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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 757 records · Page 42
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Challenges in atomic layer etching of gallium nitride using surface oxidation and ligand-exchange

Two atomic layer etching (ALE) methods were studied for crystalline GaN, based on oxidation, fluorination, and ligand exchange. Etching was performed on unintentionally doped GaN grown by hydride vapor phase epitaxy. For the first step, the GaN surfaces were oxidized using either water vapor or remote O 2 -plasma exposure to produce a thin oxide layer. Removal of the surface oxide was addressed using alternating exposures of hydrogen fluoride (HF) and trimethylgallium (TMG) via fluorination and ligand exchange, respectively. Several HF and TMG super cycles were implemented to remove the surface oxide. Each ALE process was monitored in situ using multiwavelength ellipsometry. X-ray photoelectron spectroscopy was employed for the characterization of surface composition and impurity states. Additionally, the thermal and plasma-enhanced ALE methods were performed on patterned wafers and transmission electron microscopy (TEM) was used to measure the surface change. The x-ray photoelectron spectroscopy measurements indicated that F and O impurities remained on etched surfaces for both ALE processes. Ellipsometry indicated a slight reduction in thickness. TEM indicated a removal rate that was less than predicted. In conclusion, we suggest that the etch rates were reduced due to the ordered structure of the oxide formed on crystalline GaN surfaces.

36 MATERIALS SCIENCE↗
DOE OSTI2022

A General Route to Flame Aerosol Synthesis and In Situ Functionalization of Mesoporous Silica

Mesoporous silica is a versatile material for energy, environmental, and medical applications. In this work, for the first time, we report a flame aerosol synthesis method for a class of mesoporous silica with hollow structure and specific surface area exceeding 1000 m 2 /g -1 . We show its superior performance in water purification, drug carrier, and thermal insulation. Moreover, we propose a general route to produce mesoporous nanoshell supported nanocatalysts by in situ decorating active nanoclusters, including noble metal (Pt/SiO 2 ), transition metal (Ni/SiO 2 ), metal oxide (CrO 3 /SiO 2 ), and alumina support (Co/Al 2 O 3 ). As a prototypical application, we perform dry reforming of methane using Ni/SiO 2 , achieving constant 97% CH 4 and CO 2 conversions for more than 200 hours, dramatically outperforming MCM-41 supported Ni catalyst. This work provides a scalable strategy to produce mesoporous nanoshells and proposes an in situ functionalization mechanism to flexible catalysts design for many reactions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Investigation of the temperature-dependent failure processes in PVD Cr-coated ZIRLO nuclear fuel cladding using in situ X-ray micro-tomography imaging

In this work, an accident tolerant fuel cladding system with Cr coating deposited using physical vapour deposition (PVD) method onto commercial Optimized ZIRLO™ was studied. The cladding tubes were machined into C-rings and loaded to failure under compression with real-time synchrotron micro-X-ray computed tomography (XCT) imaging at room temperature (RT), 345 °C, 650 °C and 950 °C in argon (Ar) atmosphere. The mechanical behaviour and failure processes were found strongly temperature-dependent where the Cr coating showed brittle fracture at RT and 345 °C, ductile fracture at 650 °C and a reversion to brittle fracture at 950 °C. Nanoindentation measurements and scanning electron microscopy (SEM) imaging were conducted on the materials after high temperature testing. It was found that recrystallisation of the Cr coating occurred at elevated temperatures, which significantly affected its local properties hence the failure behaviour at different temperatures. This work represents the first in situ 3D XCT observation of progressive failure processes in PVD Cr-coated ZIRLO claddings up to 950 °C providing critical insights into its brittle-to-ductile transition (BDTT) behaviour and subsequent ductile-to-brittle reversion with the increase in temperature. Moreover, results are compared with other PVD Cr-coated Zircaloy materials from open literature; the influences of the coating microstructure and local properties on the failure stress/strain and fracture processes are discussed.

Yuan, Guanjie↗
NASA NTRSDate not supplied

OPTIMIZING MEASUREMENTS OF THE NEAR-SURFACE WATER CYCLE ON MARS: INSIGHTS FOR HABITABILITY.

