Search NASA⌕ Search

SEARCH · Search NASA

Results for “in situ processing”

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.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 199 records · Page 11
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

In situ monitoring of microstructure evolution during thermal processing of uranium-zirconium alloys using laser-generated ultrasound

In this study, laser-generated ultrasound was used to monitor microstructure evolution during thermal processing of as-cast, polycrystalline binary uranium-zirconium metallic fuel alloys with compositions of U-20wt.%Zr (U-20Zr), U-50wt.%Zr (U-50Zr) and U-80wt.%Zr (U-80Zr). Ultrasonic waveforms were recorded during heating and cooling the samples from room temperature to >973 K and back. A phase transition temperature for all three compositions was estimated from the temperature at which an abrupt and rapid reduction in ultrasonic velocities was observed. Microstructural features on the length scale of tens of micrometers were inferred from the observation of scattering of ultrasonic waves by elastic heterogeneities above ~823 K in U-20Zr, while a hysteresis in the ultrasonic velocities of U-80Zr upon cooling was attributed to a partial retention of the high temperature phase following thermal annealing. The U-50Zr alloy exhibited a reversible viscoelastic response above 933 K, as evidenced by the observation of high frequency attenuation of the shear component of the waveforms at high temperature. Ultrasonic measurements were supplemented by in situ transmission electron microscopy (TEM). The TEM images revealed that the δ-U-Zr matrix in the three compositions underwent a spinodal decomposition above ~823 K into nanoscale regions. The ultrasonic measurements revealed larger, micron-scale structure evolution in the U-20Zr alloy at the same temperature. This large-scale structure is associated with heterogeneous regions having different Zr content. Our findings show the potential heating rate dependence of microstructural evolution in U-Zr alloys and highlight differences in the thermomechanical response and associated length scales during thermal annealing between single- and dual-phase compositions. These results demonstrate the utility of laser ultrasonics to rapidly and efficiently scan phase boundaries and monitor micrometer-scale structure evolution in metallic fuel alloys.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2020

In situ investigation of phosphonate retarder interaction in oil well cements at elevated temperature and pressure conditions

In this paper, the effect of a high-performance retarding additive in oil well cements was investigated under elevated temperature (165°C) and pressure (1000 psi) conditions via in situ synchrotron-based X-ray diffraction (XRD) and quasielastic neutron scattering (QENS) techniques. Under these temperature and pressure conditions, crystalline calcium silicate hydrates (C–S–H) are formed through the cement hydration process. From in situ XRD experiments, the retardation effect was observed by a change in the rate of the appearance of 11 Å tobermorites as well as a change in the rate of the α-C 2 SH generation and depletion. QENS analysis revealed that the retardation effect was related to the non-conversion of free water to chemical and constrained water components. A high presence of free water components was attributed to a decrease in 11Å tobermorites along with slower consumption of the quartz and portlandite phases. Furthermore, QENS results infer that the water molecules experienced confinement in the restricted pore spaces. The retarder inhibited this initial water confinement by slowing the bulk diffusion of free water in the confined region.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Solutionization via Severe Plastic Deformation: Effect on Natural Aging in an Al-Mg-Si-(Mn) Alloy

Shear Assisted Processing and Extrusion (ShAPE), a severe plastic deformation technique that is fast and scalable, was used to produce thin-wall tubing from alloy 6082 (Al-0.8Mg-0.9Si-0.7Mn) with in-situ solutionization during processing quickly followed by quenching. Quench medium and input material heat treatment were varied and natural aging behavior (T1 heat treatment) was evaluated using tensile testing. As-cast input material was found to have higher strength early in post-ShAPE natural aging and homogenized input material was found to have strengthening during natural aging. Compared to air quenching, water quenching gave greater strength both early in and after natural aging. These observations along with microscopy suggest that: 1. air quenching was too slow; 2. as-cast material was not fully solutionized but plastic deformation broke up the coarse intermetallic particles, which provided strengthening; and 3. homogenized material was solutionized well, which led to good natural aging behavior.

