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NASA NTRS2003

Flame Synthesis Of Single-Walled Carbon Nanotubes And Nanofibers

Carbon nanotubes are widely sought for a variety of applications including gas storage, intercalation media, catalyst support and composite reinforcing material [1]. Each of these applications will require large scale quantities of CNTs. A second consideration is that some of these applications may require redispersal of the collected CNTs and attachment to a support structure. If the CNTs could be synthesized directly upon the support to be used in the end application, a tremendous savings in post-synthesis processing could be realized. Therein we have pursued both aerosol and supported catalyst synthesis of CNTs. Given space limitations, only the aerosol portion of the work is outlined here though results from both thrusts will be presented during the talk. Aerosol methods of SWNT, MWNT or nanofiber synthesis hold promise of large-scale production to supply the tonnage quantities these applications will require. Aerosol methods may potentially permit control of the catalyst particle size, offer continuous processing, provide highest product purity and most importantly, are scaleable. Only via economy of scale will the cost of CNTs be sufficient to realize the large-scale structural and power applications on both earth and in space. Present aerosol methods for SWNT synthesis include laser ablation of composite metalgraphite targets or thermal decomposition/pyrolysis of a sublimed or vaporized organometallic [2]. Both approaches, conducted within a high temperature furnace, have produced single-walled nanotubes (SWNTs). The former method requires sophisticated hardware and is inherently limited by the energy deposition that can be realized using pulsed laser light. The latter method, using expensive organometallics is difficult to control for SWNT synthesis given a range of gasparticle mixing conditions along variable temperature gradients; multi-walled nanotubes (MWNTs) are a far more likely end products. Both approaches require large energy expenditures and produce CNTs at prohibitive costs, around $500 per gram. Moreover these approaches do not possess demonstrated scalability. In contrast to these approaches, flame synthesis can be a very energy efficient, low-cost process [3]; a portion of the fuel serves as the heating source while the remainder serves as reactant. Moreover, flame systems are geometrically versatile as illustrated by innumerable boiler and furnace designs. Addressing scalability, flame systems are commercially used for producing megatonnage quantities of carbon black [4]. Although it presents a complex chemically reacting flow, a flame also offers many variables for control, e.g. temperature, chemical environment and residence times [5]. Despite these advantages, there are challenges to scaling flame synthesis as well.

Wal, Randy L. Vander↗

NASA NTRS2003

Bandwidth Efficient Baseband Multi-Modulator

The High Rate Baseband Multi-Modulator (HRBM) ASIC is being developed to provide High-speed Bandwidth Efficient Modulations to NASA missions. Bandwidth efficiencies from 2.0 bits/symbol/Hz to 2.75 bits/symbl/Hz are selectable from three CCSDS modulations: Gaussian Minimum Shift Keying (GMSK), Filter Offset Quadrature Phase Shift Keying (Filtered- OQSK) and 8-Phase Shift Keying Trellis Coded Modulation (8-PSK TCM). An FPGA version of the HRBM is developed first to verify the individual modulation designs and characterize timing and performance issues involved with digital baseband modulation synthesis. A Finite Input Response (FIR) filter is included to provided baseband pulse shaping to reduce out-of-band spectral emissions. This is filter is programmable and can be tailored to meet system requirements. The ASIC is targeted to provide up to 600 Mbps throughput and will provide serial as well as parallel input. This paper provides an overview of the technology development and current status.

Fong, Wai↗

DOE OSTI2025

Online Bayesian State Estimation for Real-Time Monitoring of Growth Kinetics in Thin Film Synthesis

Rapid validation of newly predicted materials through autonomous synthesis requires real-time adaptive control methods that exploit physics knowledge, a capability that is lacking in most systems. Here, in this study, we demonstrate an approach to enable real-time control of thin film synthesis by combining in situ optical diagnostics with a Bayesian state estimation method. We developed a physical model for film growth and applied the direct filter (DF) method for real-time estimation of nucleation and growth rates during pulsed laser deposition (PLD). We validated the approach using simulated and experimental reflectivity data for WSe 2 growth and ultimately deployed the algorithm on an autonomous PLD system during the growth of 1T'-MoTe 2 . The DF robustly estimates growth parameters in real time at early stages of growth, down to 15% monolayer area coverage. This fusion of in situ diagnostics, data assimilation, and physical modeling opens new opportunities in adaptive control of synthesis trajectories toward desired material states.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Collaborative Research: Unravelling the Physics Associated with the Production of Extremely Dense Plasma States of Microscale (Final Report) Nanosecond-pulsed Discharges