The Martian regolith may act as a sink and source of water vapor for the lower atmosphere through processes such as frost formation, physisorption, solid-state hydration, and brine formation [e.g., 1- 12]. These processes are all dependent on temperature and humidity, as well as regolith properties such as porosity, tortuosity, and composition. In particular, the salty nature of the Martian regolith may increase its role in atmosphere-regolith interactions as hygroscopic salts interact with the ambient water vapor. Although to date experimental works near Mars-relevant conditions have constrained some of the potential effects of a salty regolith on water vapor exchange processes [e.g., 13-18], vital in situ measurements are lacking to link these to the near-surface water cycle on Mars. This is because previous and ongoing environmental payloads for landed Mars missions were not designed to investigate atmosphere-regolith exchange processes [12, 19-20]. Resolving the Martian near-surface water cycle is relevant to both climatic processes and astrobiology. There is the potential to presently form (meta)stable brines on Mars; their stability would be largely controlled by water vapor exchange processes [9, 21]. Here we argue for optimizing in situ measurements of water vapor exchange processes and regolith properties to advance our understanding of the local scale Martian water cycle and inform habitability studies.

E G Rivera-Valentin↗
DOE OSTI2021

Promoting the Selectivity of Pt/m-ZrO 2 Ethanol Steam Reforming Catalysts with K and Rb Dopants

The ethanol steam reforming reaction (ESR) was investigated on unpromoted and potassium- and rubidium-promoted monoclinic zirconia-supported platinum (Pt/m-ZrO 2 ) catalysts. Evidence from in situ diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) characterization indicates that ethanol dissociates to ethoxy species, which undergo oxidative dehydrogenation to acetate followed by acetate decomposition. The acetate decomposition pathway depends on catalyst composition. The decarboxylation pathway tends to produce higher overall hydrogen selectivity and is the most favored route at high alkali loading (2.55 wt.% K and higher or 4.25 wt.% Rb and higher). On the other hand, decarbonylation is a significant route for the undoped catalyst or when a low alkali loading (e.g., 0.85% K or 0.93% Rb) is used, thus lowering the overall H 2 selectivity of the process. Results of in situ DRIFTS and the temperature-programmed reaction of ESR show that alkali doping promotes forward acetate decomposition while exposed metallic sites tend to facilitate decarbonylation. In previous work, 1.8 wt.% Na was found to hinder decarbonylation completely. Due to the fact that 1.8 wt.% Na is atomically equivalent to 3.1 wt.% K and 6.7 wt.% Rb, the results show that less K (2.55% K) or Rb (4.25% Rb) is needed to suppress decarbonylation; that is, more basic cations are more efficient promoters for improving the overall hydrogen selectivity of the ESR process.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

In Situ Ion‐Exchange Metathesis Induced Conformal LiF Surface Films on Cathode (NMC811) as a Cathode Electrolyte Interphase

High-capacity cathodes (LiNi 0.8 Mn 0.1 Co 0.1 O 2 , NMC811) are promising for vehicle electrification because of their high gravimetric energy density. However, their electrochemical performance still relies upon the stability of the cathode electrolyte interphase (CEI). A highly reactive cathode interface leads to parasitic side reactions with electrolytes, resulting in accelerated capacity fading. Well-developed LiF and LiF-like inorganic compounds are believed to be good CEI components for stabilizing such reactive electrode interfaces. However, it is challenging to form an optimal surface sub-nanolayer of LiF on the cathode surfaces because of the complexity of the electrochemical reaction during battery cycling. Herein, the formation of a conformal LiF layer on the NMC811 electrode surface via an in situ ion-exchange metathesis process is reported, demonstrating a promising electrochemical performance because of a LiF-stabilized CEI. In situ generated LiF-coated NMC811 electrodes exhibit ≈97% capacity retention up to 100 cycles at a 0.3 C rate with average coulombic efficiency of ≈99.9% and ≈80% capacity retention up to 200 cycles at a 1 C rate with average coulombic efficiency of >99.6%. This finding may pave the way for reengineering the CEI to enhance the electrochemical performances and cycling stability of the high-capacity cathodes.

