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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 307 records · Page 17
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Blade-Type Reaction Front in Micrometer-Sized Germanium Particles during Lithiation

To investigate the lithium transport mechanism in micrometer-sized germanium (Ge) particles, in situ focused ion beam-scanning electron microscopy was used to monitor the structural evolution of individual Ge particles during lithiation. Our results show that there are two types of reaction fronts during lithiation, representing the differences of reactions on the surface and in bulk. Further, the cross-sectional SEM images and transmission electron microscopy characterizations show that the interface between amorphous Li x Ge and Ge has a wedge shape because of the higher Li transport rate on the surface of the particle. The blade-type reaction front is formed at the interface of the amorphous Li x Ge and crystalline Ge and is attributed to the large strain at the interface.

25 ENERGY STORAGE↗
DOE OSTI2023

A Sustainable and Environmentally Friendly Concrete for Structural Applications

The purpose of this study is to utilize waste products—precipitated calcium carbonate (PCC) and upcycled recycled concrete aggregate (upcycled RCA or UCA)—in civil works projects. To do so, tests must be performed to determine the engineering properties of the materials in which PCC and UCA are sequestered. PCC is a fine to coarse grain waste product generated during the production of sugar from sugar beets. UCA is produced from demolished and returned concrete by the extraction of primarily calcium and alkalinity. The study also includes the use of both PCC and UCA in the same concrete mix design. The test results on PCC alone show that the optimum content to achieve a minimum 28 MPa (4000 psi) compressive strength is 25% and 30%. The corresponding compressive strength of mixes in which conventional aggregate was replaced by UCA is about 48 MPa (7000 psi) to 55 MPa (8000 psi) at the same water: cement ratio (0.44) by weight. The compressive strength of concrete with 25% to 30% cement replaced by PCC and varying aggregates replaced with UCA ranges from 19.3 to 40 MPa (2800 to 5800 psi). Other tests on PCC and UCA include tensile strength of 2 to 3 MPa (293 to 423 psi) and flexural strength of 1.3 to 1.9 MPa (183 to 279 psi). Analytical techniques such as X-ray diffraction (XRD), energy-dispersive X-ray spectrometry (EDX), and scanning electron microscopy (SEM) were used to identify the constituent elements and chemical compounds present in PCC, including calcium carbonate and silica. Based on the test results, the composition of PCC by weight indicates 45.9% calcium, 39.4% oxygen, and 9.2% carbon. Based on the results of this study, we can expect to reduce carbon emissions in the production of cement and aggregates, as well as utilize waste products in the civil engineering field.

42 ENGINEERING↗
DOE OSTI2020

Novel PBX formulations containing thermally-expandable microspheres for on-demand control of explosive behavior

In this work, we present the formulation and analysis of inert Plastic-Bonded eXplosive (PBX)-surrogates loaded with thermally expandable microspheres (TEMs). TEMs consist of a thermoplastic acrylonitrile shell (10-50 µm diameter) encapsulating an inert low boiling hydrocarbon. Upon heating, the TEMs expand as the shell softens while the hydrocarbon gasifies, increasing the internal pressure and expanding the particle by as much as 120 vol%. We hypothesize that TEM expansion within a PBX will introduce tunable changes in local density and porosity, and ultimately the shock sensitivity. This paper focuses on microstructural analysis of surrogate PBX-TEM formulations, both before and after thermally- induced TEM expansion. The formulations were analyzed by scanning electron microscopy (SEM), ultra-small angle neutron scattering (USANS), and X-ray Computed Tomography (x-ray CT) under various thermal conditions. Evidence suggests that TEM expansion within a PBX is a viable method to impart microstructural changes that are predicted to have a measurable, on-demand effect on the initiation sensitivity. Future work includes development of PBX-TEM formulations with HMX and shock initiation experiments.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2022

The effect of hardness on polymer-bonded pentaerythritol tetranitrate (PETN) explosive impact sensitivity

