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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 541 records · Page 30
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Methods for Determining the Infrared Complex Refractive Indices n (λ) and k (λ) from Organic Solid Powders: Comparison of a Sucrose Single Crystal and a Pressed Pellet

There exists a need to measure optical constants n and k for many materials, especially organic solids in the infrared spectral region, but at present, there are only two established methods for making such measurements: single-angle (SA) reflectance and infrared spectroscopic ellipsometry (IRSE). The former derives the n/k vectors via measurement of the change in the amplitude of light reflected from the sample and then uses the Kramers–Kronig transform, while the latter measures the change in polarization of the reflected light from the sample to derive n/k. Here we make a direct comparison between the n/k vectors derived from SA measurements of a sucrose single crystal and the n/k values obtained after the crystal had been crushed, ground to powder, and pressed into a pellet form. The pellet was measured not only by SA but also via the IRSE method, and we found that pressing specular-quality pellets was critical, especially for the SA data. The n/k values of this typical organic molecule all agree to within 0.04 root-mean-square error, confirming that a pressed pellet can be used instead of a crystal to derive the intrinsic n/k vectors. In conclusion, this result is important for the many organic materials that, unlike sugar, do not have centimeter-sized crystals readily available.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Strain wave pathway to semiconductor-to-metal transition revealed by time-resolved X-ray powder diffraction

One of the main challenges in ultrafast material science is to trigger phase transitions with short pulses of light. Here we show how strain waves, launched by electronic and structural precursor phenomena, determine a coherent macroscopic transformation pathway for the semiconducting-to-metal transition in bistable Ti 3 O 5 nanocrystals. Employing femtosecond powder X-ray diffraction, we measure the lattice deformation in the phase transition as a function of time. We monitor the early intra-cell distortion around the light absorbing metal dimer and the long range deformations governed by acoustic waves propagating from the laser-exposed Ti 3 O 5 surface. We developed a simplified elastic model demonstrating that picosecond switching in nanocrystals happens concomitantly with the propagating acoustic wavefront, several decades faster than thermal processes governed by heat diffusion.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Keyhole fluctuation and pore formation mechanisms during laser powder bed fusion additive manufacturing

Keyhole porosity is a key concern in laser powder-bed fusion (LPBF), potentially impacting component fatigue life. However, some keyhole porosity formation mechanisms, e.g., keyhole fluctuation, collapse and bubble growth and shrinkage, remain unclear. Using synchrotron X-ray imaging we reveal keyhole and bubble behaviour, quantifying their formation dynamics. The findings support the hypotheses that: (i) keyhole porosity can initiate not only in unstable, but also in the transition keyhole regimes created by high laser power-velocity conditions, causing fast radial keyhole fluctuations (2.5-10 kHz); (ii) transition regime collapse tends to occur part way up the rear-wall; and (iii) immediately after keyhole collapse, bubbles undergo rapid growth due to pressure equilibration, then shrink due to metal-vapour condensation. Concurrent with condensation, hydrogen diffusion into the bubble slows the shrinkage and stabilises the bubble size. The keyhole fluctuation and bubble evolution mechanisms revealed here may guide the development of control systems for minimising porosity.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2022

Observation of a reduced-turbulence regime with boron powder injection in a stellarator

Abstract In state-of-the-art stellarators, turbulence is a major cause of the degradation of plasma confinement. To maximize confinement, which eventually determines the amount of nuclear fusion reactions, turbulent transport needs to be reduced. Here we report the observation of a confinement regime in a stellarator plasma that is characterized by increased confinement and reduced turbulent fluctuations. The transition to this regime is driven by the injection of submillimetric boron powder grains into the plasma. With the line-averaged electron density being kept constant, we observe a substantial increase of stored energy and electron and ion temperatures. At the same time, the amplitude of the plasma turbulent fluctuations is halved. While lower frequency fluctuations are damped, higher frequency modes in the range between 100 and 200 kHz are excited. We have observed this regime for different heating schemes, namely with both electron and ion cyclotron resonant radio frequencies and neutral beams, for both directions of the magnetic field and both hydrogen and deuterium plasmas.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2022

In situ melt pool measurements for laser powder bed fusion using multi sensing and correlation analysis