Milligan, Brian K.↗
DOE OSTI2020

Enabling Microscale Processing: Combined Raman and Absorbance Spectroscopy for Microfluidic On-Line Monitoring

Microfluidics have many potential applications including characterization of chemical processes on a reduced scale, spanning the study of reaction kinetics using on-chip liquid–liquid extractions, sample pretreatment to simplify off-chip analysis, and for portable spectroscopic analyses. The use of in situ characterization of process streams from laboratory-scale and microscale experiments on the same chemical system can provide comprehensive understanding and in-depth analysis of any similarities or differences between process conditions at different scales. A well-characterized extraction of Nd(NO 3 ) 3 from an aqueous phase of varying NO 3– (aq) concentration with tributyl phosphate (TBP) in dodecane was the focus of this microscale study and was compared to an earlier laboratory-scale study utilizing counter current extraction equipment. Here, we verify that this same extraction process can be followed on the microscale using spectroscopic methods adapted for microfluidic measurement. Concentration of Nd (based on UV–vis) and nitrate (based on Raman) was chemometrically measured during the flow experiment, and resulting data were used to determine the distribution ratio for Nd. Extraction distributions measured on the microscale were compared favorably with those determined on the laboratory scale in the earlier study. Both micro-Raman and micro-UV–vis spectroscopy can be used to determine fundamental parameters with significantly reduced sample size as compared to traditional laboratory-scale approaches. This leads naturally to time, cost, and waste reductions.

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

Developing a Carbon Negative Biorefinery for Organic Waste Valorization

Production of bio-based chemicals have become increasingly attractive as efforts to meet carbon neutrality goals expand. Diverse organic waste feedstocks can be valorized via arrested anaerobic digestion and chain elongation to produce important key intermediates, such as medium chain carboxylic acids. Our work aims to develop a carbon negative biorefinery that funnels multiple organic waste feedstocks into a chemically consistent stream of carboxylic acids that are then upgraded to exemplary carbon negative products. The pairing of a hydrolysis reactor with a chain elongation reactor will allow each biological step to be optimized to improve the ability to valorize a variety of organic waste streams. Specifically, this work has so far been aimed at screening for potential chain elongating organisms to produce VFAs and MCCAs of interest. Four chain elongating organisms were tested for their chain elongation potential with diverse single and mixed substrates. So far, Megasphaera elsdenii and Actinobacillus succinogenes have been tested to determine potential differences in titer as well as product speciation due to variations in pH. To do this, each organism was tested under 3 different substrate combinations with pH maintained at either 5.5, 6, or 7. With better understanding of their metabolic needs and optimal operating conditions, these chain elongating organisms could provide a valuable option to facilitate the chain elongation necessary to produce precursor molecules. In addition to optimizing the bioconversion steps, downstream processing of carboxylic acids is also a key component for the overall feasibility of the process. Our group previously developed a downstream in-situ product recovery (ISPR) process for continuously recovering bio-based carboxylic acids from fermentation broth. The ISPR includes: (i) a solid-liquid separation as a cell retention device, (ii) a liquid-liquid extraction (LLE) to selectively extract the desired bio-based acids, and (iii) a distillation to obtain the neat product. The integrated process was demonstrated at bench-scale and is now scaled up for pilot-scale operations. A more cost-efficient membrane-based emulsion separation is introduced for LLE in downstream separation process with greatly promoted mass transfer, leading to -2800 times smaller needed membrane area than membrane contactors to achieve the same butyric acid extraction rate.