Handling sensitivity is an important property to assess when working with explosive samples and can be measured using a variety of tests, including drop-weight impact sensitivity. There exists a longstanding interest in the explosives community on the importance of measurable chemical, physical, and mechanical properties of explosives in impact sensitivity. However, most recent work in this area has explored chemical attributes rather than physical and mechanical properties of explosives. In this study, we measure hardness of explosive samples of pentaerythritol tetranitrate and Sylgard binder (XTX) during the curing process. The samples have been characterized for particle morphology through scanning electron microscopy and handling sensitivity through drop-weight impact testing. The relative importance of states of cure, methods of curing, morphology, and age of material are discussed. The data indicate that although there is a notable difference in morphology and mechanical properties for the samples as the polymer-bonded mixtures cure, the resulting changes to mechanical properties have a minimal effect on the sensitivity of the XTX.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Formation, structure, and thermal stability evolution of ternesite based on a single-stage sintering process

Highlights: • The synthesis of high-purity ternesite based on a single-stage sintering process was firstly studied. • The formation mechanism and crystallization behaviour of ternesite during sintering were investigated. • The structure perfection and symmetry of ternesite crystals were increased with its growth. • The growth and structural development of ternesite crystals during sintering resulted in a higher thermal stability of itself. Ternesite was prepared via a single-stage solid-state reaction from stoichiometric quantities of the CaCO{sub 3}, SiO{sub 2} and CaSO{sub 4}·2H{sub 2}O precursors. In this paper, the formation, structure, and thermal stability evolution of ternesite during sintering were investigated ex situ after quenching. The optimal sintering temperature for the formation of high-purity ternesite was approximately 1200 °C for 12 h, of which the purity level can reach as high as 96.3%. The results from scanning electron microscopy analysis suggest that the formation of ternesite benefited from the preformation of the intermediate silicate phase. Increasing the sintering temperature from 1100 °C to approximately 1250 °C was favourable for the growth of ternesite crystals, and a prolonged duration can also promote this behaviour. The structural perfection and symmetry of ternesite crystals increased with its growth, which was demonstrated by a multimethod approach. By means of thermal analysis, the growth and structural development of ternesite crystals during sintering eventually resulted in a higher thermal stability.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Multiscale Characterization of Photovoltaic Modules—Case Studies of Contact and Interconnect Degradation

The current popularity of photovoltaic (PV) systems is due in large part to their exceptional reliability and significantly lower cost than other energy sources. Studying cell and module degradation is key to promote further development in the state of the art. Fielded or accelerated aged modules exhibit different failure modes, of which metallization degradation (contacts and interconnections) is prevalent. In this work, we discuss how multiscale characterization methods can be applied to a variety of module technologies that have been field exposed and have undergone accelerated age testing. These methods include performing characterization on the module level, cell level, and finally the materials level. The observed performance losses from the module- and cell-level characterization can be correlated with materials properties to find out the root cause of degradation. We recommend an initial nondestructive characterization suite, including module- and cell-level current-voltage ( I--V ), Suns-V OC , photoluminescence and electroluminescence imaging, quantum efficiency, ultraviolet fluorescence imaging, and thermal infrared imaging. Samples are then extracted from particularly degraded regions of the module and prepared for materials characterization techniques, such as top-down and cross-sectional scanning electron microscopy, energy-dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy, secondary ion mass spectrometry, Raman spectroscopy, and transmission electron microscopy, allowing a deeper look into the mechanism behind the metallization degradation. This article serves as an instructional review to introduce the different multiscale characterization methods and how they can be effectively applied to perform PV degradation studies. Furthermore, we also share some of our examples and discuss the strengths, limitations, and best practices for each of the characterization techniques.

14 SOLAR ENERGY↗
DOE OSTI2024

Corrosion Behavior of a Reactive Bond Between Stainless Steel and a Cast AlCeMg Alloy

