In situ imaging of three dimensional freeze printing process using rapid x-ray synchrotron radiography
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Guang Yang↗
SEARCH · Engineering Papers
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.
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Final Report--Optical Photothermal Infrared (OPTIR) microscope for in-situ characterization of cellular metabolism and chemical processes
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47 OTHER INSTRUMENTATION↗
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↗
In situ dynamic TEM characterization of unsteady crystallization during laser processing of amorphous germanium
The unsteady propagation mechanism for the crystallization of amorphous germanium (a-Ge) was studied with in situ movie-mode dynamic transmission electron microscopy (MM-DTEM). We used short laser pulses to heat sputter-deposited a-Ge films and the resulting crystallization process was imaged with up to 16 sequential 50 ns long electron pulses separated by a controlled delay that was varied between 0.5 and 5 μs. The unsteady crystallization in the radial, net-growth direction was observed to occur at a decreasing rate of ~1.5–0.2 m/s through a mechanism involving the formation of discrete ~1.1 μm wide bands that grew with velocities of 9–12 m/s perpendicular to the radial direction and along the perimeter of the crystallized area. The crystallization rate and resulting microstructure were consistent with a liquid-mediated growth mechanism, which suggests that locally the band front reaches the amorphous melting temperature of Ge. Furthermore, a mechanism based on the notion of a critical temperature is proposed to explain the unsteady, banded behavior.
36 MATERIALS SCIENCE↗
3D Nanoprinting via laser-assisted electron beam induced deposition: growth kinetics, enhanced purity, and electrical resistivity
Here, we investigate the growth, purity, grain structure/morphology, and electrical resistivity of 3D platinum nanowires synthesized via electron beam induced deposition with and without an in situ pulsed laser assist process which photothermally couples to the growing Pt–C deposits. Notably, we demonstrate: 1) higher platinum concentration and a coalescence of the otherwise Pt–C nanogranular material, 2) a slight enhancement in the deposit resolution and 3) a 100-fold improvement in the conductivity of suspended nanowires grown with the in situ photothermal assist process, while retaining a high degree of shape fidelity.
36 MATERIALS SCIENCE↗
In Situ Elucidation of the Active State of Co–CeO x Catalysts in the Dry Reforming of Methane: The Important Role of the Reducible Oxide Support and Interactions with Cobalt
The activation of methane and its dry reforming with CO 2 was systematically studied over a series (2–30 wt %) of Co (~5 nm in size) loaded CeO 2 catalysts, with an effort to elucidate the interplay between Co and CeO 2 during the catalytic process using in situ methods. The results of in situ time-resolved X-ray diffraction (TR-XRD) show a strong interaction of methane with the CoOx–CeO 2 systems at temperatures between 200 and 350 °C. The hydrogen produced by the dissociation of C–H bonds in methane leads to a full reduction of Co oxide, Co 3 O 4 → CoO → Co, and a partial reduction of ceria with the formation of some Ce 3+ . Upon the addition of CO 2 , a catalytic cycle for dry reforming of methane (DRM) was achieved on the CoOx–CeO 2 powder catalysts at temperatures below 500 °C. A 10 wt % Co–CeO 2 catalyst was found to possess the best catalytic activity among various cobalt loading catalysts, and it exhibits a desirable stability for the DRM with a minimal effect of carbon accumulation. The phase transitions and the nature of active components in the catalyst were investigated under reaction conditions by in situ time-resolved XRD and ambient-pressure X-ray photoelectron spectroscopy (AP-XPS). These studies showed dynamic evolutions in the chemical composition of the catalysts under reaction conditions. CO 2 attenuated the reducing effects of methane. Under optimum CO- and H 2 -producing conditions, both XRD and AP-XPS indicated that the active phase involved a majority of metallic Co with a small amount of CoO, both supported on a partially reduced ceria (Ce 3+ /Ce 4+ ). Finally, we identified the importance of dispersing Co, anchoring it onto the ceria surface sites, and then utilizing the redox properties of CeO 2 for activating and then oxidatively converting methane while inhibiting coke formation. Furthermore, a synergistic effect between cobalt and ceria and likely the interfacial sitee are essential to successfully close the catalytic cycle.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
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↗
Radio Frequency (RF) Attenuation Measurements of the Space Shuttle Vehicle
Following the loss of Columbia, the Columbia Accident Investigation Board (CAIB) provided recommendations to be addressed prior to Return To Flight (RTF). As a part of CAIB Recommendation 3.4.1 - Ground Based Imagery, new C-band and X-band radars were added to the array of ground-based radars and cameras already in-situ at Kennedy Space Center. Because of higher power density considerations and new operating frequencies, the team of Subject Matter Experts (SMEs) assembled to investigate the technical details of introducing the new radars recommended a series of radio frequency (RF) attenuation tests be performed on the Space Shuttle vehicle to establish the attenuation of the vehicle outer mold line structure with respect to its external RF environment. Because of time and complex logistical constraints, it was decided to split the test into two separate efforts. The first of these would be accomplished with the assistance of the Air Force Research Laboratory (AFRL), performing RF attenuation measurements on the aft section of OV-103 (Discovery) while in-situ in Orbiter Processing Facility (OPF) 3, located at Kennedy Space Center. The second would be accomplished with the assistance of the National Institute of Standards and Technology (NIST) and the electromagnetic interference (EMI) laboratory out of the Naval Air Warfare Center, Patuxent River, Maryland (PAX River), performing RF attenuation measurements on OV-105 (Endeavour) in-situ inside the Space Shuttle Landing Facility (SLF) hangar, also located at Kennedy Space Center. This paper provides a summary description of these efforts and their results.
