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All sources NASA NTRS DOE OSTI

DOE OSTI2024

AEcroscopy: A Software–Hardware Framework Empowering Microscopy Toward Automated and Autonomous Experimentation

Microscopy has been pivotal in improving the understanding of structure-function relationships at the nanoscale and is by now ubiquitous in most characterization labs. However, traditional microscopy operations are still limited largely by a human-centric click-and-go paradigm utilizing vendor-provided software, which limits the scope, utility, efficiency, effectiveness, and at times reproducibility of microscopy experiments. Here, in this work, a coupled software–hardware platform is developed that consists of a software package termed AEcroscopy (short for Automated Experiments in Microscopy), along with a field-programmable-gate-array device with LabView-built customized acquisition scripts, which overcome these limitations and provide the necessary abstractions toward full automation of microscopy platforms. The platform works across multiple vendor devices on scanning probe microscopes and electron microscopes. It enables customized scan trajectories, processing functions that can be triggered locally or remotely on processing servers, user-defined excitation waveforms, standardization of data models, and completely seamless operation through simple Python commands to enable a plethora of microscopy experiments to be performed in a reproducible, automated manner. This platform can be readily coupled with existing machine-learning libraries and simulations, to provide automated decision-making and active theory-experiment optimization to turn microscopes from characterization tools to instruments capable of autonomous model refinement and physics discovery.

47 OTHER INSTRUMENTATION↗

DOE OSTI2022

AtomAI framework for deep learning analysis of image and spectroscopy data in electron and scanning probe microscopy

Over the past several decades, electron and scanning probe microscopes have become critical components of condensed matter physics, materials science and chemistry research. At the same time, the infrastructure for establishing a connection between microscopy observations and materials behaviour over a broader parameter space is lacking. In this work, we introduce AtomAI, an open-source software package bridging instrument-specific Python libraries, deep learning and simulation tools into a single ecosystem. AtomAI allows direct applications of deep neural networks for atomic and mesoscopic image segmentation converting image and spectroscopy data into class-based local descriptors for downstream tasks such as statistical and graph analysis. For atomically resolved imaging data, the output is types and positions of atomic species, with an option for subsequent refinement. AtomAI further allows the implementation of a broad range of image and spectrum analysis functions, including invariant variational autoencoders for disentangling structural factors of variation and im2spec type of encoder–decoder models for mapping structure–property relationships. Finally, our framework allows seamless connection to the first principles modelling with a Python interface on the inferred atomic positions.

36 MATERIALS SCIENCE↗

DOE OSTI2015

SU-E-T-30: A Factor for Converting Dose to a Gold Nanoparticle Mixture to a Biologically-Relevant Dose

Purpose: Monte Carlo studies of gold nanoparticle (GNP) dose enhancement on macroscopic scales in radiotherapy have modeled GNPs in tissue as a homogeneous mixture of gold and tissue. Using an explicit model of GNPs randomly positioned in a small volume (1 µm{sup 3}) of tissue, this study aims to quantify the dose to the biologically relevant component of a goldtissue mixture, enabling a conversion from macroscopically-scored dose. Methods: Using the PENELOPE Monte Carlo code with the penEasy package, we modeled a 1 µm{sup 3} volume containing either a tissue-gold mixture or GNPs suspended in ICRU 4-component tissue at various gold concentrations (0, 5, 10, and 15 mg Au/g tissue) and GNP diameters (20, 30, 40, 50 nm). The volume was irradiated with monoenergetic photon and electron beams, ranging from 110 eV to 6 MeV. Interaction forcing was utilized to increase simulation efficiency. Energy deposition was scored in the tissue for each case and was converted to dose. For each scenario, we calculated a conversion factor, the ratio of dose-to-tissue to dose-to-mixture as a function of energy. Results: The conversion factor was plotted as a function of energy for both photons and electrons. For electrons, the conversion factor was relatively unaffected by any of the parameters, including energy, ranging between 0.98–1.02. For photons, the factor was very energy dependent, with a range of 0.49–1.02. The factor was lowest for 10–100 keV photons. The conversion factor generally decreased with increasing GNP concentration and increasing GNP size. Conclusion: With a large variation in the conversion factor with incident energy, dose deposition is dependent on the spectrum incident on a volume. By scoring the energy spectrum in a given volume, one can provide a scenario-specific conversion factor, allowing fast, detailed Monte Carlo simulations without the need for explicit GNP-definition.