25 ENERGY STORAGE↗
DOE OSTI2021

In-situ ion irradiation study of alloy 709 stainless steels with different processing histories

Alloy 709 stainless steel (A709 SS) has gained an increased interest in nuclear applications due to its advanced properties at high temperatures over the widely used Type 316 SS. However, how this alloy behaves under irradiation with concurrent environmental factors, such as mechanical deformation and/or thermal annealing, has not been studied. In this work, we used in-situ ion irradiation inside a transmission electron microscope (TEM) to investigate the effects of irradiation on the microstructures of A709 SS samples with different prior processing histories, including as-received, annealed, and creep-deformed. It was found that, compared to room temperature irradiation, 600 degrees C irradiation led to larger dislocation loop sizes and lower loop densities. Furthermore, with 600 degrees C irradiation, the creep-deformed sample, which had the highest precipitate density and the highest dislocation density, had the smallest loop size and the lowest loop density compared to others. This observation has been rationalized with quantitative evaluation of the sink strength factors in each sample. This study shows that in-service deformation can significantly affect the irradiation performance in structural materials at reactor operating conditions.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Targeted in situ metatranscriptomics for selected taxa from mesophilic and thermophilic biogas plants

Summary Biogas production is performed anaerobically by complex microbial communities with key species driving the process. Hence, analyses of their in situ activities are crucial to understand the process. In a previous study, metagenome sequencing and subsequent genome binning for different production‐scale biogas plants ( BGP s) resulted in four genome bins of special interest, assigned to the phyla Thermotogae , Fusobacteria , Spirochaetes and Cloacimonetes , respectively, that were genetically analysed. In this study, metatranscriptome sequencing of the same BGP samples was conducted, enabling in situ transcriptional activity determination of these genome bins. For this, mapping of metatranscriptome reads on genome bin sequences was performed providing transcripts per million ( TPM ) values for each gene. This approach revealed an active sugar‐based metabolism of the Thermotogae and Spirochaetes bins and an active amino acid‐based metabolism of the Fusobacteria and Cloacimonetes bins. The data also hint at syntrophic associations of the four corresponding species with methanogenic Archaea .

Biotechnology & Applied Microbiology↗
DOE OSTI2019

Engineered microbial biofuel production and recovery under supercritical carbon dioxide

Culture contamination, end-product toxicity, and energy efficient product recovery are long-standing bioprocess challenges. To solve these problems, we propose a high-pressure fermentation strategy, coupled with in situ extraction using the abundant and renewable solvent supercritical carbon dioxide (scCO 2 ), which is also known for its broad microbial lethality. Towards this goal, we report the domestication and engineering of a scCO 2 -tolerant strain of Bacillus megaterium, previously isolated from formation waters from the McElmo Dome CO 2 field, to produce branched alcohols that have potential use as biofuels. After establishing induced-expression under scCO 2 , isobutanol production from 2-ketoisovalerate is observed with greater than 40% yield with co-produced isopentanol. Finally, we present a process model to compare the energy required for our process to other in situ extraction methods, such as gas stripping, finding scCO 2 extraction to be potentially competitive, if not superior.

09 BIOMASS FUELS↗
DOE OSTI2018

Design and Integration of Flexible Sensor Matrix for in Situ Monitoring of Polymer Composites

Sensory polymer composites are highly desirable for applications such as in situ and real-time production processes and structural health monitoring, and for technologies that include human–machine interfaces for the next generation of Internet of Things. However, the development of these materials is still in its infancy: these materials have been reported, but large-scale fabrication of polymer composites with versatile and customizable sensing capabilities has yet to be demonstrated. Here, we report on a scalable fabrication strategy that enables such materials by designing and integrating PCB technology-inspired large-area flexible sensor matrices into polymer composites. The integrated sensor matrices successfully monitored in situ the production processes and structural health of an industrial polymer composite: from the application of vacuum, resin flow and polymerization, production defects, and temperature distribution. Our results demonstrate that the proposed strategy is a simple and effective solution as a distributed monitoring platform for polymer composites and shows the potential towards next generation of sensory polymer composites.

47 OTHER INSTRUMENTATION↗
DOE OSTI2022

Formation and growth of cerium (III) oxalate nanocrystals by liquid-cell transmission electron microscopy

Using rare earth elements as analogs for actinide series elements enables studying the chemistry of these radioactive materials without the inherent risks. A fundamental understanding of the nucleation and growth of actinide oxalates is crucial for processing nuclear waste. Using in-situ liquid cell TEM (LC-TEM), we show particle attachment processes occurring during the nucleation and growth of cerium oxalate. The early stages of the observed non-classical growth mechanisms have important implications for particle evolution and predictions of final particle morphology. In this work, we observed particle formation via monomer-by-monomer addition or the particle aggregation pathway depending on the selected precursor concentration. At the highest precursor concentration at a high dose rate, we observed particle alignment in a branch structure is due to the interfacial instability. It was demonstrated that in-situ LC-TEM is an invaluable tool in studying the cerium oxalate formation and ultimately a path to understanding actinide chemistry.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Photo-induced oxidation and amorphization of trigonal tellurium: A means to engineer hybrid nanostructures and explore glass structure under spatial confinement