Corrosion is a longstanding issue for metal components, especially those used in heat exchanger applications. Al–Ce–Mg alloys may provide a potential solution to this problem due to their good mechanical properties and potential reaction bonding with other metals. The reaction bonding involves a “reactive” bond that occurs upon casting of Al–Ce–Mg alloy over stainless steel (SS). Here this study examined the corrosion response of Al–2Ce–6Mg (atomic percent)/(SS) reactive bond interfaces after samples were completely submerged in nitric, sulfuric, formic, and mixed acids for 267 h. Scanning electron microscopy revealed that in the as-cut condition, reactive bond formations were seen frequently throughout the length of the casting and maintained a secure bond between the alloy and the SS tubes. Furthermore, the nitric, sulfuric, and the mixed acids did not have a deleterious effect on the reactive bond structure. However, formic acid did produce changes in both the microstructural appearance and the elemental profile across the bond due to the formation of corrosion reaction products on the acid-exposed surface.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Evolution of TiS and TiN in Fe-40 MassPctNi Austenitic Alloy During Heating at 1273 K (1000 °C)

Evolution of TiS in composition and morphology as well as the change in size distribution of TiS and TiN in Fe-40 masspctNi austenitic alloy during heating at 1273 K (1000 °C) was investigated using manual/automatic scanning electron microscopy energy-dispersive X-ray spectroscopy (SEM/EDS). Two types of TiS morphologies, spindle and spherical, were maintained during heating. The molar ratio of Ti/S of TiS increased while the aspect ratio of TiS was maintained in both alloys during heating. The number density of TiN inclusions was low compared with TiS in each alloy during heating. The pinning effect of TiS during heating was confirmed, and was stronger in alloy with a larger volume fraction of TiS. The results contribute to the establishment of optimum heat treatment processes for austenitic stainless steel to obtain better pitting corrosion resistance.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Real-Time and Online Monitoring of Glucose Contents by Using Molecular Imprinted Polymer-Based IDEs Sensor

A highly sensitive, selective, reversible, and reusable glucose sensor is developed by using molecularly imprinted polymer-based artificial receptors onto interdigital transducer. Sensor receptors were synthesized through bulk imprinting technology by using styrene as monomer, ethylene glycol dimethacrylate (EGDMA) as cross-linker, and AIBN as free radical initiator. Topography of the synthesized receptors was investigated by scanning electron microscopy (SEM). Fabricated sensor showed concentration-dependent linear and reversible response with lower limit of detection of 30 ppb and upper limit of detection ~ 500 ppm. Furthermore, newly fabricated sensor is highly selective towards its analyte of interest in the presence of other competing agents, and the regeneration of sensor response has been assessed with the percentage error of less than 2% under the period of 1 year at room temperature and pressure conditions. The reported sensor may have potential technological applications in the field of medical diagnostics, food, and pharmaceutical industry.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2019

Microstructural Changes and Kinetics of Reduction of Hematite to Magnetite in CO/CO{sub 2} Gas Atmospheres

The microstructures of porous magnetite formed on gaseous reduction of dense hematite have been examined using high-resolution scanning electron microscopy. It has been shown that cellular pores are formed on reduction in the temperature range 573 K to 973 K (300 °C to 700 °C). Dendritic shaped gas pores are formed on reduction at temperatures between 1073 K and 1273 K (800 °C and 1000 °C). The apparent chemical reaction rate constant for the reduction of hematite to magnetite in CO/CO{sub 2} gas mixtures has been derived from measurements of product thickness against reaction time; the rate constant is described by the relation φ{sub CO} = 0.232exp(76,000/RT) µm s{sup −1} atm{sup −1}.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Sigma phase evolution and nucleation mechanisms revealed by atom probe tomography in a 347H stainless steel

The size evolution and phase composition of sigma phases were investigated for a 347H stainless steel subject to isothermal aging at 750 °C for up to 10,000 h. Scanning electron microscopy reveals that sigma phases are present before 336 h aging and they continue to grow for all aging times studied. Atom probe tomography shows little variation in the sigma phase composition with aging time up to 10,000 h, and only the C content decreases with aging time. The comparison of C concentration suggests that the sigma phase does not nucleate within the C-depleted matrix or precipitate free grain boundaries, leaving dissolving metastable M 23 C 6 as the only possible nucleation site. Based on the experimental results and thermodynamic simulations, the desirable Nb concentration is discussed to reduce the kinetics of sigma phase growth, and possible design directions are suggested to improve 347H.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Single-event burnout in homojunction GaN vertical PiN diodes with hybrid edge termination design