The aim of this project is to study and establish the physical mechanisms that contribute to the formation of anomalously dense plasmas in high-pressure nanosecond-pulsed discharges. These discharges have a broad range of applications such as plasma-assisted combustion, plasma flow actuators, biomedical sterilization and exotic materials synthesis. The structure and formation of these discharges, producing high plasma densities of ~10 14 -10 15 cm -3 , are well-studied and understood. Fast-pulsed microscale high-pressure discharges can be driven to even higher densities of > 10 19 cm -3 , approaching warm dense matter conditions. The mechanisms that generate these plasmas have not been understood. Analysis of the warm dense matter state under laboratory conditions is an expensive and non-trivial endeavor. For instance, dense plasmas can be generated by electrical explosions of metal foils and wires. Plasmas generated after the explosion have a short lifetime and often present difficult conditions for diagnostics. Generation of dense plasmas was also achieved during high-voltage nanosecond pulsed discharges when the so-called explosive electron emission is obtained. Unfortunately, this process is very difficult to control for the studies of warm dense matter. In our recent study, we have shown that additional heating of plasma by lasers can further increase the density of plasma and even lead to the fully ionized state. This method, potentially, allows better control of the plasma parameters. In this work, we studied a second stage laser-heated micro-discharge using a self-consistent one-dimensional particle-in-cell Monte Carlo-collision (1D PIC-MCC) model coupled with Maxwell’s equations. We predicted the generation of a fully ionized plasma on the picosecond time scale. However, this model considered the plasma as an ideal gas despite the high pressure and the nearly fully ionized state. The ideal plasma model assumes that the dilute gas approximation is valid, where the inter-particle interactions are negligible. For charged particles this assumption holds as long as the shielded Coulomb potential assumption is valid. For very high plasma densities, this concept breaks down since the Debye sphere surrounding each charged particle no longer contains enough electrons to statistically provide the shielding of the single particle Coulomb interaction potential. At such densities, the plasma can no longer be described as ideal and non-ideal coupling effects need to be considered. In this report, we elucidate our recent work of developing a PIC-MCC model with improvements for non-ideal plasma conditions due to Coulomb coupling at high densities. In particular, we study the interaction of green light radiation and a dense microplasma, and explore the non-ideal plasma effects in this interaction. In this computational model, we implement the two most important non-ideal effects: ionization potential depression (IPD) and enhanced collision cross sections. Our primary goal is to study the physics associated with electromagnetic (EM) wave heating, also called the second-stage wave-heating, and establish the role of plasma non-ideality in this phenomenon. Our secondary goal is to improve the chemistry mechanism of the 1D PIC-MCC model by including a more detailed excited species collision treatment. At high pressures, stepwise ionization from excited species might play an important role in the ionization process. Previously, this ionization mechanism was neglected due to the excitation collision cross section of xenon being smaller than that of ionization. However, a preliminary study showed that the excited species density in the initial microplasma was an order of magnitude higher than the electron density. Therefore, my aim is to determine the significance of this additional ionization pathway to the plasma generation.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