BIOMASS FUELS↗
DOE OSTI2020

In-situ resonant band engineering of solution-processed semiconductors generates high performance n-type thermoelectric nano-inks

Thermoelectric devices possess enormous potential to reshape the global energy landscape by converting waste heat into electricity, yet their commercial implementation has been limited by their high cost to output power ratio. No single “champion” thermoelectric material exists due to a broad range of material-dependent thermal and electrical property optimization challenges. While the advent of nanostructuring provided a general design paradigm for reducing material thermal conductivities, there exists no analogous strategy for homogeneous, precise doping of materials. Here, we demonstrate a nanoscale interface-engineering approach that harnesses the large chemically accessible surface areas of nanomaterials to yield massive, finely-controlled, and stable changes in the Seebeck coefficient, switching a poor nonconventional p- type thermoelectric material, tellurium, into a robust n -type material exhibiting stable properties over months of testing. These remodeled, n -type nanowires display extremely high power factors (~500 µW m -1 K -2 ) that are orders of magnitude higher than their bulk p -type counterparts.

42 ENGINEERING↗
DOE OSTI2025

Polytype selection in the antisolvent-free crystallization of formamidinium lead iodide using alkylammonium chlorides

This work presents a systematic study of how the size of the C 0 –C 4 alkylammonium chloride additive directs the crystallization pathway in antisolvent-free FAPbI 3 films. We find that larger cations promote the intermediate formation of hexagonal polytypes, correlating with enhanced film crystallinity. Understanding the nucleation, crystallization, and phase transition mechanisms in perovskite thin films produced without antisolvent quenching is crucial for improving phase stability and optoelectronic performance at scale. By means of in situ grazing incidence wide-angle X-ray scattering experiments, we show that the nature of alkylammonium chloride (RACl) additives significantly influences the crystallization dynamics and temperature-dependent stability of formamidinium lead iodide (FAPbI 3 ) perovskite films formed using antisolvent-free processes. The in situ experiments reveal that the effective radius of the RA + cation and the vapor pressure of the RA 0 conjugate base are critical factors affecting the crystallization pathway and film morphology. C 2 –C 3 additives with moderate chain lengths may strike a balance between promoting the early crystallization of the cubic 3C phase while suppressing unwanted phases. This balance promotes the formation of highly crystalline cubic perovskite phase with well-oriented structure and better optoelectronic properties. These findings provide guidance regarding the design of additives to crystallize more stable and efficient perovskite films for optoelectronic applications.

Marchezi, Paulo E↗
DOE OSTI2025

Unveiling the Role of In Situ Al 2 O 3 Passivation in Molecular-Ink-Processed CuIn(S,Se) 2 Photovoltaics

Here, we report on the optimization of in situ passivation of ink-based CuIn(S,Se) 2 thin-film solar cells via controlled incorporation of Al 2 O 3 in CuIn(S,Se) 2 films by the addition of Al(NO 3 ) 3 to the molecular ink precursor. For this purpose, the Al/(Al + In) (AAI) metal ratio was varied from 0.05 to 0.30. We observe that the efficiency of the cells made of Al 2 O 3 -incorporated CuIn(S,Se) 2 is consistently higher than those without Al 2 O 3 , especially due to an improvement in open-circuit voltage (V OC ) and fill factor (FF), for all tested AAI ratios. With an AAI of 0.05, a maximum efficiency of 11.2% and an average efficiency of 8.5% (measured across 18 cells) was achieved, compared to 8.5% maximum efficiency and 6.5% average efficiency for Al-free CuIn(S,Se) 2 . Furthermore, we find that cells made of Al 2 O 3 -incorporated CuIn(S,Se) 2 with an AAI of 0.2 show a narrow distribution in the photovoltaic performance, indicating higher reproducibility and higher FF. Energy-dispersive X-ray spectroscopy shows that, at AAI = 0.2, Al 2 O 3 is distributed more homogeneously at the surface of the Al 2 O 3 -incorporated CISSe. Capacitance-voltage measurements reveal a reduced defect density by incorporation of Al 2 O 3 , which could be partly responsible for the higher V OC . Furthermore, using detailed surface analysis with various X-ray and electron spectroscopy methods, we derive chemical and electronic structure information from the surface. With ultraviolet photoelectron (UPS) and inverse photoemission spectroscopies (IPES), the electronic band gap of the CuIn(S,Se) 2 thin-film surface is found to increase from 1.22 to 1.88 eV (+-0.12 eV) with Al 2 O 3 incorporation. This is accompanied by a clear reduction of the conduction band spike at the CdS/CISSe interface due to Al 2 O 3 addition, as derived by both UPS and IPES as well as temperature-dependent V OC measurements.