GaN devices play a major role in modern electronics, providing high-power handling, efficient high-frequency operation, and resilience in harsh environments. However, electric field crowding at the edge of the anode often limits its full potential, leading to single-event effects (SEEs) at lower bias voltages under heavy ion radiation. Here, in this work, we report on the performance of homojunction GaN vertical PiN diodes with a hybrid edge termination design under heavy ion irradiation, specifically, oxygen ions, chlorine ions, Cf-252 fission fragments, and alpha particles from an Am-241 source. The unique hybrid edge termination (HET) design provides better electric field management, preventing breakdown from occurring at the edge of the anode at lower voltages. The results of this study reveal that these devices exhibit excellent tolerance to 12-MeV oxygen and 16-MeV chlorine ions, owing to their low linear energy transfer (LET) and range in GaN. However, single-event burnout (SEB) is observed during the Cf-252 exposure at about 50% of the diodes' electrical breakdown voltage due to the presence of higher LET and longer-range ions. Optical and scanning electron microscopy (SEM) reveal that the damage that caused by SEB lies close to the center of these devices rather than the anode edge. Devices with junction termination extension (JTE) instead of HET edge termination also show similar SEB when irradiated with Cf-252 fission fragments. Physical damage due to SEB occurs at the edge of the anode for these devices. These comparative results show the benefits of HET for enhancing the resistance of GaN-based PiN diodes to heavy ion irradiation.

42 ENGINEERING↗
DOE OSTI2025

Thermal oxidation of nuclear graphite and pyrolytic carbon coatings

The oxidation of pyrolytic carbon (PyC) deposited via fluidized bed chemical vapor deposition was characterized and compared with that of standard nuclear-grade graphite. The materials were heated at 700 to 1000 °C in a thermogravimetric analysis system under 20% v/v O 2 flow, allowing for direct comparison of dynamic oxidative mass change in each material. Further, three different PyC samples fabricated under different conditions exhibited variation in total mass loss and mass loss rate, varying by as much as 709 mg/cm 2 in total mass loss and 14.2 (mg/cm 2 )/min in mass loss rate at a single temperature. These variations highlight the correlation between PyC microstructure/defect density and oxidation susceptibility. Additionally, changes in the microstructure and composition between PyC and graphite were characterized via scanning electron microscopy and correlated to the mass loss results. The results of this work have implications toward the safety of tristructural isotropic (TRISO) and other coated particle fuels, especially under off-normal conditions, given the limited information that exists about the oxidation behavior of PyC.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Determination of the Maturation Status of Dendritic Cells by Applying Pattern Recognition to High-Resolution Images

The maturation or activation status of dendritic cells (DCs) directly correlates with their behavior and immunofunction. A common means to determine the maturity of dendritic cells is from high-resolution images acquired via scanning electron microscopy (SEM) or atomic force microscopy (AFM). While direct and visual, the determination has been made by directly looking at the images by researchers. Here we report a machine learning approach using pattern recognition in conjunction with cellular biophysical knowledge of dendritic cells to determine the maturation status of dendritic cells automatically. The determination from AFM images reaches 100% accuracy. The results from SEM images reaches 94.9%. The results demonstrate the accuracy of using machine learning for accelerating data analysis, extracting information, and drawing conclusions from high-resolution cellular images, paving the way for future applications requiring high-throughput and automation, such as cellular sorting and selection based on morphology, quantification of cellular structure, and DC-based immunotherapy.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

A mild calcium carbonate treatment improves moisture resistance and mechanical/interfacial properties of jute and hemp fibers

Natural fibers are attractive, sustainable reinforcements, but often exhibit high moisture uptake and weak bonding with polymer matrices. In this study, jute and hemp were treated by immersion in aqueous calcium carbonate (CaCO3) suspensions (10–40?wt.%, 1.5?h, room temperature) and were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), moisture sorption testing, single-fiber tensile testing, and bundle pull-out testing. SEM showed granular CaCO3 deposition on fiber surfaces, with particulates bridging surface voids and microcracks. At 40 wt.% CaCO3, equilibrium moisture uptake decreased to ~5% (hemp) and ~3% (jute), while tensile strength increased to ~904 MPa (hemp) and ~960 MPa (jute). Apparent interfacial shear strength from pull-out testing increased up to ~1.35 MPa (hemp) and ~0.56 MPa (jute). These results indicate that CaCO3 deposition is a mild, scalable surface treatment that improves moisture resistance, fiber tensile strength, and interfacial load transfer relevant to semi-structural composite applications, including interior and secondary automotive components.