Laser powder bed fusion is a promising technology for local deposition and microstructure control, but it suffers from defects such as delamination and porosity due to the lack of understanding of melt pool dynamics. To study the fundamental behavior of the melt pool, both geometric and thermal sensing with high spatial and temporal resolutions are necessary. This work applies and integrates three advanced sensing technologies: synchrotron X-ray imaging, high-speed IR camera, and high-spatial-resolution IR camera to characterize the evolution of the melt pool shape, keyhole, vapor plume, and thermal evolution in Ti–6Al–4V and 410 stainless steel spot melt cases. Aside from presenting the sensing capability, this paper develops an effective algorithm for high-speed X-ray imaging data to identify melt pool geometries accurately. Preprocessing methods are also implemented for the IR data to estimate the emissivity value and extrapolate the saturated pixels. Quantifications on boundary velocities, melt pool dimensions, thermal gradients, and cooling rates are performed, enabling future comprehensive melt pool dynamics and microstructure analysis. The study discovers a strong correlation between the thermal and X-ray data, demonstrating the feasibility of using relatively cheap IR cameras to predict features that currently can only be captured using costly synchrotron X-ray imaging. Such correlation can be used for future thermal-based melt pool control and model validation.

47 OTHER INSTRUMENTATION↗
DOE OSTI2026

High-pressure neutron powder diffraction study of an arsenolite deuterium inclusion compound: structure and formation kinetics

High-pressure variable-temperature neutron powder diffraction was employed to investigate the synthesis and structural properties of arsenolite (As 4 O 6 ), a cubic arsenic( III ) oxide polymorph, and its inclusion compound with deuterium. The compound forms with the stoichiometry As 4 O 6 ·2D 2 , consistent with earlier findings. At 295 K and 1.96(2) GPa, D 2 molecules occupy the 16c site (0, 0, 0) and are aligned along the <111> direction. The diffraction data suggest that the D 2 molecules at this site become rotationally disordered upon decompression to 0.78(2) GPa at 120 K, while no occupancy is observed at the 8a position (⅛, ⅛, ⅛) under any of the studied conditions. The kinetic data of the high-pressure inclusion compound synthesis at 1.56(2) and 1.96(2) GPa were analyzed using the Avrami model. The Avrami exponent, 0.135(16), remains invariant with pressure, demonstrating that the reaction topochemistry is unaffected by compression. Similarly, the reaction rates, 0.29(3) and 0.23(3) min −0.135 at 1.56(2) and 1.96(2) GPa, respectively, exhibit negligible pressure dependence and suggest a surprisingly low activation volume of 1.6 cm 3 mol −1 for the reaction. These results provide detailed insight into the structural dynamics and kinetics of deuterium inclusion in arsenolite under high pressure.

Guńka, Piotr A. [Warsaw University of Technology (↗
DOE OSTI2022

High-throughput, in situ imaging of multi-layer powder-blown directed energy deposition with angled nozzle

Laser metal additive manufacturing (AM) has become an increasingly popular technology due to its flexibility in geometry and materials. As one of the commercialized additive processes, powder-blown directed energy deposition (DED) has been used in multiple industries such as aerospace, automotive, medical device, etc. However, a lack of fundamental understanding remains for this process, and many opportunities for alloy development and implementation can be identified. A high-throughput, in situ DED system capable of multi-layer builds that can address these issues is presented here. In this work, implications of layer heights and energy density are investigated through an extensive process parameter sweep, showcasing the power of a high-throughput setup while also discussing multi-layer interactions.

47 OTHER INSTRUMENTATION↗
DOE OSTI2022

A laser powder bed fusion system for operando synchrotron x-ray imaging and correlative diagnostic experiments at the Stanford Synchrotron Radiation Lightsource

