Engineering Papers⌕ Search

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.

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

At least 703 records · Page 39

In-Situ Detection and Prediction of WAAM Cross Feature Geometry

Abstract Wire arc additive manufacturing (WAAM) is increasingly used by manufacturers due to its relatively low cost and high deposition rate compared to other metal AM methods, but the parts produced by WAAM can be subject to localized variations in part quality. One such variation is the cross-feature defect, whereby a localized part height increase occurs due to the crossing of deposition toolpaths. Mitigation of this defect is typically achieved using manual path planning strategies, but closed-loop control is underutilized. Since the nature of this defect and of the WAAM process is such that the previous layer’s geometry influences that of the subsequent layer’s, the cross-feature defect geometry changes throughout the deposition. Therefore, any closed-loop control strategy will need to incorporate the dynamic trait of this defect. The present work seeks to implement an in-situ process modeling approach where a regression model can be continuously updated to predict the defect geometry of the subsequent deposition layer based on the historical process data. Several multi-layer cross-feature geometries are deposited and current, voltage, and optical camera data is taken for each layer. The resulting cross-feature geometries are characterized using 3D scanning and the performance and accuracy of the in-situ modeling approach is evaluated.

Thien, Austen↗

In Situ Modification and Analysis of the Composition and Crystal Structure of a Silicon Target by Ion-Beam Methods

The method of Rutherford backscattering (RBS) with channeling is widely used in compositional analysis and structural determination. An experimental process line for in situ ion implantation and RBS spectrometry is presented, and its technical parameters are given. The parameters of a probing beam needed to reach a several-percent error in the study of distribution profiles of impurities and defects are detailed. The resolution of this method was estimated using the spectrum of alpha particles produced in the decay of {sup 239}Pu and based on the RBS spectrum from a silicon monocrystal. The implantation of Xe{sup +} ions with an energy of 100 keV into a silicon monocrystal and the RBS analysis of targets in the channeling mode were performed without breach of vacuum conditions. The distribution profiles of implanted atoms and defects in irradiated monocrystals were examined.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Observation of Materials Processes in Liquids in the Electron Microscope

Materials synthesis and the functioning of devices often indispensably involve liquid media. But direct visualization of dynamic process in liquids, especially with high spatial and temporal resolution, has been challenging. For solid materials, advances in aberration corrected electron microscopy have made observation of atomic level features a routine practice. Here we discuss the extent to which one can take advantage of the resolution of modern electron microscopes to image phenomenon occuring in liquids. We will describe the fundamentals of two different experimental approaches, closed and open liquid cells. We will illustrate the capabilities of each approach by considering processes in batteries and nucleation and growth of nanoparticles from solution. We conclude that liquid cell electron microscopy appears to be duly fulfilling its role for in situ studies of nanoscale processes in liquids, revealing physical and chemical processes otherwise difficult to observe.

Environmental Molecular Sciences Laboratory↗

A New Low-Temperature Approach for Efficient and Low-Cost Group V Doping in CdTe Thin Film Solar Cells (Final Technical Report)

The goal of this project is to develop a highly efficient low-temperature ex-situ Group V diffusion doping approach in the CdCl 2 treated polycrystalline CdTe film using the group V chlorides (i.e., PCl 3 , AsCl 3 , SbCl 3 , and BiCl 3 ) as dopants source. For the first time, our innovative doping strategies through the low-temperature ex-situ Group V doping process in polycrystalline CdSeTe successfully demonstrated a promising power conversion efficiency of ~19% compared to the Cu-doped counterparts. Our newly developed low-temperature ex-situ group V doping allows dedicated control of group V diffusion amount, generates a desirable depth profile, and is completely compatible with commercial CdTe module manufacturing. We built the partnership with the largest CdTe solar module manufacturing in the US, e.g., First Solar, Inc to further develop these low-temperature diffusion doped CdSeTe solar cells. Our technology was granted US Patent No. US11257977B2. In this project, we systematically investigate and characterize the new ex-situ group V doping mechanisms, defect chemistry, microstructure, and device physics in CdTe solar cells by combining experimental and theoretical means to pave the way to achieve lower cost toward $\$$0.02/kWh and higher power conversion efficiency (PCE) toward 25% in polycrystalline CdTe solar technology. This project will benefit the public by providing more affordable solar electricity and provide an effective way to address climate change.

