properties based on missions and requirements. This talk will aim to provide a seed to start bridging the gap between microscale modeling of TPS materials and additive manufacturing.

Conductivity↗

Specifications of EBR-II Neutron Radiography Method Description and Digitization Approach

All neutron radiography (NRAD) images of fuel pins in Argonne’s collection were originally generated using the NRAD imaging facility established in the Hot Fuel Examination Facility (HFEF) at Idaho National Laboratory (INL). The NRAD reactor facility was built in 1977 and has been operating since. The reactor is a TRIGA-type reactor operating at a power level of 250 kWth to provide a neutron source for radiography imaging. The reactor is equipped with two beam tubes (i.e., east beam tube and north beam tube) to guide the neutron beams to two radiography stations. The east radiography station is directly under the HFEF main cell and is dedicated for specimens already in the HFEF hot cell. The north radiography station is outside of the main HFEF hot cell and allows NRAD imaging of non-irradiated items. The NRAD images of EBR-II irradiated metallic fuel pins were taken in the east radiography station. Thermal neutrons have the capability to transmit through most materials and are ideal for NRAD imaging. However, because of their high thermal neutron absorption cross-section, fissile materials (e.g., highly-enriched nuclear fuels) may not be as transmissible to thermal neutrons. This is also the case for oversize specimens with extraneous thickness. Epithermal neutron imaging is therefore used as a complement to thermal neutron NRAD imaging. At HFEF’s NRAD facility, both thermal and epithermal neutrons can be used for NRAD imaging. Irradiated nuclear fuels emit high levels of γ radiation that can easily darken X-ray films, so direct exposure NRAD cannot be used to image them. Instead, an indirect NRAD imaging method was developed at HFEF’s NRAD facility. In this method, foils made of materials that can be activated by neutrons (i.e., with large neutron absorption cross section) are used to collect transmitted neutron signals. Then the activated foils are then placed against X-ray films and enclosed in a vacuum cassette so that the γ decay from the activated foils can produce images on the X-ray films. Then, general X-ray film processing procedures are used to digitize and store the images. By using different foil materials, different energy neutrons can be used for NRAD imaging. At the HFEF NRAD station, two types of films are commonly used: dysprosium (Dy) foils with thickness of 130 microns are used to capture thermal neutron signal, while indium (In) foils with thickness of 130 microns are used to capture epithermal neutron signal. A cadmium or gadolinium foil is put before the indium foil to work as a thermal neutron filter. The thermal and epithermal NRAD images can be taken simultaneously by using a Dy/Cd/In sandwiched foil combination. The typical NRAD exposure time is approximately 20 minutes. Then the exposed foils are transferred to film vacuum cassettes. The vacuum ensures that there is no gap between the foil and the film. The foil-to-film exposure time is at least three half-lives of the corresponding radioisotopes, which are 3 hours for In and 7.5 hours for Dy, respectively. Exposed films are processed using an automatic film processor to produce completed NRAD images.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Evaporated Se x Te 1-x Thin Films with Tunable Bandgaps for Short-Wave Infrared Photodetectors

Semiconducting absorbers in high-performance short-wave infrared (SWIR) photodetectors and imaging sensor arrays are dominated by single-crystalline germanium and III-V semiconductors. However, these materials require complex growth and device fabrication procedures. In this work, thermally evaporated Se x Te 1- x alloy thin films with tunable bandgaps for the fabrication of high-performance SWIR photodetectors are reported. From absorption measurements, it is shown that the bandgaps of Se x Te 1- x films can be tuned continuously from 0.31 eV (Te) to 1.87 eV (Se). Owing to their tunable bandgaps, the peak responsivity position and photoresponse edge of Se x Te 1- x film-based photoconductors can be tuned in the SWIR regime. By using an optical cavity substrate consisting of Au/Al 2 O 3 to enhance its absorption near the bandgap edge, the Se 0.32 Te 0.68 film (an optical bandgap of ≈0.8 eV)-based photoconductor exhibits a cut-off wavelength at ≈1.7 μm and gives a responsivity of 1.5 AW -1 and implied detectivity of 6.5 × 10 10 cm Hz 1/2 W -1 at 1.55 μm at room temperature. Importantly, the nature of the thermal evaporation process enables the fabrication of Se 0.32 Te 0.68 -based 42 × 42 focal plane arrays with good pixel uniformity, demonstrating the potential of this unique material system used for infrared imaging sensor systems.