Laser powder bed fusion (LPBF) is a highly dynamic multi-physics process used for the additive manufacturing (AM) of metal components. Improving process understanding and validating predictive computational models require high-fidelity diagnostics capable of capturing data in challenging environments. Synchrotron x-ray techniques play a vital role in the validation process as they are the only in situ diagnostic capable of imaging sub-surface melt pool dynamics and microstructure evolution during LPBF-AM. In this article, a laboratory scale system designed to mimic LPBF process conditions while operating at a synchrotron facility is described. The system is implemented with process accurate atmospheric conditions, including an air knife for active vapor plume removal. Significantly, the chamber also incorporates a diagnostic sensor suite that monitors emitted optical, acoustic, and electronic signals during laser processing with coincident x-ray imaging. The addition of the sensor suite enables validation of these industrially compatible single point sensors by detecting pore formation and spatter events and directly correlating the events with changes in the detected signal. Experiments in the Ti–6Al–4V alloy performed at the Stanford Synchrotron Radiation Lightsource using the system are detailed with sufficient sampling rates to probe melt pool dynamics. X-ray imaging captures melt pool dynamics at frame rates of 20 kHz with a 2 µm pixel resolution, and the coincident diagnostic sensor data are recorded at 470 kHz. Furthermore, this work shows that the current system enables the in situ detection of defects during the LPBF process and permits direct correlation of diagnostic signatures at the exact time of defect formation.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Energy dispersive x-ray diffraction of luminescent powders: A complement to visible phosphor thermometry

Energy-dispersive x-ray diffraction of thermographic phosphors has been explored as a complementary temperature diagnostic to visible phosphor thermometry in environments where the temperature-dependent optical luminescence of the phosphors is occluded. Powder phosphor samples were heated from ambient to 300°C in incremental steps and probed with polychromatic synchrotron x rays; scattered photons were collected at a fixed diffraction angle of 3.9°. Crystal structure, lattice parameters, and coefficients of thermal expansion were calculated from the diffraction data. Finally, of the several phosphors surveyed, YAG:Dy, ZnO:Ga, and GOS:Tb were found to be excellent candidates for diffraction thermometry due to their strong, distinct diffraction peaks that shift in a repeatable and linear manner with temperature.

47 OTHER INSTRUMENTATION↗
DOE OSTI2024

Direct mechanistic connection between acoustic signals and melt pool morphology during laser powder bed fusion

Various nondestructive diagnostic techniques have been proposed for in situ process monitoring of laser powder bed fusion (LPBF), including melt pool pyrometry, whole-layer optical imaging, acoustic emission, atomic emission spectroscopy, high speed melt pool imaging, and thermionic emission. Correlations between these in situ monitoring signals and defect formation have been demonstrated with acoustic signals having been shown to predict pore formation with especially high confidence in recent machine learning studies. Here, in this work, time-resolved acoustic data are collected in both the conduction and keyhole welding regimes of LPBF-processed Ti-6Al-4V alloy. A non-dimensionalized Strouhal number analysis, used in whistle aeroacoustics, is applied to demonstrate that the acoustic signals recorded in the keyhole regimes can be directly associated with the vapor depression morphology. This mechanistic understanding developed from whistle aeroacoustics shows that acoustic monitoring during the LPBF process can provide a direct probe into the vapor depression dynamics and defect occurrence, especially in the keyhole regimes relevant to printing and defect formation.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Vented and sealed cookoff of powdered and pressed ε-CL-20

In this work, we have completed a series of vented and sealed cookoff experiments of the ε-polymorph of CL-20 in our Sandia Instrumented Thermal Ignition (SITI) apparatus using both powder and pressed pellets at nominal densities of 313 ± 8 kg/m 3 and 1030 ± 4 kg/m 3 , respectively. The boundary temperature of our aluminum confinement cylinder was ramped in 10 minutes from room temperature to a prescribed set-point temperature ranging between 448 nd 468 K and held at the set-point temperature until ignition. A universal cookoff model (UCM) has been calibrated using the ε-CL-20 SITI data to predict pressurization and thermal ignition of ε-CL-20. The ignition model was validated by using one-dimensional time-to-explosion (ODTX) ignition data from a different laboratory. We found that a thirtyfold increase in the reaction rates due to liquefaction at 520 K could explain the high temperature ODTX cookoff data. The model gives a plausible explanation of why melting is important in fast cookoff events involving CL-20. Our model also gives support to 520 K as the liquefaction point of CL-20, which has different values in the literature.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Embedding thermocouples in SS316 with laser powder bed fusion