Scully, R. C.↗
Mechanically Assisted Self‐Healing of Ultrathin Gold Nanowires
Abstract As the critical feature sizes of integrated circuits approaching sub‐10 nm, ultrathin gold nanowires (diameter <10 nm) have emerged as one of the most promising candidates for next‐generation interconnects in nanoelectronics. Also due to their ultrasmall dimensions, however, the structures and morphologies of ultrathin gold nanowires are more prone to be damaged during practical services, for example, Rayleigh instability can significantly alter their morphologies upon Joule heating, hindering their applications as interconnects. Here, it is shown that upon mechanical perturbations, predamaged, nonuniform ultrathin gold nanowires can quickly recover into uniform diameters and restore their smooth surfaces, via a simple mechanically assisted self‐healing process. By examining the local self‐healing process through in situ high‐resolution transmission electron microscopy, the underlying mechanism is believed to be associated with surface atomic diffusion as evidenced by molecular dynamics simulations. In addition, mechanical manipulation can assist the atoms to overcome the diffusion barriers, as suggested by ab initio calculations, to activate more surface adatoms to diffuse and consequently speed up the self‐healing process. This result can provide a facile method to repair ultrathin metallic nanowires directly in functional devices, and quickly restore their microstructures and morphologies by simple global mechanical perturbations.
Wang, Binjun↗
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↗
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↗
Study on Tensile Deformation Behavior of TC21 Titanium Alloy
To investigate the tensile deformation behavior of TC21 titanium alloy wires, the isothermal tensile deformation tests were conducted by a Geeble-1500D simulator in the temperature range of 720-880 °C and strain rates of 0.01-10 s{sup −1}. The in situ tensile deformation behavior has been studied by SEM SURPA40. The stress–strain curves indicate that the flow stress has shown an inverse relationship with temperature and a direct relationship with strain rate. The flow stress immediately reached the peak value and, then, gradually decreased due to the dynamic softening induced by dynamic recovery and dynamic recrystallization. According to the hot processing maps, the temperatures ranging from 720 to 760 °C (corresponding to the strain rates of 0.01-0.032 s{sup −1}) and 800-840 °C (corresponding to the strain rates of 0.01-0.056 s{sup −1}) are suitable for processing. The in situ tensile results reveal that the cracks initiated at the pre-fabricated defects with the concentrated stress and mainly propagated in the transgranular mode.
36 MATERIALS SCIENCE↗
High-stress triaxial direct-shear fracturing of Utica shale and in situ X-ray microtomography with permeability measurement
The challenge of characterizing subsurface fluid flow has motivated extensive laboratory studies, yet fluid flow through rock specimens in which fractures are created and maintained at high-stress conditions remains underinvestigated at this time. The studies of this type that do exist do not include in situ fracture geometry measurements acquired at stressed conditions, which would be beneficial for interpreting the flow behavior. Therefore, this study investigates the apparent permeability induced by direct-shear fracture stimulation through Utica shale (a shale gas resource and potential caprock material) at high triaxial stress confinement and for the first time relates these values to simultaneously acquired in situ X-ray radiography and microtomography images. Change in fracture geometry and apparent permeability was also investigated at additional reduced stress states. Finite element and combined finite-discrete element modeling were used to evaluate the in situ observed fracturing process. Results from this study indicate that the increase in apparent permeability through fractures created at high-stress (22.2 MPa) was minimal relative to the intact rock (less than 1 order of magnitude increase), while fractures created at low stress (3.4 MPa) were significantly more permeable (2 to 4 orders of magnitude increase). Here, this study demonstrates the benefit of in situ X-ray observation coupled with apparent permeability measurement to analyze fracture creation in the subsurface. Our results show that the permeability induced by fractures through shale at high stress can be minor and therefore favorable in application to CO 2 sequestration caprock integrity but unfavorable for hydrocarbon recovery from unconventional reservoirs.
58 GEOSCIENCES↗
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↗
Metal matrix composite micromechanics: In-situ behavior influence on composite properties
Recent efforts in computational mechanics methods for simulating the nonlinear behavior of metal matrix composites have culminated in the implementation of the Metal Matrix Composite Analyzer (METCAN) computer code. In METCAN material nonlinearity is treated at the constituent (fiber, matrix, and interphase) level where the current material model describes a time-temperature-stress dependency of the constituent properties in a material behavior space. The composite properties are synthesized from the constituent instantaneous properties by virtue of composite micromechanics and macromechanics models. The behavior of metal matrix composites depends on fabrication process variables, in situ fiber and matrix properties, bonding between the fiber and matrix, and/or the properties of an interphase between the fiber and matrix. Specifically, the influence of in situ matrix strength and the interphase degradation on the unidirectional composite stress-strain behavior is examined. These types of studies provide insight into micromechanical behavior that may be helpful in resolving discrepancies between experimentally observed composite behavior and predicted response.
Murthy, P. L. N.↗
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↗
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↗