NASA NTRS2001

Synthesis of Two-Photon Materials and Two-Photon Liquid Crystals

The duration of the grant was interrupted by two major accidents that the PI met with-- an auto accident in Pasadena, CA during her second summer at JPL which took almost eight months for recovery and a second accident during Fall 2000 that left her in crutches for the entire semester. Further, the time released agreed by the University was not given in a timely fashion. The candidate has been given post-grant expire time off. In spite of all these problems, the PI synthesized a number of new two-photon materials and studied the structure-activity correlation to arrive at the best-optimized structure. The PI's design proved to be one of the best in the sense that these materials has a hitherto unreported two-photon absorption cross section. Many materials based on PI's design was later made by the NASA colleague. This is Phase 1. Phase II of this grant is to orate liquid crystalline nature into this potentially useful materials and is currently in progress. Recent observations of nano- and pico-second response time of homeotropically aligned liquid crystals suggest their inherent potentials to act as laser hardening materials, i.e., as protective devices against short laser pulses. The objective of the current project is to exploit this potential by the synthesis of liquid crystals with high optical nonlinearity and optimizing their performance. The PI is trying structural variations to bring in liquid crystalline nature without losing the high two-photon cross section. Both Phase I and Phase II led to many invited presentations and publications in reputed journals like 'Science' and 'Molecular Crystals'. The list of presentations and reprints are enclosed. Another important and satisfying outcome of this grant is the opportunity that this grant offered to the budding undergraduate scientists to get involved in a visible research of international importance. All the students had a chance to learn a lot during research, had the opportunity to present their work at the National level conferences. They continue to retain their interest in their research and went on to accomplish further laurels.

Subramaniam, Girija↗

DOE OSTI2024

Investigation of W-SiC compositionally graded films as a divertor material

W-SiC composite material is a promising plasma-facing material candidate alternative to pure W due to the low neutron activation, low impurity radiation, and low tritium diffusivity of SiC while leveraging the high erosion resistance of the W armor. Additionally, W and SiC have high thermomechanical compatibility given their similar thermal expansion rates. The present study addresses the synthesis and performance of compositionally graded W-SiC films fabricated by pulsed-DC magnetron sputtering. Compositional gradients were characterized using transmission electron microscopy (TEM) and energy-dispersive X-ray spectroscopy (EDS), and crystallographic information was obtained using electron diffraction and X-ray diffraction (XRD). Samples were exposed to L-mode deuterium plasma discharges in the DIII-D tokamak using the Divertor Material Evaluation System (DiMES). Post-mortem characterizations were performed using scanning electron microscopy (SEM) and XRD. Electron diffraction and XRD showed that the compositionally graded W-SiC films were composed of polycrystalline W and amorphous SiC with amorphous W+SiC interlayers. No macroscopic delamination or microstructural changes were observed under mild exposure conditions. Here, this study serves as a preliminary examination of W-SiC compositionally graded composites as a potential candidate divertor material in future tokamak devices.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Optical properties of differing nanolayered structures of divalent europium doped barium fluoride thin films synthesized by pulsed laser deposition

Optically-active thin films are employed in a variety of applications, such as LEDs and photovoltaics, due to their ability to act as up- or down-photon energy converters. Their performance depends critically on their composition and structure; thus, the use of novel synthesis techniques that allow for their control at the nanoscale level can result in improved efficiency and practicality. Here, layered thin films consisting of Eu 2+ - doped BaF 2 nanocrystalline layers separated by amorphous Al 2 O 3 were synthesized via sequential pulsed laser deposition using three separate targets for the different components; this synthesis technique provides precise control of layer thickness at the nanoscale along with dopant distribution within the film. Cross-sectional transmission electron microscopy analysis verified the desired nano-layering. Post-deposition heat treatments in a nitrogen atmosphere resulted in samples exhibiting steady emission with a broad peak ranging from 400 to 600 nm and a shoulder at 410 nm. The CIE 1931 chromaticity coordinates are x = 0.26-0.29 and y = 0.32-0.35 and vary as a function of the sample configuration. Because the chromaticity coordinates are close to those of a pure white light (x = 0.33, y = 0.33), these films demonstrate advantageous properties for applications with UV-pumped white light LEDs.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Complex Attosecond Waveform Synthesis at FEL FERMI

Free-electron lasers (FELs) can produce radiation in the short wavelength range extending from the extreme ultraviolet (XUV) to the X-rays with a few to a few tens of femtoseconds pulse duration. These facilities have enabled significant breakthroughs in the field of atomic, molecular, and optical physics, implementing different schemes based on two-color photoionization mechanisms. In this article, we present the generation of attosecond pulse trains (APTs) at the seeded FEL FERMI using the beating of multiple phase-locked harmonics. We demonstrate the complex attosecond waveform shaping of the generated APTs, exploiting the ability to manipulate independently the amplitudes and the phases of the harmonics. The described generalized attosecond waveform synthesis technique with an arbitrary number of phase-locked harmonics will allow the generation of sub-100 as pulses with programmable electric fields.