14 SOLAR ENERGY↗

In situ probing of interfacial roughness and transient phases during ceramic cold sintering process

The ceramic cold sintering process (CSP) offers an eco-friendly approach to producing fully dense ceramics at low temperatures. However, an incomplete mechanistic understanding hinders its optimization and widespread adoption. In this study, we analyze the microstructural and structural changes in ZnO, a model CSP system, using in situ synchrotron-based high-energy small-angle X-ray scattering and X-ray diffraction techniques. Our results reveal the time evolution of ZnO particles' surface area and roughness, reflecting the dissolution and re precipitation processes that enable densification. The in situ measurements supply valuable kinetic data for these stages of CSP. Alongside microstructural changes and densification, we observed the evolution of secondary phases representing reaction products between ZnO and acetic acid, the solvent used. The initial ZnO/solvent mixture's dominant secondary phase is attributed to zinc acetate, which is gradually replaced by a zinc soap-type structure during CSP. This structure has a large (≈ 21 Å) lattice parameter and is assumed to have a layered nature. The formation of this soap phase, which is retained in the sintered product as an intergranular component, appears to be a signature of successful cold sintering as it facilitates mass transport, leading to densification. Here, our study underscores the potential of in situ synchrotron characterization for revealing microstructural and phase-evolution details during CSP. These findings, which would be challenging to obtain through ex situ measurements, provide crucial data to guide and validate theoretical models, ultimately enhancing CSP's effectiveness and adoption.

36 MATERIALS SCIENCE↗

Determining Individual Phase Flow Properties in a Quench and Partitioning Steel with In Situ High-Energy X-Ray Diffraction and Multiphase Elasto-Plastic Self-Consistent Method

The micromechanical properties of the constituent phases were characterized for an advanced high strength steels (AHSS) produced by a quenching and partitioning (Q&P) process with in-situ tensile loading under Synchrotron-based high energy X-ray diffraction. The constituent phases present are retained austenite and three martensites (tempered, untempered and freshly formed martensites). For the material investigated, the 200 and 220 lattice strains of the retained austenite phase were calculated by examining the changes of the X-ray diffraction peak positions during deformation. The 200 and 211 lattice strains of the various martensitic phases with similar crystal structures were determined by separating their overlapped diffraction peaks. Apart from tempered and untempered martensite, the diffraction peaks of freshly formed martensite as a result of austenite to martensite transformation can also be able separated due to high initial austenite volume fraction. The phase stresses are first estimated with an empirical relationship through the X-ray diffraction elastic constants (XREC). A multi-phase elasto-plastic self constant model (EPSC) is next used for more accurate determination of the constitutive behaviors of the various phases by comparing the predicted lattice strain distributions and global stress-strain curves with the measured ones. The determined constitutive laws will be used for microstructure-based modeling for sheet formability of the Q&P AHSS steel.

Hu, Xiaohua↗

An in situ imaging investigation of the effect of gas flow rates on directed energy deposition

Gas flow rates in Directed Energy Deposition (DED) Additive Manufacturing (AM) can significantly affect the quality of built parts by altering melt pool geometry. Using a DED process replicator and in situ synchrotron radiography, together with analogous experiments in an industrial DED machine, we investigate the impact of carrier gas and shield gas flow rates on build quality. The results reveal that there is a critical shield gas flow rate above which melt pools are flattened, tracks widen, and thus layer thickness decreases. The reduction in layer thickness is most prominent in conditions with low carrier gas flow rate, as the highly turbulent shield gas flow may divert slow moving powder particles away from the melt pool, decreasing capture efficiency. Very high flow rates increase internal porosity, as fast-moving particles impacting the melt pool surface can entrain chamber gas behind them. High gas flow rates also cool the melt pool, creating shallower melt pools with increased thermal gradients near the solidification front, increasing pore entrapment in the solidified track.

Additive manufacturing↗

Plasma structuring by the gradient drift instability at high latitudes and comparison with velocity shear driven processes

Using results of the in situ measurements made by the DE 2 satellite, the nature of plasma structuring at high latitudes, caused by the gradient drift instability process, is described. Using noon-midnight and dawn-dusk orbits of the DE 2 satellite, it was possible to examine the simultaneous density and electric field spectra of convecting large-scale plasma density enhancements in the polar cap known as 'patches', in directions parallel and perpendicular to their antisunward convection. The results provide evidence for the existence of at least two generic classes of instabilities operating in the high-latitude ionosphere: one driven by large-scale density gradients in a homogeneous convection field with respect to the neutrals, and the other driven by the structured convection field itself in an ambient ionosphere where density fluctuations are ubiquitous.