Recent advances in manufacturing technologies have enabled the fabrication of complex geometries for a wide range of applications, including the energy, aerospace, and civil sectors. The ability to integrate sensors at critical locations within these complex components during the manufacturing process could benefit process monitoring and control by reducing reliance on models to relate surface measurements to internal phenomena. This study investigated embedding thermocouples in a SS316 matrix using laser powder bed fusion. Under optimal processing conditions, embedded thermocouples were characterized post-building, finding good bonding to the matrix with no melt pool penetration to the sensing elements. Futher, the embedded thermocouple performed similarly to an identical non-embedded thermocouple during thermal testing to 500 °C with only a slight difference in response time, which was attributed to the differences in mass and the associated thermal time constants.

image analysis↗
DOE OSTI2022

Real-time wall conditioning and recycling modification utilizing boron and boron nitride powder injections into the Large Helical Device

Controlled particulate injections from the PPPL impurity powder dropper (IPD) into the Large Helical Device have demonstrated positive effects on the wall conditions on both an intra and inter-shot basis. Here injections over a range of densities, input powers, pulse lengths, heating schemes, injection quantities and main ion species show conclusive evidence of improvement to plasma wall conditions. Successful injections are confirmed by both spectroscopic measurements as well as real-time visible camera signals. In 7 s long plasmas the responses include a reduction in wall recycling as well as a reduction in native impurity content as observed over the course of several discharges. For plasmas longer than 40 s, improvements to the recycling rate and increased impurity control are observed in real time as a consequence of the extended particulate injections. These experiments demonstrate the extended applicability of this solid particulate conditioning technique to the control and maintenance of the plasma wall conditions. In addition they are an important initial step in the development of the real-time boronization technique as a supplement to standard conditioning scenarios.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2024

Target development using the method of High-Intensity Vibrational Powder Plating (HIVIPP) at the Center for Accelerator Target Science (CATS) at Argonne National Laboratory (ANL)

One of the primary goals of the Center for Accelerator Target Science (CATS) is to provide targets and foils in support of the ATLAS User Facility and the Low-Energy community at large. While a wide array of target production techniques are available at CATS, new methods that must be explored invariably arise. One such technique, the High-Intensity Vibrational Powder Plating (HIVIPP), was first reported in 1997 by Isao Sugai. It was developed to produce targets and stripper foils that were difficult to make by standard methods. At Argonne National Laboratory (ANL), we have successfully constructed and tested a simple system for this purpose. We have produced targets of carbon and titanium on various metal backings using the HIVIPP method. We are currently in the exciting phase of exploring the production of other elements, including isotopically enriched and radioactive material. This work is in progress and will be further detailed with specific examples.

47 OTHER INSTRUMENTATION↗
DOE OSTI2022

Low temperature CVD growth of WSe 2 enabled by moisture-assisted defects in the precursor powder

Two-dimensional transition metal dichalcogenides (TMDs) have been proposed for a wide variety of applications, such as neuromorphic computing, flexible field effect transistors, photonics, and solar cells, among others. However, for most of these applications to be feasible, it is necessary to integrate these materials with the current existing silicon technology. Although chemical vapor deposition is a promising method for the growth of high-quality and large-area TMD crystals, the high temperatures necessary for the growth make this technique incompatible with the processes used in the semiconductor industry. Herein, we demonstrate the possibility of low-temperature growth of TMDs, using tungsten selenide (WSe 2 ) as a model, by simply using moisture-assisted defective tungsten oxide (WO 3 ) precursor powders during the growth of these materials. Density functional theory calculations reveal the mechanism by which moisture promotes the defect formation on the precursor crystal structure and how it dictates the reduction of the temperature of the growth. The results were compared with the standard growth at high temperatures and with a precursor mixture with alkali salts to show the high quality of the WSe 2 grown at temperatures as low as 550 °C. To conclude, the work improves the understanding of nucleation and growth mechanisms of WSe 2 at low temperatures and provides a useful strategy for the growth of TMDs at temperatures required for the back-end-of-line compatibility with current silicon technology.