Controlled photo-induced oxidation and amorphization of elemental trigonal tellurium are achieved by laser irradiation at optical wavelengths. These processes are monitored in situ by time-resolved Raman scattering and ex situ by electron microscopies. Ultrathin TeO₂ films form on Te surfaces, as a result of irradiation, with an interface layer of amorphous Te intervening between them. It is shown that irradiation, apart from enabling the controllable transformation of bulk Te to one-dimensional nanostructures, such as Te nanotubes and hybrid core-Te/sheath-TeO₂ nanowires, causes also a series of light-driven (athermal) phase transitions involving the crystallization of the amorphous TeO₂ layers and its transformation to a multiplicity of crystalline phases including the γ-, β-, and α-TeO₂ crystalline phases. The kinetics of the above photo-induced processes is investigated by Raman scattering at various laser fluences revealing exponential and non-exponential kinetics at low and high fluence, respectively. In addition, the formation of ultrathin (less than 10 nm) layers of amorphous TeO₂ offers the possibility to explore structural transitions in 2D glasses by observing changes in the short- and medium-range structural order induced by spatial confinement.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2013

In situ analyses on negative ions in the indium-gallium-zinc oxide sputtering process

The origin of negative ions in the dc magnetron sputtering process using a ceramic indium-gallium-zinc oxide target has been investigated by in situ analyses. The observed negative ions are mainly O{sup -} with energies corresponding to the target voltage, which originates from the target and barely from the reactive gas (O{sub 2}). Dissociation of ZnO{sup -}, GaO{sup -}, ZnO{sub 2}{sup -}, and GaO{sub 2}{sup -} radicals also contributes to the total negative ion flux. Furthermore, we find that some sputtering parameters, such as the type of sputtering gas (Ar or Kr), sputtering power, total gas pressure, and magnetic field strength at the target surface, can be used to control the energy distribution of the O{sup -} ion flux.

36 MATERIALS SCIENCE↗
NASA NTRS1993

Thermal processing of omicron-terphenyl - A Raman study

Raman spectra from omicron-terphenyl sealed in glass capillary tubes were acquired over temperatures ranging from 233 to 343 K. Over this temperature range, omicron-terphenyl can exist in the solid-crystalline, molten, supercooled-liquid, and amorphous-glassy states. Representative structure-sensitive spectra are presented along with a qualitative description. The lattice spectral feature occurring at a Raman shift of 123/cm displays abrupt changes in profile and intensity as melting and glass transition occur. The intensity ratio of the C-C stretching 996/cm line and C-H stretching line at 1008/cm displays a change related to the transformation of the ordered-crystalline phase to the disordered-liquid or glassy state. At a Raman shift of 1162/cm the solid-crystalline state shows a splitting due to the effect of the crystal field. The possibility of using these structure-sensitive Raman characteristics for in situ diagnostics during materials processing is discussed.

Biswas, A.↗
DOE OSTI2019

Viability of Data Analytics to Ascertain Component Performance for Additive Manufacturing

The Transformational Challenge Reactor (TCR) program is leveraging additive manufacturing (AM) technologies to produce multiple nuclear components to be assembled into a fully functional microreactor core. AM was selected as the main manufacturing technology for TCR because it has the potential to disrupt the nuclear industry on two fronts: (1) it enables the manufacturing of very complex geometries with optimized and tailored material properties for the intended use of the component, opening up new options for reactor designs, and (2) it allows for a better understanding of the manufacturing process through real-time in situ monitoring, data analytics, and artificial intelligence, which can lead to a streamlined qualification and certification process. Within TCR, the development and deployment of a digital platform aims at addressing the latter opportunity. As part of this effort, the collection of pedigree datasets is vital, should these data be generated before, during or after the manufacturing process. This report focuses on the development of data analytics tools enabling qualitative assessment of the manufacturing processes to automate the identification of flaws in in situ monitoring imagery and to correlate those flaws to the resulting mechanical testing data. Through examples, the report gives an overview of the data collected and presents a path forward for the digital platform.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗
NASA NTRS2008