Basu, Sunanda↗

Technology Transfer of the CIGS Technology from the Laboratory to the PVMC: Cooperative Research and Development Final Report, CRADA Number CRD-12-496

PVMC, Inc. (PVMC) and Contractor (NREL) will work together under a CRADA, through a distinct statement of work (SOW) for each project. Each SOW will be negotiated as a modification of the CRADA between PVMC and NREL with a principal investigator (PI) identified by the contractor so as to define specific tasks and funding that reflect the scope and objectives of that project. Projects will focus on extended collaborations with well-defined, long-term goals that are mutually beneficial to PVMC and NREL. Projects under the CRADA may fall within the areas listed below in the summary of research results, calling upon the NREL capabilities and expertise. Modification 1: The first year of the CRADA will involve training PVMC personnel in the deposition process of the layers in the CIGS device based on the evaporation process, characterization methods used to track the properties of the films, device fabrication and integration of the layers into device compatible with the PVMC approach, and use standard ex-situ characterization tools, and standard and novel in-situ metrology tools for process characterization to insure that the unit films in the MDF facility have the properties defined above in the unit step evaluation. The scope of the CRADA statement of work is based on knowledge already in the literature and/or in background published IP. Modification 2: NREL loaned Ocean Optics spectrometer to PVMC. This was returned on 2/15/2018. Modification 3: The work under this CRADA is aimed at understanding several process effects on silicon wafers and/or solar cells. These include: (i) effects of wafering by diamond wire sawing on the surface damage and the strength of wafers, (ii) electronic characteristics of dielectric-Si interfaces, and (iii) characteristics of Si-Al interfaces formed during firing of silicon solar cells.

14 SOLAR ENERGY↗

In Situ TEM Investigation of Congruent Phase Transition and Structural Evolution of Nanostructured Silicon/Carbon Anode for Lithium Ion Batteries

It is well known that upon lithiation both crystalline and amorphous Si transform to a armorphous LixSi phase, which subsequently crystallizes to a (Li, Si) crystalline compound, either Li15Si or Li22Si5. Up to date, the detailed atomistic mechanism of this phase transformation, and degradation process in nanostructured Si, are not fully understood. Here, we report the microstructural evolution and phase transformation characteristic of a specially designed amorphous silicon (a-Si) coated carbon nanofiber (CNF) composite during charge/discharge process using in-situ TEM and density function theory molecular dynamic (DFT-MD) calculation. We found that the crystallization of Li15Si4 from amorphous LixSi is a spontaneous, congruent phase transition process without phase separation or large scale atomic motion, which is drastically different from what is expected from a classic nucleation and growth process. The a-Si layer is strongly bonded to the CNF and no spallation or cracking is observed during the early stages of cyclic charge/discharge. Reversible volume expansion/contraction upon charge/discharge is fully accommodated along the radial direction. However, with progressive cycling, damage in the form of surface roughness was gradually accumulated on the coating layer, which is believed to be the mechanism for the eventual capacity fade of the composite anode during long term charge/discharge cycling.

25 ENERGY STORAGE↗

Catabolism and interactions of uncultured organisms shaped by eco-thermodynamics in methanogenic bioprocesses

We currently understand the carbon cycle in methanogenic environments as trophic interactions revolving around interspecies H 2 transfer between organotrophs and methanogens. However, many H 2 -generating processes are thermodynamically sensitive to H 2 accumulation and can be inhibited by high H 2 concentrations produced by other metabolisms. To uncover how anaerobes combat this H 2 conflict in situ, we employ metagenomics and metatranscriptomics to revisit a model ecosystem that has inspired many foundational discoveries in anaerobic ecology – methanogenic bioreactors. Through analysis of 15 anaerobic digesters, we recover 1343 high-quality metagenome-assembled genomes (MAGs) and corresponding gene expression profiles for diverse uncultured lineages spanning 66 phyla and reconstruct their individual metabolic capacities. We discover that diverse uncultured organotrophic populations can drive H 2 -sensitive degradation through (i) metabolic coupling with concurrent H 2 -tolerant catabolism, (ii) unprecedented shifts from H 2 generation to CO 2 -reducing formate transfer and cytochrome/pili-mediated direct interspecies electron transfer for avoiding thermodynamic conflict, and (iii) integration of low-concentration O 2 as an ancillary thermodynamics-enhancing electron sink. Archaeal populations in situ support the above processes through novel metabolisms distinct from conventional methanogenesis – high-affinity H 2 oxidation driven by methyl-reducing methanogenesis and concomitant uptake of formate, electrons, and acetate from HS metabolism by Methanothrix. In total, synthesis of omics analyses and eco-thermodynamics reveals overlooked metabolic behavior and interactions of uncultured organisms that address a central issue in methanogenic carbon cycling, thermodynamic conflict among diverse concurrent metabolic processes.

