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At least 469 records · Page 26
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Low Field NMR Relaxometry Characterization of Water Adsorption in Corn Stover Anatomical Fractions

Low magnetic field 2 MHz NMR relaxometry is applied to measure water adsorption processes of intact corn stover anatomical fractions. Comparison with high magnetic field 250 MHz relaxometry of milled corn stover fractions as a function of water activity, i.e., relative humidity, provides insight into the microstructural changes of the biomass and varying water molecular dynamics during adsorption. As a result, the data presented establish a basis for low field portable NMR of biomass in situ in field and processing environments.

09 BIOMASS FUELS↗
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 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↗
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.↗
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.↗
NASA NTRS2020

Monitoring of Dust Devil Tracks Around the InSight Landing Site, Mars, and Comparison With In Situ Atmospheric Data

The NASA InSight mission on Mars is a unique opportunity to study atmospheric processes both from orbit and in situ observations. We use post-landing high-resolution satellite images to monitor dust devil activity during the first 8 months of the mission. We perform mapping and semiautomatic detection of newly formed dust devil tracks and analyze their characteristics (sizes, azimuths, distances, and directions of motion).We find a large number of tracks appearing shortly after landing, followed by a significant decrease of activity during late winter, then a progressive increase during early spring. New tracks are characterized by dark linear, to slightly curvilinear, traces ranging from a few to more than 10 m wide. Tracks are oriented in the ambient wind direction, according to measurements made by InSight's meteorological sensors. The systematic analysis of dust devil tracks is useful to have a better understanding of atmospheric and aeolian activity around InSight.

C. Perrin↗
NASA NTRS2012

Terrain Generation from Stereo Imagery in the JPL/MIPL Pipeline

Multimission Image Processing Lab (MIPL) at JPL is responsible for (among other things) the ground-based operational image processing of all the recent in-situ Mars missions. Terrains and meshes are probably the most important products from MIPL for in-situ operations

Multimission Instrument (Image) Processing Lab at ↗
DOE OSTI2024

Effect of fabrication processes on BaTiO 3 capacitor properties

There is an increasing desire to utilize complex functional electronic materials such as ferroelectrics in next-generation microelectronics. As new materials are considered or introduced in this capacity, an understanding of how we can process these materials into those devices must be developed. Here, the effect of different fabrication processes on the ferroelectric and related properties of prototypical metal oxide (SrRuO 3 )/ferroelectric (BaTiO 3 )/metal oxide (SrRuO 3 ) heterostructures is explored. Two different types of etching processes are studied, namely, wet etching of the top SrRuO 3 using a NaIO 4 solution and dry etching using an Ar + -ion beam (i.e., ion milling). Polarization-electric-field hysteresis loops for capacitors produced using both methods are compared. For the ion-milling process, it is found that the Ar + beam can introduce defects into the SrRuO 3 /BaTiO 3 /SrRuO 3 devices and that the milling depth strongly influences the defect level and can induce a voltage imprint on the function. Realizing that such processing approaches may be necessary, work is performed to ameliorate the imprint of the hysteresis loops via ex situ “healing” of the process-induced defects by annealing the ferroelectric material in a barium-and-oxygen-rich environment via a chemical-vapor-deposition-style process. This work provides a pathway for the nanoscale fabrication of these candidate materials for next-generation memory and logic applications.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Application of an Embedded Fracture and Borehole Modeling Approach to the Understanding of EGS Collab Experiment 1

EGS Collab is a series of meso-scale experiments and associated numerical simulation activities being funded by the United States Department of Energy, Geothermal Technologies Office (GTO) to investigate enhanced geothermal system processes under in-situ stress and slightly elevated temperature conditions. This project is designed to provide scientists and engineers with immediate access to impermeable rock at scales larger than possible in the laboratory, but generally smaller than those for commercial production. Immediate access to rock is provided via the existing drifts of the former Homestake Gold Mine, now operated as the Sanford Underground Research Facility in Lead, South Dakota. The objectives of the EGS Collab project are to develop well controlled fracture networks between injector and producer boreholes using normal and shear stimulation for permeability enhancement. The first experimental site was located off the West Access drift on the 4850 Level (4850 feet below ground surface) in phyllite of the Precambrian Poorman formation, and involved the creation of a fracture network comprising a combination of hydraulic and natural fractures. A second experimental site is now being considered near the battery alcove on the 4100 Level in amphibolite and rhyolite of the Yates Unit. Data generated during these experiments will be compared against predictions of a suite of computer codes specifically designed to solve problems involving coupled thermal, hydrological, geomechanical, and geochemical processes. Comparisons between experimental and numerical simulation results will provide code developers with direction for improvements and verification of process models, build confidence in the suite of available numerical tools, and ultimately identify critical future development needs for the geothermal modeling community. Moreover, conducting thorough comparisons of models, modelling approaches, measurement approaches and measured data, via the EGS Collab project, will serve to identify techniques that are most likely to succeed at the Frontier Observatory for Research in Geothermal Energy (FORGE), the GTO’s flagship EGS research effort. Experiment 1 has comprised a series of successful tests, including a long-term chilled-water circulation test, but the testbed has two atypical EGS elements. Active ventilation in the adjacent drift over a 50-year period cooled the testbed rock mass and hydraulic fracturing intersected monitoring boreholes making them conduits for fluid flow. Numerical simulations executed in support of the design of the EGS Collab Experiment 1, computed a radial temperature distribution and stress gradient orthogonal to the drift axis, resulting in the forecast of an oblong hydraulic fracture geometry, extended in the direction of the drift from the stimulation borehole. This paper describes the numerical simulation of long-term chilled-water circulation test with an embedded fracture and borehole modeling approach. The principal objective of the simulation work is show agreement between experimental observations in terms of production fluid temperatures, monitoring borehole temperatures, injection and production pressures, and tracer recoveries using a single conceptual model for the fracture network, using characterization and monitoring data generally available for EGS. A secondary objective is to improve the numerical simulation result comparisons with additional data available from the broader monitoring equipment within the testbed versus deeper, hotter, and more remote EGS. One complicating factor for comparisons between the numerical simulation results and experimental observations, is the Joule-Thomson heating associated with large pressure drops across the fracture network.

numerical simulation, embedded fractures and boreh↗
NASA NTRS1988

Insitu measurement and control of processing properties of composite resins in a production tool

An in situ measuring technique for use in automated composite processing and quality control is discussed. Frequency dependent electromagnetic sensors are used to measure processing parameters at four ply positions inside a thick section 192-ply graphite-epoxy composite during cure in an 8 x 4 in. autoclave. Viscosity measurements obtained using the sensors are compared with the viscosities calculated using the Loos-Springer cure process model. Good overall agreement is obtained. In a subsequent autoclave run, the output from the four sensors was used to control the autoclave temperature. Using the 'closed loop' sensor controlled autoclave temperature resulted in a more uniform and more rapid cure cycle.

Kranbuehl, D.↗