60 APPLIED LIFE SCIENCES↗

NASA NTRS2017

Milli-Watt Radioisotope Power to Enable Small, Long-Term Robotic “Probe” Space Exploration

Milli-watt Radioisotope Power Systems (RPS) based on Radioisotope Heater Units (RHUs) could be an ideal power source for certain spacecraft that cannot use solar power due to large distances from the sun, or other environmental constraints, and where they enable or significantly enhance the ability of a mission to meet its scientific or operational goals. Various modular, compact RHU-based thermoelectric (TE) generator concepts developed or derived from current NASA Small Business Innovation Research (SBIR) projects satisfying this need have been investigated. These modular, compact and low mass power systems could support small, highly-mobile robotic exploration packages, and could be incorporated into different robotic package concepts, spacecraft or satellites. Current modular RPS design concepts with 40mW, 80mW and 120mW power levels use RHUs and Bi2Te3 TE converters. Skutterudites materials could be used in the future if new higher thermal energy output and higher temperature miniature heat sources were developed, for example, using technologies currently in the General Purpose Heat Source (GPHS) used in higher electric power output RTGs. Small (a.k.a., “mice-like”) robotic packages could effectively utilize these RHU-driven power levels to accommodate crawling, climbing, monitoring, taking measurements, and communicating during long-term planetary missions aimed at gathering environmental and geologic data (i.e., over multiple decades). Waste heat from the cold side of the TE converter could also be directed toward the electronics and / or energy storage (e.g. batteries) to keep them within design temperature ranges. In addition to power generation and electronics / battery heating, the RHU / TE configuration could be designed to survive an external 500°C bake out procedure for critical spacecraft sterilization, environmental certification and planetary protection. Analytical studies have been performed to optimize various design configurations for power, mass, volume and robotic mobility. Specific power (mW/kg) and volumetric specific power (mW/cm3) characteristics of various design configurations will be presented and key conceptual design tradeoffs will be discussed. Hot- and cold-side thermal interfaces required to meet power and mass goals and associated design sensitivities will also be discussed. RHU / TE systems must overcome critical design challenges to survive high-g loadings in some robotic applications and we will examine the mass impacts required to satisfy various dynamic loading environments up to 10,000 g’s. Power can be generated for a minimum of 30 years or more using plutonium-238 dioxide heat sources (given that Pu-238 has an 87.7 year half-life) with some reduction in power as the heat source naturally degrades.

Bahrami, Poyan↗

DOE OSTI2021

The very high n Rydberg series of Ar 16+ in Alcator C-Mod tokamak plasmas

We report x-ray transitions of the very high-n Rydberg series in Ar 16+ have been observed from Alcator C-Mod tokamak plasmas. Individual emission lines up to 1s16p-1s 2 have been resolved and the central chord line brightnesses with principal quantum number n between 7 and 16 are generally found to decay as 1/n α , with α slightly larger than 3. In the plasma periphery, emission from 1s9p-1s 2 and 1s10p-1s 2 are found to be significantly enhanced relative to this decrease, indicative of selected population of these levels through charge exchange between background neutral deuterium in the ground state and Ar 17+ . An unresolved feature between the wavelengths of 1s27p-1s 2 and 1s30p-1s 2 is also present, which arises through charge exchange with neutral deuterium in the n* = 3 excited state. The brightnesses of transitions populated by charge exchange are spatially up/down asymmetric, with an excess on the side of the magnetic surface X-point. The relative brightness of the unresolved very high-n feature compared to 1s7p-1s 2 is found to increase with electron temperature and decrease with electron density. Simulations of line emission just on the long wavelength side of the Ar 16+ ionization limit indicate that the principal quantum number decay exponent is closer to α = 4 at very high n. The brightness dependence on n below 16 is in excellent agreement with calculations from the flexible atomic code package.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2023

PCB-on-DBC GaN Power Module Design with High-Density Integration and Double-Sided Cooling