59 BASIC BIOLOGICAL SCIENCES↗

Composite with In Situ Plenums

A document describes a high-performance thermal distribution panel (TDP) concept using high-conductivity (greater than 800 W/mK) macro composite skin with in situ heat pipes. The processing technologies proposed to build such a panel result in a one-piece, inseparable assembly with high conductance in both the X and Y planes. The TDP configuration can also be used to produce panels with high structural stiffness. The one-piece construction of the TDP eliminates the thermal interface between the cooling plenums and the heat spreader base, and obviates the need for bulky mounting flanges and thick heat spreaders used on baseline designs. The conductivity of the TDP can be configured to exceed 800 W/mK with a mass density below 2.5 grams per cubic centimeter. This material can provide efficient conductive heat transfer between the in situ heat plenums, permitting the use of thinner panel thicknesses. The plenums may be used as heat pipes, loop heat pipes, or liquid cooling channels. The panel technology used in the TDP is a macro-composite comprised of aluminum-encapsulated annealed pyrolytic graphite (APG). APG is highly aligned crystalline graphite with an in-plane thermal conductivity of 1,700 W/mK. APG has low shear strength and does not constrain the encapsulating material. The proposed concept has no thermal interfaces between the heat pipes and the spreader plate, further improving the overall conductance of the system. The in situ plenums can also be used for liquid cooling applications. The process can be used to fabricate structural panels by adding a second thin sheet.

Montesano, Mark↗

Deep Learning for In-Situ Layer Quality Monitoring during Laser-Based Directed Energy Deposition (LB-DED) Additive Manufacturing Process

Defects are a leading issue for the rejection of parts manufactured through the Directed Energy Deposition (DED) Additive Manufacturing (AM) process. In an attempt to illuminate and advance in situ quality monitoring and control of workpieces, we present an innovative data-driven method that synchronously collects sensing data and AM process parameters with a low sampling rate during the DED process. The proposed data-driven technique determines the important influences that individual printing parameters and sensing features have on prediction at the inter-layer qualification to perform feature selection. Three Machine Learning (ML) algorithms including Random Forest (RF), Support Vector Machine (SVM), and Convolutional Neural Network (CNN) are used. During post-production, a threshold is applied to detect low-density occurrences such as porosity sizes and quantities from CT scans that render individual layers acceptable or unacceptable. This information is fed to the ML models for training. Training/testing are completed offline on samples deemed “high-quality” and “low-quality”, utilizing only features recorded from the build process. CNN results show that the classification of acceptable/unacceptable layers can reach between 90% accuracy while training/testing on a “high-quality” sample and dip to 65% accuracy when trained/tested on “low-quality”/“high-quality” (respectively), indicating over-fitting but showing CNN as a promising inter-layer classifier.

36 MATERIALS SCIENCE↗

Phase transformations, microstructural refinement and defect evolution mechanisms in Al-Si alloys under non-hydrostatic diamond anvil cell compression

Non-hydrostatic compression of materials using a diamond anvil cell (DAC) can transform equilibrium microstructure of an alloy to novel, potentially metastable states. In this study, in situ synchrotron X-ray diffraction (XRD) during compression up to 24 GPa and subsequent ex situ, high resolution analytical electron microscopy (AEM) after decompression of an Al-Si alloy provided insight into the crystallographic changes during the compression as well as microstructural refinement, and defect structures caused by such a high pressure compression-decompression process. Pressure resolved in-situ synchrotron XRD was used to detail the phase transformation pathway of the eutectic Si phase in Al-Si alloy, from Si-I → Si-XI → Si-V during compression, and a final transformation predominantly to Si-III after decompression. Using scanning and transmission electron microscopy (S/TEM), site specific analysis of the alloy immediately underneath the anvil contact surface demonstrated a highly complex microstructure. A narrow region of thick amorphous Al oxide interspersed with nanocrystalline grains was found at the top surface. Underneath this Al oxide, while the majority the eutectic Si was transformed into highly-deformed, polycrystalline (PC) Si-III, a complex intermediate layer was discovered at the interface between Al and Si, comprised of a small fraction of Al nanocrystals and a majority of nanocrystalline Si-I. This combination of pressure resolved in-situ synchrotron XRD coupled with subsequent high resolution, electron microscopy resolved the phase transformation as well as non-equilibrium microstructures in a metallic alloy induced by a non-hydrostatic high pressure compression followed by decompression.