36 MATERIALS SCIENCE↗

High-temperature thermal imaging to inform the arc-melt synthesis of nuclear materials

The advancement of nuclear energy technology necessitates the development of novel materials and synthesis methods to produce materials which enable new fuel cycles. Alongside the maturation of R&D scale technologies to produce these materials, there is an ongoing effort to develop in situ monitoring capabilities to reduce the time to the discovery and development of these fuels. Monitoring data can be leveraged in artificial intelligence platforms to detect phenomena which lead to varied macro- and microstructural features which impact the application and performance of samples synthesized. The present study presents early-stage findings of the implementation of high-temperature, high-frame-rate infrared thermal imaging to monitor the arc-melt synthesis of novel fuels and compounds relevant to advanced nuclear reactors. The study illustrates both the challenges and opportunities of this methodology, highlighting the importance of internal standards while determining emissivity and transmission values as well as visualizing volatilization during melt synthesis.

Stone, Jordan↗

Using block-copolymer nanolithography as a tool to sensitively evaluate variation in chemical dry etching rates of semiconductor materials with sub-5 nm resolution

Ion implantation is a robust and established method to customize the electronic properties of Si. However, fabricating doped, ultrafine semiconductor nanostructures can be challenging. Ion implantation has well-established effects on the dry etch rates of Si, which becomes increasingly consequential as the target dimension shrinks below a few tens of nanometers. While dry etching arrays of block copolymer-templated nanoscale holes (pitch = 37.5 nm, diameter ~25 nm) into p-type, n-type, and undoped Si, we observed that the lateral etch rate was notably larger for the n-type regions than p-type or undoped regions. By doing image analyses on high resolution electron micrographs of the nanostructured hole arrays, we were able to extract the porosity and average radii of the holes with subnanometer sensitivity and compare the relative etch rates between different doping conditions. We found that degenerately doped n-type silicon consistently etches between approximately 17% and 27% faster in the lateral direction than p-type Si, resulting in significantly larger porosity and, consequently, less mechanical stability. Here, we demonstrate that top-down dimensional analysis of a densely packed porous nanostructure is a robust method for assessing extremely small differences in the lateral, chemical etch rate of doped Si to a degree of sensitivity that was previously unachievable. The minute, dense-packed nature of block copolymer self-assembled nanostructures is shown to be ideal for this application. This proposed method could be useful for designing fabrication processes for heterogeneous nanostructures, as slight dry etch rate variations that may be within process tolerance at the micrometer-scale appear to have nontrivial consequences at the nanometer scale.

42 ENGINEERING↗

4D-STEM of Beam-Sensitive Materials

We report that a scanning electron nanobeam diffraction, or 4D-STEM (four-dimensional scanning transmission electron microscopy), is a flexible and powerful approach to elucidate structure from "soft" materials that are challenging to image in the transmission electron microscope because their structure is easily damaged by the electron beam. In a 4D-STEM experiment, a converged electron beam is scanned across the sample, and a pixelated camera records a diffraction pattern at each scan position. This four-dimensional data set can be mined for various analyses, producing maps of local crystal orientation, structural distortions, crystallinity, or different structural classes. Holding the sample at cryogenic temperatures minimizes diffusion of radicals and the resulting damage and disorder caused by the electron beam. The total fluence of incident electrons can easily be controlled during 4D-STEM experiments by careful use of the beam blanker, steering of the localized electron dose, and by minimizing the fluence in the convergent beam thus minimizing beam damage. This technique can be applied to both organic and inorganic materials that are known to be beam-sensitive; they can be highly crystalline, semicrystalline, mixed phase, or amorphous. One common example is the case for many organic materials that have a π-π stacking of polymer chains or rings on the order of 3.4-4.2 Å separation. If these chains or rings are aligned in some regions, they will produce distinct diffraction spots (as would other crystalline spacings in this range), though they may be weak or diffuse for disordered or weakly scattering materials. We can reconstruct the orientation of the π-π stacking, the degree of π-π stacking in the sample, and the domain size of the aligned regions. This Account summarizes illumination conditions and experimental parameters for 4D-STEM experiments with the goal of producing images of structural features for materials that are beam-sensitive. We will discuss experimental parameters including sample cooling, probe size and shape, fluence, and cameras. 4D-STEM has been applied to a variety of materials, not only as an advanced technique for model systems, but as a technique for the beginning microscopist to answer materials science questions. It is noteworthy that the experimental data acquisition does not require an aberration-corrected TEM but can be produced on a variety of instruments with the right attention to experimental parameters.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Editorial: Applications of spectroscopy and chemometrics in nuclear materials analysis