2D materials↗
DOE OSTI2024

Sub-millisecond keyhole pore detection in laser powder bed fusion using sound and light sensors and machine learning

Laser powder bed fusion is a mainstream additive manufacturing technology widely used to manufacture complex parts in prominent sectors, including aerospace, biomedical, and automotive industries. However, during the printing process, the presence of an unstable vapor depression can lead to a type of defect called keyhole porosity, which is detrimental to the part quality. In this study, we developed an effective approach to locally detect the generation of keyhole pores during the printing process by leveraging machine learning and a suite of optical and acoustic sensors. Simultaneous synchrotron x-ray imaging allows the direct visualization of pore generation events inside the sample, offering high-fidelity ground truth. A neural network model adopting SqueezeNet architecture using single-sensor data was developed to evaluate the fidelity of each sensor for capturing keyhole pore generation events. Our comparative study shows that the near infrared images gave the highest prediction accuracy, followed by 100 kHz and 20 kHz microphones, and the photodiode sensitive to processing laser wavelength had the lowest accuracy. Using a single sensor, over 90% prediction accuracy can be achieved with a temporal resolution as short as 0.1 ms. A data fusion scheme was also developed with features extracted using SqueezeNet neural network architecture and classification using different machine learning algorithms. Our work demonstrates the correlation between the characteristic optical and acoustic emissions and the keyhole oscillation behavior, and thereby provides strong physics support for the machine learning approach.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Cost of Using Laser Powder Bed Fusion to Fabricate a Molten Salt-to-Supercritial Carbon Dioxide Heat Exchanger for Concentrating Solar Power

Advances in manufacturing technologies and materials are crucial to the commercial deployment of energy technologies. We present the case of concentrating solar power (CSP) with molten salt (MS) thermal storage, where low-cost, high-efficiency heat exchangers (HXs) are needed to achieve cost competitiveness. Here, the materials required to tolerate the extreme operating conditions in CSP systems make it difficult or infeasible to produce them using conventional manufacturing processes. Although it is technically possible to produce HXs with adequate performance using additive manufacturing, specifically laser powder bed fusion (LPBF), here we assess whether doing so is cost-effective. We describe a process-based cost model (PBCM) to estimate the cost of fabricating a MS-to-supercritical carbon dioxide HX using LPBF. The PBCM is designed to identify modifications to designs, process choices, and manufacturing innovations that have the greatest effect on manufacturing cost. Our PBCM identified HX design and LPBF process modifications that reduced projected HX cost from $\$750$ per kilo-Watt thermal (kW-th) ($\$8$ /cm 3 ) to $\$350$ /kW-th ($\$6/$ cm 3 ) using currently available LPBF technology, and down to $\$220$ /kW-th ($\$4$ /cm 3 ) with improvements in LPBF technology that are likely to be achieved in the near term. The PBCM also informed a redesign of the HX design that reduced projected costs to $\$140$ –160/kW-th ($\$3$ /cm 3 ).

36 MATERIALS SCIENCE↗
DOE OSTI2022

Laser melting modes in metal powder bed fusion additive manufacturing

In laser powder bed fusion additive manufacturing of metals, extreme thermal conditions create many highly dynamic physical phenomena such as vaporization and recoil, Marangoni convection, and protrusion and keyhole instability. Collectively however, the full set of phenomena is too complicated for practical applications and, in reality, the melting modes are used as a guideline for printing. With increasing local material temperature beyond the boiling point, the mode can change from conduction to keyhole. These mode designations ignore laser-matter interaction details but in many cases are adequate to determine the approximate microstructures and hence the properties of the build. To date, no consistent, common, and coherent definitions have been agreed upon because of historic limitations in melt pool and vapor depression morphology measurements. Here, we distinguish process-based definitions of different melting modes from those based on postmortem evidence. The latter are mainly derived from the transverse cross-sections of the fusion zone, whereas the former come directly from time-resolved x-ray imaging of melt pool and vapor depression morphologies. These process-based definitions are more strict and physically sound, and they offer new guidelines for laser additive manufacturing practices and create new research directions. Further, we highlight the significance of the keyhole, which substantially enhances the laser energy absorption by the melt pool. Recent studies strongly suggest that stable-keyhole laser melting enables efficient, sustainable, and robust additive manufacturing. The realization of this scenario demands the development of multiphysics models, signal translations from morphology to other feasible signals, and in-process metrology across platforms and scales.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