Some Expected Characteristics of Lunar Dust: A Geological View Applied to Engineering

Compared to the Earth the geologic nature of the lunar regolith is quite distinct. Even though similar minerals exist on the Earth and Moon, they may have very different properties due to the absence of chemical modification in the lunar environment. The engineering properties of the lunar regolith reflect aspects of the parent rock and the consequences of hypervelocity meteor bombardment. On scales relevant to machinery and chemical processing for In-Situ Resource Utilization, ISRU (such as water production), the lunar regolith compositional range is much more restricted than terrestrial material. This fact impacts predictions of properties required by design engineers for constructing equipment for lunar use. In this paper two examples will be covered. 1) Abrasion is related to hardness and hardness is a commonly measured property for both minerals and engineering materials. Although different hardness scales are routinely employed for minerals and engineering materials, a significant amount of literature is available relating the two. As one example, we will discuss how to relate hardness to abrasion for the design of lunar equipment. We also indicate how abundant the various mineral phases are and typical size distributions for lunar regolith which will impact abrasive nature. 2) Mineral characteristics that may seem trivial to the non-geologist or material scientist may have significant bearing on ISRU processing technologies. As a second example we discuss the impact of traces of F-, Cl-, and OH-, H2O, CO2, and sulfur species which can radically alter melting points and the corrosive nature of reaction products thereby significantly changing bulk chemistry and associated processing technologies. For many engineering uses, a simulant s fidelity to bulk lunar regolith chemistry may be insufficient. Therefore, simulant users need to engage in continuing dialogue with simulant developers and geoscientists.

Street, Kenneth W.↗
NASA NTRS2008

Some Expected Characteristics of Lunar Dust: A Geological View Applied to Engineering

Compared to the Earth the geologic nature of the lunar regolith is quite distinct. Even though similar minerals exist on the Earth and Moon, they may have very different properties due to the absence of chemical modification in the lunar environment. The engineering properties of the lunar regolith reflect aspects of the parent rock and the consequences of hypervelocity meteor bombardment. On scales relevant to machinery and chemical processing for In-Situ Resource Utilization, ISRU (such as water production), the lunar regolith compositional range is much more restricted than terrestrial material. This fact impacts predictions of properties required by design engineers for constructing equipment for lunar use. In this paper two examples will be covered. 1) Abrasion is related to hardness and hardness is a commonly measured property for both minerals and engineering materials. Although different hardness scales are routinely employed for minerals and engineering materials, a significant amount of literature is available relating the two. As one example, we will discuss how to relate hardness to abrasion for the design of lunar equipment. We also indicate how abundant the various mineral phases are and typical size distributions for lunar regolith which will impact abrasive nature. 2) Mineral characteristics that may seem trivial to the non-geologist or material scientist may have significant bearing on ISRU processing technologies. As a second example we discuss the impact of traces of fluoride, chloride, and hydroxide, water, carbon dioxide, and sulfur species which can radically alter melting points and the corrosive nature of reaction products thereby significantly changing bulk chemistry and associated processing technologies. For many engineering uses, a simulant's fidelity to bulk lunar regolith chemistry may be insufficient. Therefore, simulant users need to engage in continuing dialogue with simulant developers and geoscientists.

Street, Kenneth W.↗
NASA NTRS2012

X-Ray Radiographic Observation of Directional Solidification Under Microgravity: XRMON-GF Experiments on MASER12 Sounding Rocket Mission

The European Space Agency (ESA) - Microgravity Application Promotion (MAP) programme entitled XRMON (In situ X-Ray MONitoring of advanced metallurgical processes under microgravity and terrestrial conditions) aims to develop and perform in situ X-ray radiography observations of metallurgical processes in microgravity and terrestrial environments. The use of X-ray imaging methods makes it possible to study alloy solidification processes with spatio-temporal resolutions at the scales of relevance for microstructure formation. XRMON has been selected for MASER 12 sounding rocket experiment, scheduled in autumn 2011. Although the microgravity duration is typically six minutes, this short time is sufficient to investigate a solidification experiment with X-ray radiography. This communication will report on the preliminary results obtained with the experimental set-up developed by SSC (Swedish Space Corporation). Presented results dealing with directional solidification of Al-Cu confirm the great interest of performing in situ characterization to analyse dynamical phenomena during solidification processes.

Reinhart, G.↗