Calcium carbonate treatment↗
DOE OSTI2021

edxia: Microstructure characterisation from quantified SEM-EDS hypermaps

The characterisation of cement paste microstructure is an important step towards understanding durability mechanisms in cementitious materials. Scanning electron microscopy (SEM) coupled with energy dispersive spectroscopy (EDS) is a widely used technique to analyse the microstructure at the micron-scale. However, it is challenging, notably because the characteristic size of many phases is found on a scale smaller than the EDS interaction volume. This work presents a new image analysis framework to identify phases and quantify the microstructure of cementitious materials from SEM-EDS hypermaps. By leveraging domain knowledge, representative points are attributed to phases and mixtures of phases based on ratio plots. Then, quantitative analysis of the microstructure can be carried out (chemical composition, particle size distributions, volume fractions, …). We demonstrate the abilities of the framework, and we present possible applications and extensions of the method. The framework is available as both a graphical interface and a Python code.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Polyvinyl Alcohol (PVA)–Azadirachta indica (Neem) Nanofibrous Mat for Biomedical Application: Formation and Characterization

The present study provides credence to the formation of polyvinyl alcohol (PVA)–Azadirachta indica (neem) nanofibrous mat (PNNM) under optimum processing conditions of electrospinning technique from a mixer of PVA and neem extract to utilize the inherent medicinal properties of this herb for biomedical application. The bonding behavior, orientation of fibers, thermal behavior, and moisture management properties were evaluated by Fourier transforms infrared spectroscopy (FTIR), scanning electron microscopy (SEM), thermo gravimetric analysis (TGA) and moisture management tester (MMT) reports respectively. The antibacterial activity of the developed sample at the maximum mixing ratio of neem extract (80%) was tested against Gram-positive (S. aureus) bacteria using agar disc diffusion method. The results reveal that the prepared nanofibrous mat exhibited better thermal and moisture management properties in comparison with PVA nanofiber alone. The formation of smooth fibers was confirmed by SEM images having average diameter of 185 nm under 5k, 10k and 15k magnifications. The characteristic peaks of PVA and neem constituents in FTIR spectra of the developed mat confirmed the presence of both components. Bacterial resistance was reached up to 20 mm due to the antibacterial constituents of neem extract. Thus the developed mat could be used as a biocompatible and bio based in biomedical applications. Graphic Abstract: .

36 MATERIALS SCIENCE↗
DOE OSTI2023

Advances in imaging, scattering, spectroscopy, and machine learning-aided approaches for multiscale characterization of cementitious systems

Recent progress in methods used in the multiscale characterization of cementitious systems is reviewed, focusing on advances in imaging, scattering, and spectroscopy. The review includes relevant applications and developments in machine learning and other data analytics approaches to enhance characterization. Developments in imaging using light and electron microscopy as well as x-ray (i.e., from synchrotron) methods are summarized. Updates include scanning electron microscopy (SEM), transmission electron microscopy (TEM), tomography, and holography. A critical overview of spectroscopy (e.g., MAS NMR, Raman) and scattering (e.g., neutron, x-ray, synchrotron x-ray) methods is provided, and the intersection of these with imaging is developed (e.g., Raman imaging). Additionally, the paper summarizes recent developments in and implementations of state-of-the-art machine-learning algorithms and data analytics methods for automated, systematic, and/or quantitative analyses of image data sets. The review considers but is not limited to the application of these methods for investigating the hydration and microstructure development of cement phases, low-carbon-footprint cements (e.g., limestone calcined clay cements, LC3), environmental interactions (e.g., ASR) and model systems. Finally, the present work provides a critical presentation of advances in characterization methods that link together the composition and multiscale structure of cementitious materials.

42 ENGINEERING↗