36 MATERIALS SCIENCE↗

Process-Defect-Structure-Property Correlations During Laser Powder Bed Fusion of Alloy 718: Role of In Situ and Ex Situ Characterizations

Components made by laser powder bed fusion (L-PBF) additive processes require extensive trial and error optimization to minimize defects and arrive at targeted microstructure and properties. In this paper, in situ infrared thermography and ex situ surface roughness measurements were explored as methodologies to ensure Inconel ® 718-part quality. For a given laser energy of 200 Watts, prismatic samples were produced with different exposure times (80 to 110 µs) and point spacings (80 to 110 µm). The infrared intensities from laser–material interaction zones were measured spatially and temporally. The conditions leading to higher IR intensity and lowest surface roughness values correlated well with less porosity and coarse solidification grain structure. The transition from highly columnar to misoriented growth is attributed to changes in thermal gradients and liquid–solid interface velocities. Hardness measurements and electron microscopy of the as-processed and post-processed heat-treated samples show complex transitions in microstructural states including the heavily dislocated FCC matrix, reduction of dislocation density, and copious precipitation, respectively. These results show that the geometry-process-structure-property correlations are dynamic, and they cascade depending on the transitions of phase states from powder to liquid to solid, as well as phase decompositions and deformations within the solid FCC phase. Finally, validity of using analytical weld process models to describe the above phenomena is also highlighted.

36 MATERIALS SCIENCE↗

Strategies to overcome electron-beam issues in liquid phase TEM: Study of chemical processes

Abstract Liquid phase (or liquid cell) transmission electron microscopy (TEM) has become a powerful platform for in situ investigation of various chemical processes at the nanometer or atomic level. The electron beam for imaging can also induce perturbation to the chemical processes. Thus, it has been a concern that the observed phenomena in a liquid cell could deviate from the real-world processes. Strategies have been developed to overcome the electron-beam-induced issues. This article provides an overview of the electron-beam effects, and discusses various strategies in liquid cell TEM study of nucleation, growth, and self-assembly of nanoscale materials, where an electron beam is often used to initiate the reactions, and highly electron-beam-sensitive electrochemical reactions. Graphical abstract

Zheng, Wenjing↗

Mechanistic Probes of Zeolitic Imidazolate Framework for Photocatalytic Application

In this work, we report a zeolitic imidazolate framework (ZIF-67) with remarkable activity for hydrogen evolution reaction (HER) of 40,500 μmol H 2 /g MOF, which is, to the best of our knowledge, the highest activity achieved by any MOF system. This result necessitated assessment of its atomic-scale mechanistic function for HER using advanced spectroscopy techniques including time-resolved optical (OTA) and in situ X-ray absorption (XAS) spectroscopy. Through the correlation of OTA results with catalytic performance, we demonstrated that the electron transfer (ET) rather than energy transfer (ENT) pathway between photosensitizer and ZIF-67 is the key factor that controls the efficiency of HER activity, as HER activity that undergoes ET pathway is 3 orders of magnitude higher than that of ENT process. Here, using in situ XAS, we unraveled the spectral features for key intermediate species which are likely responsible for the rate determining process under turn over conditions. Finally, this work represents an original approach to study porous ZIF materials at the molecular level using advanced spectroscopic techniques, providing unprecedented insights into the photoactive nature of ZIF frameworks.

36 MATERIALS SCIENCE↗

Dynamic Transmission Electron Microscopy

Dynamic transmission electron microscopy (DTEM) combines the benefits of high spatial resolution electron microscopy with the high temporal resolution of ultrafast lasers. The incorporation of these two components into a single instrument provides a perfect platform for in situ observations of material processes. However, previous DTEM applications have focused on observing structural changes occurring in samples exposed to high vacuum. Therefore, in order to expand the pump-probe experimental regime to more natural environmental conditions, in situ gas and liquid chambers must be coupled with Dynamic TEM. This chapter describes the current and future applications of in situ liquid DTEM to permit time-resolved atomic scale observations in an aqueous environment, Although this chapter focuses mostly on in situ liquid imaging, the same research potential exists for in situ gas experiments and the successful integration of these techniques promises new insights for understanding nanoparticle, catalyst and biological protein dynamics with unprecedented spatiotemporal resolution.

Dynamic TEM↗