Optical analysis techniques, including spectroscopy and image analysis, have many advantages when applied to the study of nuclear materials. They require small sample sizes, can be performed remotely, and can be proceduralized through consistent practice. Most importantly, they provide a wealth of information by generating multivariate data. For example, ultraviolet–visible–near-infrared absorbance spectroscopy of actinides in aqueous and organic solutions is dependent on the oxidation state, anionic complexation, and temperature. These variables are important for solution-based separation processes, and sensitivity to these factors, combined with online monitoring, can drive the efficiency and control of these processes. The morphology and chemical composition of actinide particles can also provide a vital clue to the mechanisms by which the particles were formed, providing forensic information on the origins of the particles.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Two-Dimensional Nonlinear Finite Element Analysis of CMC Microstructures

Detailed two-dimensional finite element analyses of the cross-sections of a model CVI (chemical vapor infiltrated) SiC/SiC (silicon carbide fiber in a silicon carbide matrix) ceramic matrix composites are performed. High resolution images of the cross-section of this composite material are generated using serial sectioning of the test specimens. These images are then used to develop very detailed finite element models of the cross-sections using the public domain software OOF2 (Object Oriented Analysis of Material Microstructures). Examination of these images shows that these microstructures have significant variability and irregularity. How these variabilities manifest themselves in the variability in effective properties as well as the stress distribution, damage initiation and damage progression is the overall objective of this work. Results indicate that even though the macroscopic stress-strain behavior of various sections analyzed is very similar, each section has a very distinct damage pattern when subjected to in-plane tensile loads and this damage pattern seems to follow the unique architectural and microstructural details of the analyzed sections.

Mital, Subodh K.↗

Rotational Millimeter-Wave Shoe Scanner Using the Discrete Fourier Transform for Backprojection-Based Image Reconstruction

An active 3D microwave / millimeter-wave shoe scanner was previously developed at the Pacific Northwest National Laboratory (PNNL) using two linear arrays scanned over a rectilinear aperture. The radar system chirps a frequency sweep from 10-40 GHz. These frequencies allow imaging through optically opaque material such as leather, rubber, plastics, and other dielectrics. The system was designed to detect concealed items in the soles of shoes while allowing people to leave their shoes on through a security checkpoint. To shrink the footprint of the system, a new iteration of the design has been developed that scans the two linear arrays over a circular aperture. This new footprint opens the possibility of it being installed in the floor of a cylindrical millimeter-wave body scanner. The backprojection-based multilayer dielectric image reconstruction developed at PNNL can easily handle arbitrary spatial sampling, accommodating the new rotational shoe scanner design. Commonly, the fast Fourier transform (FFT) is used to efficiently compute the range response from the data collected by the system as a preprocessing step to the backprojection algorithm. It was found that converting to range using the discrete Fourier transform (DFT) directly has some advantages over the FFT. For example, nonlinear and non-uniform frequency sweeps can easily be compensated for during the computation of the DFT and only the range bins of interest need to be computed and their spacing can be chosen arbitrarily. Because the range conversion step of the image reconstruction is the fastest part of the process there is very little speed penalty for using the DFT over the FFT and it can even increase the speed of image reconstruction when the ranges of interest are fewer than the total span that is calculated in the FFT.

Millimeter-wave imaging, microwave imaging, shoe s↗