47 OTHER INSTRUMENTATION↗

DOE OSTI2022

Standardized excitable elements for scalable engineering of far-from-equilibrium chemical networks

Engineered far-from-equilibrium synthetic chemical networks that pulse or switch states in response to environmental signals could precisely regulate the kinetics of chemical synthesis or self-assembly. Currently, such networks must be extensively tuned to compensate for the different activities of and unintended reactions between a network’s various chemical components. Modular elements with standardized performance could be used to rapidly construct networks with designed functions. Here we develop standardized excitable chemical regulatory elements, termed genelets, and use them to construct complex in vitro transcriptional networks. We develop a protocol for identifying >15 interchangeable genelet elements with uniform performance and minimal crosstalk. Furthermore, these elements can be combined to engineer feedforward and feedback modules whose dynamics match those predicted by a simple kinetic model. Modules can then be rationally integrated and organized into networks that produce tunable temporal pulses and act as multistate switchable memories. Standardized genelet elements, and the workflow to identify more, should make engineering complex far-from-equilibrium chemical dynamics routine.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

Automated Laboratory Kilogram-Scale Graphene Production from Coal

The flash Joule heating (FJH) method converts many carbon feedstocks into graphene in milliseconds to seconds using an electrical pulse. This opens an opportunity for processing low or negative value resources, such as coal and plastic waste, into high value graphene. Here, in this work, a lab-scale automation FJH system that allows the synthesis of 1.1 kg of turbostratic flash graphene from coal-based metallurgical coke (MC) in 1.5 h is demonstrated. The process is based on the automated conversion of 5.7 g of MC per batch using an electrical pulse width modulation system to conduct the bottom-up upcycle of MC into flash graphene. This study then compare this method to two other scalable graphene synthesis techniques by both a life cycle assessment and a technoeconomic assessment.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2026

Pulse control of superconducting cavity-based qudits with a Fock-state basis

Fock-basis-encoding qudits allow quantum gates to operate on multiple qudit levels simultaneously. This capability is advantageous for applications involving complex local gate operations, such as the digital quantum simulation of non-Abelian gauge theories. However, compiling unitary operations to native qudit gates remains a challenging task, often requiring substantial computational resources. In this work, we theoretically investigate the direct pulse control of a superconducting radio-frequency cavity coupled to an ancilla transmon for gate synthesis. We will discuss the improvements and limitations applicable to high Fock states. This work paves the way toward more efficient and robust qudit-gate synthesis.

Li, Andy C.Y. [Fermilab] (ORCID:0000000345423739)↗

DOE OSTI2026

Pulse control of superconducting cavity-based qudits with a Fock-state basis

Li, Andy C.Y. [Fermilab] (ORCID:0000000345423739)↗

NASA NTRS1989

Synthesis and degradation of nitrate reductase during the cell cycle of Chlorella sorokiniana

Studies on the diurnal variations of nitrate reductase (NR) activity during the life cycle of synchronized Chlorella sorokiniana cells grown with a 7:5 light-dark cycle showed that the NADH:NR activity, as well as the NR partial activities NADH:cytochrome c reductase and reduced methyl viologen:NR, closely paralleled the appearance and disappearance of NR protein as shown by sodium dodecyl sulfate gel electrophoresis and immunoblots. Results of pulse-labeling experiments with [35S]methionine further confirmed that diurnal variations of the enzyme activities can be entirely accounted for by the concomitant synthesis and degradation of the NR protein.

Non-NASA Center↗

NASA NTRS1986

A simple method for designing or analyzing an optical communication link

A simple method is described for determining the performance of a free space optical communication link. The method can be used either in the system design (synthesis) mode or in the performance evaluation (analysis) mode. Although restricted to photo counting based detection of pulse position modulated signals, the method is still sufficiently general to accommodate space-based, as well as ground-based, reception.