Lateral gallium nitride (GaN) high-electron-mobility transistors (HEMTs) present better electrical characteristics compared to silicon or silicon carbide devices such as high switching speed and low gate charge, but also present additional challenges on the module design. Here, this paper discusses a high-density GaN power module with double-sided cooling, low inductance, on-package decoupling capacitors, and integrated gate drivers. The GaN dies as well as the gate drive are sandwiched between the printed circuit board (PCB) and direct bonded copper (DBC) substrate to achieve compact loop and double-sided cooling effect. Design considerations and thermal performance are analyzed. A module assembly procedure is presented utilizing the layer-by-layer attachment process. Finally, a 2.7 cm x 1.8 cm half-bridge GaN power module is fabricated and tested, achieving a low power-loop inductance of 1.03 nH, and the overshoot voltage of the switching waveform is less than 5% under a 400-V/25-A double-pulse test. The thermal resistance is 0.32 K/W, verified by simulation and experimental results. The design and assembly process can be generalized and applied to high power applications to achieve high power density and high performance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2016

Accurate design of megadalton-scale two-component icosahedral protein complexes

Nature provides many examples of self- and co-assembling protein-based molecular machines, including icosahedral protein cages that serve as scaffolds, enzymes, and compartments for essential biochemical reactions and icosahedral virus capsids, which encapsidate and protect viral genomes and mediate entry into host cells. Inspired by these natural materials, we report the computational design and experimental characterization of co-assembling, two-component, 120-subunit icosahedral protein nanostructures with molecular weights (1.8 to 2.8 megadaltons) and dimensions (24 to 40 nanometers in diameter) comparable to those of small viral capsids. Electron microscopy, small-angle x-ray scattering, and x-ray crystallography show that 10 designs spanning three distinct icosahedral architectures form materials closely matching the design models. In vitro assembly of icosahedral complexes from independently purified components occurs rapidly, at rates comparable to those of viral capsids, and enables controlled packaging of molecular cargo through charge complementarity. The ability to design megadalton-scale materials with atomic-level accuracy and controllable assembly opens the door to a new generation of genetically programmable protein-based molecular machines.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2016

Documentation of operational protocol for the use of MAMA software

Image analysis of Scanning Electron Microscope (SEM) micrographs is a complex process that can vary significantly between analysts. The factors causing the variation are numerous, and the purpose of Task 2b is to develop and test a set of protocols designed to minimize variation in image analysis between different analysts and laboratories, specifically using the MAMA software package, Version 2.1. The protocols were designed to be “minimally invasive”, so that expert SEM operators will not be overly constrained in the way they analyze particle samples. The protocols will be tested using a round-robin approach where results from expert SEM users at Los Alamos National Laboratory, Lawrence Livermore National Laboratory, Pacific Northwest National Laboratory, Savannah River National Laboratory, and the National Institute of Standards and Testing will be compared. The variation of the results will be used to quantify uncertainty in the particle image analysis process. The round-robin exercise will proceed with 3 levels of rigor, each with their own set of protocols, as described below in Tasks 2b.1, 2b.2, and 2b.3. The uncertainty will be developed using NIST standard reference material SRM 1984 “Thermal Spray Powder – Particle Size Distribution, Tungsten Carbide/Cobalt (Acicular)” [Reference 1]. Full details are available in the Certificate of Analysis, posted on the NIST website (http://www.nist.gov/srm/).

97 MATHEMATICS AND COMPUTING↗

DOE OSTI2022

Quantum Chemical Treatment of Strongly Correlated Magnetic Systems Based on Heavy Elements. Final Report

The objective of this project over the years has been to develop novel quantum chemical methods and employ them to study the chemistry of systems containing actinides, and transactinides. We have focused on their electronic and spectroscopic properties, their reactivity and utilization as single molecule magnets. We have developed wave-function based methods that are optimal to treat strongly correlated systems, namely systems with many electronic configurations that are all important and should be treated on an equal foot. Moreover, relativistic effects have to be included in the model, with special focus on spin-orbit coupling. We have derived our theories and developed our codes and made them available to the community as parts of open source packages. We have modelled systems in collaboration with experimentalists in the program, so that we could address some of the questions that are relevant to this community. We have also worked in collaboration with people at Lawrence Livermore National Laboratories on a project on super-heavy atoms. We hope that our theoretical predictions will inspire novel experiments. We have trained about 10 students/postdocs during this period, which are now faculty, researchers at national laboratories and in companies.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