14 SOLAR ENERGY↗
DOE OSTI2021

Meshfree simulation and experimental validation of extreme thermomechanical conditions in friction stir extrusion

Abstract Friction stir extrusion (FSE) is a novel solid-phase processing technique that consolidates and extrudes metal powders, flakes, chips, or billets into high-performance parts by plastic deformation, which has the potential to save substantial processing time and energy. Currently, most studies on FSE are experimental and only a few numerical models have been developed to explain and predict the complex physics of the process. In this work, a meshfree simulation framework based on smoothed particle hydrodynamics (SPH) was developed for FSE. Unlike traditional grid-based methods, SPH is a Lagrangian particle-based method that can handle severe material deformations, capture moving interfaces and surfaces, and monitor the field variable histories explicitly without complicated tracking schemes. These aspects of SPH make it attractive for the FSE process, where in situ evolution of field variables is difficult to observe experimentally. To this end, a 3-D, fully thermomechanically coupled SPH model was developed to simulate the FSE of aluminum wires. The developed model was thoroughly validated by comparing the numerically predicted material flow, strain, temperature history, and extrusion force with experimental results for a certain set of process parameters. The validated SPH model can serve as an effective tool to predict and better understand the extreme thermomechanical conditions during the FSE process.

99 GENERAL AND MISCELLANEOUS↗
DOE OSTI2020

In Situ Investigation of Chemomechanical Effects in Thiophosphate Solid Electrolytes

Solid-state batteries can suffer from catastrophic failure at high current densities due to solid electrolyte fracture, interface decomposition, or lithium filament growth. Failure is linked to chemomechanical material transformations that can manifest during electrochemical cycling. We systematically investigate how solid electrolyte microstructure and interfacial decomposition (e.g., interphase) affect failure mechanisms in lithium thiophosphates (Li3PS4, LPS) electrolytes. Kinetically metastable interphases are engineered with iodine doping, and microstructural control is achieved using milling and annealing processing techniques. In situ transmission electron microscopy reveals iodine diffusion to the interphase, and upon electrochemical cycling, pores are formed in the interphase region. In situ synchrotron tomography reveals that interphase pore formation drives edge fracture events, which are the origin of through-plane fracture failure. Fractures in thiophosphate electrolytes actively grow toward regions of higher porosity and are affected by heterogeneity in microstructure (e.g., porosity factor). This report provides fundamental design guidelines for high-performance solid-state batteries.

25 ENERGY STORAGE↗
DOE OSTI2021

Process Intensification for the Biological Production of the Fuel Precursor Butyric Acid from Biomass

The production of fuels from lignocellulosic biomass is key to reduce our reliance on petroleum and to promote a sustainable bioeconomy. Butyric acid (BA) is a promising chemical precursor for the production of renewable diesel and jet fuels. BA can be biologically produced from lignocellulosic sugars. However, challenges associated with product selectivity and recovery must be overcome to achieve industrially relevant metrics. Here, we evaluate various fermentation configurations and demonstrate near-homo-butyrate production by using the biocatalyst Clostridium tyrobutyricum. We also develop an advanced in situ product recovery process based on hybrid extraction-distillation (HED-ISPR) and conduct techno-economic analyses and life cycle assessments. We demonstrate that the HED-ISPR process lowers the overall capital and operating expenses and environmental impact compared to other traditional fermentation processes. Overall, BA minimum product selling price from biomass is 55% of the current BA selling price from petroleum, a significant decrease toward viable renewable fuel production.