Lesh, J. R.↗

DOE OSTI2023

Search for High-Pressure Silicon Phases: Reaching the Extreme Conditions with High-Intensity Laser Irradiation

Controlling electronic and optical properties of semiconducting materials could substantially expand their functionality and enable new pathways for the formation of ‘smart’ materials for emerging innovative applications. An emerging new path for the synthesis of exotic silicon (Si) polymorphs is irradiation of bulk diamond-cubic Si by ultrashort laser pulses at relativistic intensity above 1019 W/cm2. Exotic polymorphs are formed due to interaction with MeV-energy electrons generated in laser-produced high-temperature plasma state. The unusual Si structures are found in the form of 5–10 nm nanoparticles confined deep in the bulk of 500-μm-thick Si samples. Raman spectroscopy, electron microscopy and X-ray diffraction studies provide an unequivocal evidence of exotic Si phase formation. A key advantage of such relativistic irradiation lies thereby in the fact that large quantities of such exotic Si is synthesised embedded within the bulk diamond-cubic Si and that further the formed Si polymorphs are stable at ambient temperature and pressure. They are thus available for further studies for electronic applications in selective band gap engineering.

Rapp, Ludovic↗

DOE OSTI2026

Self-driving thin film laboratory: autonomous epitaxial atomic-layer synthesis via real-time computer vision analysis of electron diffraction

Emerging materials science platforms with the ability to make autonomous decisions on the fly are fundamentally changing the outlook and protocols for materials optimization and discovery. Because AI-driven self-navigating schemes can effectively reduce the total number of iterations needed to arrive at the "answer" (i.e. the best stochiometric composition for a desired physical property, optimum materials processing parameters, etc.) by significant margins, they have the potential to revolutionize materials and chemical manufacturing processes at large in research laboratory settings as well as in industrial plants. Here, we demonstrate a successful implementation of real-time closed-loop autonomous navigation of a multi-dimensional materials synthesis parameter space for fabricating phase-pure epitaxial films of a metastable phase of a functional oxide in a combinatorial pulsed laser deposition chamber. Sequential epitaxial growth iterations in search of the optimized recipe to stabilize the desired crystal phase were performed using frame-by-frame quantitative computer vision analysis of reflection high-energy electron diffraction (RHEED) images of the unit-cell level film being deposited. The autonomous scheme regularly resulted in > 30-fold reduction in the number of required experiments compared to a comprehensive mapping of the parameter space. The real-time workflow developed here can be readily extended to a variety of thin film synthesis platforms opening the door for self-driving atomic-level materials design as well as autonomous optimization of semiconductor manufacturing.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Revealing core-valence interactions in solution with femtosecond X-ray pump X-ray probe spectroscopy

Abstract Femtosecond pump-probe spectroscopy using ultrafast optical and infrared pulses has become an essential tool to discover and understand complex electronic and structural dynamics in solvated molecular, biological, and material systems. Here we report the experimental realization of an ultrafast two-color X-ray pump X-ray probe transient absorption experiment performed in solution. A 10 fs X-ray pump pulse creates a localized excitation by removing a 1 s electron from an Fe atom in solvated ferro- and ferricyanide complexes. Following the ensuing Auger–Meitner cascade, the second X-ray pulse probes the Fe 1 s → 3 p transitions in resultant novel core-excited electronic states. Careful comparison of the experimental spectra with theory, extracts +2 eV shifts in transition energies per valence hole, providing insight into correlated interactions of valence 3 d with 3 p and deeper-lying electrons. Such information is essential for accurate modeling and predictive synthesis of transition metal complexes relevant for applications ranging from catalysis to information storage technology. This study demonstrates the experimental realization of the scientific opportunities possible with the continued development of multicolor multi-pulse X-ray spectroscopy to study electronic correlations in complex condensed phase systems.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

NASA NTRS1986

Simple method for designing or analyzing an optical communication link

A simple method is described for determining the performance of a free space optical communication link. The method can be used either in the system design (synthesis) mode, or in the performance evaluation (analysis) mode. Although restricted to photo counting based detection (e.g., photomultiplier tube or equivalent) of pulse position modulated signals, the method is still sufficiently general to accommodate space-based, as well as ground-based, reception.

Lesh, James R.↗