The Very High n Rydberg Series of Ar^16+ in Alcator C-Mod Tokamak Plasmas

X-ray transitions of the very high-n Rydberg series in Ar^16+ have been observed from Alcator C-Mod tokamak plasmas. Individual emission lines up to 1s16p - 1s^2 have been resolved and the central chord line brightnesses with principal quantum number n between 7 and 16 are generally found to decay as 1/n^alpha, with alpha slightly larger than 3. In the plasma periphery, emission from 1s9p - 1s^2 and 1s10p - 1s^2 are found to be significantly enhanced relative to this decrease, indicative of selected population of these levels through charge exchange between background neutral deuterium in the ground state and Ar^17+. An unresolved feature between the wavelengths of 1s27p - 1s^2 and 1s30p - 1s^2 is also present, which arises through charge exchange with neutral deuterium in the n^* = 3 excited state. The brightnesses of transitions populated by charge exchange are spatially up/down asymmetric, with an excess on the side of the magnetic surface X-point. The relative brightness of the unresolved very high-n feature compared to 1s7p - 1s^2 is found to increase with electron temperature and decrease with electron density. Simulations of line emission just on the long wavelength side of the Ar^16$ ionization limit indicate that the principal quantum number decay exponent is closer to alpha = 4 at very high n. The brightness dependence on n below 16 is in excellent agreement with calculations from the Flexible Atomic Code package.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

NASA NTRS1987

Ram ion scattering caused by Space Shuttle v x B induced differential charging

Observations of secondary, high-inclination ions streams have been reported in the literature. The authors of these previous papers attributed the source of the secondary ions to a disturbed region in the plasma about 10 m from the Space Shuttle Orbiter. A new theory has been developed which shows how v x B induced differential charging on the plasma diagnostics package (PDP) can scatter the ram ion flux. Some of these ions are reflected back to the PDP and may be the sorce of the observed ion distributions. The effect is unique to large spacecraft; it occurs only when the magnitude of the induced v x B potentials are much larger than the electron thermal energy and of the order of the ion ram energy. That the ion streams observed at large angles must have been reflected from the PDP surface is demonstrated with three-dimensional sheath and particle trajectory calculations using the low earth orbit version of the NASA Charging Analyzer Program (NASCAP/LEO).

Katz, I.↗

NASA NTRS2002

Implementation of Adaptive Digital Controllers on Programmable Logic Devices

Much has been made of the capabilities of FPGA's (Field Programmable Gate Arrays) in the hardware implementation of fast digital signal processing. Such capability also makes an FPGA a suitable platform for the digital implementation of closed loop controllers. Other researchers have implemented a variety of closed-loop digital controllers on FPGA's. Some of these controllers include the widely used proportional-integral-derivative (PID) controller, state space controllers, neural network and fuzzy logic based controllers. There are myriad advantages to utilizing an FPGA for discrete-time control functions which include the capability for reconfiguration when SRAM-based FPGA's are employed, fast parallel implementation of multiple control loops and implementations that can meet space level radiation tolerance requirements in a compact form-factor. Generally, a software implementation on a DSP (Digital Signal Processor) or microcontroller is used to implement digital controllers. At Marshall Space Flight Center, the Control Electronics Group has been studying adaptive discrete-time control of motor driven actuator systems using digital signal processor (DSP) devices. While small form factor, commercial DSP devices are now available with event capture, data conversion, pulse width modulated (PWM) outputs and communication peripherals, these devices are not currently available in designs and packages which meet space level radiation requirements. In general, very few DSP devices are produced that are designed to meet any level of radiation tolerance or hardness. The goal of this effort is to create a fully digital, flight ready controller design that utilizes an FPGA for implementation of signal conditioning for control feedback signals, generation of commands to the controlled system, and hardware insertion of adaptive control algorithm approaches. An alternative is required for compact implementation of such functionality to withstand the harsh environment encountered on spacecraft. Radiation tolerant FPGA's are a feasible option for reaching this goal.