09 BIOMASS FUELS↗
DOE OSTI2024

A Co-Registered In-Situ and Ex-Situ Dataset of Electrical, Acoustic, and CT Characteristics from Wire Arc Additive Manufacturing Process

Recent progress in sensing techniques and data analytics tools have significantly accelerated the development of Wire Arc Additive Manufacturing (WAAM) systems. This data centric approach emphasizes leveraging available data throughout the production process to optimize performance. Integration of extensive data analysis provides the opportunity to improve precision, reduce waste, and enhance the quality of produced parts. This method relies on AI/ML models and optimization techniques, which are developed using the data collected from various sources, including in-situ sensors, ex-situ imaging, and manufacturing process parameters. The quality and diversity of this data, along with the alignment between different data streams (achieved through spatiotemporal registration) are critical for the successful development of AI/ML and optimization models. In this work, we present a spatiotemporally registered dataset generated during the WAAM process of deposition of a rectangular block. The dataset includes the comprehensive description of deposition process, process parameters, in-situ collected welding characteristics, acoustic data, and X-Ray Computed Tomography analysis data for the build. Dataset A Co-Registered In-Situ and Ex-Situ Dataset of Electrical, Acoustic, and CT Characteristics from Wire Arc Additive Manufacturing Process has arisen under UT-Battelle, LLC’s Prime Contract No. DE-AC05-00OR22725 with the U.S. Department of Energy (DOE) to manage and operate the Oak Ridge National Laboratory. UT-Battelle, LLC will not assert any rights under United States law or under the Prime Contract it has in the dataset against any user of the dataset, including any copyrights or patent rights. UT-Battelle, LLC requests that attribution to the dataset is provided as academically appropriate.

42 ENGINEERING↗
DOE OSTI2023

Evaluation of Multi-Fidelity Soil Moisture Products Across the Continental United States

We have aggregated the most recent soil moisture datasets from a diverse range of sources, encompassing the Continental United States (CONUS). These sources encompass gridded data from remote sensing products, reanalysis products, machine learning-based projects, and land surface modeling products. Additionally, we have obtained and processed in-situ soil moisture observations from the International Soil Moisture Network. The collected datasets exhibit variations in both temporal and spatial resolutions. Among the 20 datasets, six are available at a spatial resolution of 0.25 degrees, while three are at a coarser spatial resolution of 25 km. To minimize spatial interpolation, we conducted data uncertainty evaluations at the 0.25-degree spatial resolution. For our data evaluations, we maintained a monthly temporal resolution, which effectively captures soil moisture seasonality and interannual variability. Our data processing strategy preserves the raw data and interpolated data at their original temporal resolutions. Datasets with higher temporal resolutions, including daily, three-hourly, and hourly datasets, are set aside for subsequent analyses. These analyses will delve into topics such as soil moisture changes and recovery during extreme weather events. Furthermore, we have processed auxiliary data to enhance our evaluation, leveraging tools such as Google Earth Engine. This includes incorporating topography data, land use land cover data, Köppen-Geiger climate classification, and more to provide a comprehensive assessment from multiple sources.

Li, Lingcheng↗
DOE OSTI2024

Dry etching of epitaxial InGaAs/InAlAs/InAlGaAs structures for fabrication of photonic integrated circuits

A dry etching process to transfer the pattern of a photonic integrated circuit design for high-speed laser communications is described. The laser stack under consideration is a 3.2-µm-thick InGaAs/InAlAs/InAlGaAs epitaxial structure grown by molecular beam epitaxy. The etching was performed using Cl2-based inductively-coupled-plasma and reactive-ion-etching (ICP-RIE) reactors. Four different recipes are presented in two similar ICP-RIE reactors, with special attention paid to the etched features formed with various hard mask compositions, in-situ passivations, and process temperatures. The results indicate that it is possible to produce high-aspect-ratio features with sub-micron separation on this multilayer structure. Additionally, the results of the etching highlight the tradeoffs involved with the corresponding recipes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