Gwaltney, David A.↗

DOE OSTI2022

Case studies in bias reduction and inference for electronic health record data with selection bias and phenotype misclassification

Electronic health records (EHR) are not designed for population‐based research, but they provide easy and quick access to longitudinal health information for a large number of individuals. Many statistical methods have been proposed to account for selection bias, missing data, phenotyping errors, or other problems that arise in EHR data analysis. However, addressing multiple sources of bias simultaneously is challenging. We developed a methodological framework (R package, SAMBA ) for jointly handling both selection bias and phenotype misclassification in the EHR setting that leverages external data sources. These methods assume factors related to selection and misclassification are fully observed, but these factors may be poorly understood and partially observed in practice. As a follow‐up to the methodological work, we demonstrate how to apply these methods for two real‐world case studies, and we evaluate their performance. In both examples, we use individual patient‐level data collected through the University of Michigan Health System and various external population‐based data sources. In case study (a), we explore the impact of these methods on estimated associations between gender and cancer diagnosis. In case study (b), we compare corrected associations between previously identified genetic loci and age‐related macular degeneration with gold standard external summary estimates. These case studies illustrate how to utilize diverse auxiliary information to achieve less biased inference in EHR‐based research.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2021

Leaf gas exchange and fitted parameters, San Lorenzo, Panama, 2020

This data package contains photosynthetic CO2 response curves (ACi curves), light response curves (AQ curves), dark adapted dark respiration, conductance curves, and survey measurements for leaves measured at the San Lorenzo forest canopy crane site, Panama (PA-SLZ) from January to March 2020. Leaves were sampled from both the top of the canopy and multiple heights within the canopy from 10 vertical profiles and included around 50 species. In addition, six core species were also measured, from the top of the canopy. Fitted maximum carboxylation rate (Vcmax), maximum electron transport rate (Jmax), and triose phosphate utilization rate (TPU) were derived from measured data as well as the convexity, light use efficiency, apparent quantum yield, and Rdark. The measurements can also be used to derive the conductance parameters g0 and g1 of stomatal model. All the gas exchange data and metadata are presented in .csv files and complete instrument output are included in .zip folders. Data and metadata meet the ESS-DIVE leaf-level gas exchange reporting format requirements. The protocol details are provided as pdf documents. In addition to gas exchange data described here these samples were also used for measurement of leaf optical properties, carbon and nitrogen content, and leaf mass per unit leaf area (LMA) these data can be cross linked using the unique sample ID and are provided in separate related data packages. Sample information including canopy elevation and leaf area index (LAI) can be found in the related “Leaf and canopy traits” data package.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2017

Metallic Nanocomposites as Next-Generation Thermal Interface Materials

Thermal interface materials (TIMs) are an integral and important part of thermal management in electronic devices. The electronic devices are becoming more compact and powerful. This increase in power processed or passing through the devices leads to higher heat fluxes and makes it a challenge to maintain temperatures at the optimal level during operation. Herein, we report a free standing nanocomposite TIM in which boron nitride nanosheets (BNNS) are uniformly dispersed in copper matrices via an organic linker, thiosemicarbazide. Integration of these metal-organic-inorganic nanocomposites was made possible by a novel electrodeposition technique where the functionalized BNNS (f-BNNS) experience the Brownian motion and reach the cathode through diffusion, while the nucleation and growth of the copper on the cathode occurs via the electrochemical reduction. Once the f-BNNS bearing carbonothioyl/thiol groups on the terminal edges come into the contact with copper crystals, the chemisorption reaction takes place. We performed thermal, mechanical, and structural characterization of these nanocomposites using scanning electron microcopy (SEM), diffusive laser flash (DLF) analysis, phase-sensitive transient thermoreflectence (PSTTR), and nanoindentation. The nanocomposites exhibited a thermal conductivity ranging from 211 W/mK to 277 W/mK at a filler mass loading of 0-12 wt.percent. The nanocomposites also have about 4 times lower hardness as compared to copper, with values ranging from 0.27 GPa to 0.41 GPa. The structural characterization studies showed that most of the BNNS are localized at grain boundaries - which enable efficient thermal transport while making the material soft. PSTTR measurements revealed that the synergistic combinations of these properties yielded contact resistances on the order of 0.10 to 0.13 mm2K/W, and the total thermal resistance of 0.38 to 0.56 mm2K/W at bondline thicknesses of 30-50 um. The coefficient of thermal expansion (CTE) of the nanocomposite is 11 ppm/K, which lies between the CTEs of aluminum (22 ppm/K) and silicon (3 ppm/K), which are common heat sink and heat source materials, respectively. The nanocomposite can also be deposited directly on to heat sink which will simplify the packaging processes by removing one possible element to assemble. These unique properties and ease of assembly makes the nanocomposite a promising next-generation TIM.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2017

Metallic Nanocomposites as Next-Generation Thermal Interface Materials: Preprint

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2018

Effect of Gamma Radiation on the Properties of Crosslinked Chitosan Nano-composite Film

Chitosan nano-composite film crosslinked by citric acid and with glycerol as plasticizer and MgO as antibacterial agent was prepared by casting method. MgO nanoparticles were synthesized via calcination method in furnace at 500 °C for 4 h and characterized by X-ray diffraction and transmission electron microscope. The chitosan nano-composite film with composition chitosan/citric/glycerol/magnesium oxide (1 wt%:1 wt%:75 vol%:10 wt%) has high mechanical properties than other films. The effects of different irradiation doses on the mechanical, thermal and antibacterial activity were investigated. The tensile strength enhanced by increasing irradiation dose up to 10 kGy and the elongation negligible changed as irradiation dose increased. The thermal stability slightly increased up to dose 2.5 kGy then decreased with dose increment. The antimicrobial activity film was studied against white mulberry-borne bacterial pathogens either Gram positive or Gram negative bacteria and has positive impact of gamma irradiation on the antimicrobial activity. The use of the selected chitosan nano-composite film which irradiated by dose of 2.5 kGy and has magnesium oxide of average particle size 54.3 nm as new packaging materials found to improve storage quality and shelf-life of mulberry fruit.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2018

Large Area Picosecond Photodetector (LAPPD TM ) - Pilot production and development status

Here, we discuss performance results achieved for fully functional sealed Large Area Picosecond Photodetectors (LAPPD (TM)) in tests performed at Incom Inc., as well as independent test results reported by our early adopters. The LAPPD is a microchannel plate (MCP) based large area picosecond photodetector, capable of imaging with single-photon sensitivity at high spatial and temporal resolutions in a hermetic package. The LAPPD has an active area of 350 square centimeters in an all-glass hermetic package with a fused silica window and bottom plate and sidewalls made of borosilicate float glass. Signals are generated by a bi-alkali Na 2 KSb photocathode and amplified with a stacked chevron pair of MCPs produced by applying resistive and emissive atomic layer deposition coatings to glass capillary array (GCA) substrates. Signals are collected on RF stripline anodes applied to the bottom plates which exit the detector via pin-free hermetic seals under the side walls. LAPPD test and performance results for product produced and delivered to early adopter customers during the first half of 2018 are reviewed. These results include electron gains ≥ 7.5 x 10 6 @ 850/950 V (entry/exit MCP), low dark noise rates (22 Cts/s/cm 2 ), single photoelectron (PE) timing resolution of 64 picoseconds RMS, and single photoelectron spatial resolution along and across strips of 2.8 mm and 1.3 mm RMS respectively. Many of these devices also had very high QE photocathodes that were uniform over the full 195 mm x 195 mm window active area (LAPPD #15 QE% @ 365 nm Max/Avg/Min = 25.8/22.3 ± 3/15.7). An update is additionally provided of developments that enable capacitive signal coupling from the detector to application specific pads or stripline readout patterns deployed on printed circuit boards positioned beneath the file, outside of the vacuum package. We conclude with examples of how sensors offering picosecond timing, in diverse applications can bring transformative change to detector technology and applications in future experiments.

47 OTHER INSTRUMENTATION↗