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All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Foundations of machine learning for low-temperature plasmas: methods and case studies

Abstract Machine learning (ML) and artificial intelligence have proven to be an invaluable tool in tackling a vast array of scientific, engineering, and societal problems. The main drivers behind the recent proliferation of ML in practically all aspects of science and technology can be attributed to: (a) improved data acquisition and inexpensive data storage; (b) exponential growth in computing power; and (c) availability of open-source software and resources that have made the use of state-of-the-art ML algorithms widely accessible. The impact of ML on the field of low-temperature plasmas (LTPs) could be particularly significant in the emerging applications that involve plasma treatment of complex interfaces in areas ranging from the manufacture of microelectronics and processing of quantum materials, to the LTP-driven electrification of the chemical industry, and to medicine and biotechnology. This is primarily due to the complex and poorly-understood nature of the plasma-surface interactions in these applications that pose unique challenges to the modeling, diagnostics, and predictive control of LTPs. As the use of ML is becoming more prevalent, it is increasingly paramount for the LTP community to be able to critically analyze and assess the concepts and techniques behind data-driven approaches. To this end, the goal of this paper is to provide a tutorial overview of some of the widely-used ML methods that can be useful, amongst others, for discovering and correlating patterns in the data that may be otherwise impractical to decipher by human intuition alone, for learning multivariable nonlinear data-driven prediction models that are capable of describing the complex behavior of plasma interacting with interfaces, and for guiding the design of experiments to explore the parameter space of plasma-assisted processes in a systematic and resource-efficient manner. We illustrate the utility of various supervised, unsupervised and active learning methods using LTP datasets consisting of commonly-available, information-rich measurements (e.g. optical emission spectra, current–voltage characteristics, scanning electron microscope images, infrared surface temperature measurements, Fourier transform infrared spectra). All the ML demonstrations presented in this paper are carried out using open-source software; the datasets and codes are made publicly available. The FAIR guiding principles for scientific data management and stewardship can accelerate the adoption and development of ML in the LTP community.

Physics↗
NASA NTRS1998

Tropospheric- Stratospheric Measurement Studies Summary

The two high altitude aircraft, ER-2 NASA #706 and 709 and the DC-8 NASA #717 are in active use in several programs of upper atmospheric research to study polar ozone changes, stratospheric-tropospheric exchange processes and atmospheric effects of aviation aircraft. The ER-2 has participated in seven major missions which mainly concentrated on vortex dynamics and the large losses of Ozone in the Polar regions (Ozone hole) observed in the spring. One mission verified the complex dynamical chemical and physical processes that occur during sunrise and sunset. Stratospheric Tracers of Atmospheric Transport (STRAT) obtained background measurements using the full ER-2 suite of instruments. Photochemistry of Ozone Loss in the Arctic Region in Summer (POLARIS) in 1997 assisted in understanding the mid-latitude and Arctic Ozone losses during the Northern Summer. The DC-8 with the Meteorological Measurement System (MMS) has participated in the Subsonic Aircraft: Cloud and Contrail Effects Special Study (SUCCESS), in 1996 and the Subsonic assessment Ozone and Nitrogen oxide experiment (SONEX) in 1997 missions. The MMS with its sophisticated software accurately measures ground speed and attitude, in-situ static and dynamic pressure total temperature, which are used to calculate the three dimensional wind fields, static pressure, temperature and turbulence values to meteorological accuracy. The meteorological data is not only of interest for its own sake in atmospheric dynamical processes such as mountain waves and flux measurements; but is also required by other ER-2 experiments that simultaneously measure water vapor, O3, aerosols, NO, HCl, CH4, N2O, ClO, BrO, CO2, NOy, HOx and temperature gradients. MMS products are extensively used to assist in the interpretation of their results in understanding the importance of convective effects relative to in-situ chemical changes, as may be noted by examining the list of references attached. The MMS consists of three subsystems: (a) aircraft instrumentation, inertial navigation system (INS), static and dynamic pressure taps, (b) additional dedicated instrumentation measuring angle of attack, yaw, total temperature, and a GPS which on the DC-8 measures position, velocity and attitude (c) an on board data, storage and computing acquisition system. This instrumentation and the associated software requires both an on-going laboratory ground calibration procedure for the total air temperature, static and total pressure inputs, verification of the INS dynamic response and also extensive air measurements and intercomparisons which ultimately verify and calibrate the complete system and its software. More than the usual accuracy is required because of the near cancellation occurring in the difference between the ground speed and true airspeed vectors used to give the wind vector. In the past year we have redesigned, recalibrated and used the MMS system on the NASA DC-8 that was previously used in the SUCCESS mission for the SONEX mission. Two papers were co-authored based on SUCCESS flights. Several reports and handouts were written for SONEX. Calibrations of the DC-8 pressure transducer temperature measuring thermistors was completed and an extensive analysis spanning several years of data files of the DC-8 Rosemount pressure transducer calibrations was done.

Browen, Stuart W.↗
NASA NTRS2010

Data Collected During the Post-Flight Survey of Micrometeoroid and Orbital Debris Impact Features on the Hubble Wide Field Planetary Camera 2

Over a period of five weeks during the summer of 2009, personnel from the NASA's Orbital Debris Program Office and Meteoroid Environment Office performed a post-flight examination of the Hubble Space Telescope (HST) Wide Field Planetary Camera 2 (WFPC-2) radiator. The objective was to record details about all micrometeoroid and orbital debris (MMOD) impact features with diameters of 300 micron and larger. The WFPC-2 was located in a clean room at NASA's Goddard Space Flight Center. Using a digital microscope, the team examined and recorded position, diameter, and depth information for each of 685 craters. Taking advantage of the digital microscope's data storage and analysis features, the actual measurements were extracted later from the recorded images, in an office environment at the Johnson Space Center. Measurements of the crater include depth and diameter. The depth was measured from the undisturbed paint surface to the deepest point within the crater. Where features penetrate into the metal, both the depth in metal and the paint thickness were measured. In anticipation of hypervelocity tests and simulations, several diameter measurements were taken: the spall area, the area of any bare metal, the area of any discolored ("burned") metal, and the lips of the central crater. In the largest craters, the diameter of the crater at the surface of the metal was also measured. The location of each crater was recorded at the time of inspection. This paper presents the methods and results of the crater measurement effort, including the size and spatial distributions of the impact features. This effort will be followed by taking the same measurements from hypervelocity impact targets simulating the WFPC-2 radiator. Both data sets, combined with hydrocode simulation, will help validate or improve the MMOD environment in low Earth orbit.

Opiela, J. N.↗
NASA NTRS2007

"Smart" Sensor Module

An assembly that contains a sensor, sensor-signal-conditioning circuitry, a sensor-readout analog-to-digital converter (ADC), data-storage circuitry, and a microprocessor that runs special-purpose software and communicates with one or more external computer(s) has been developed as a prototype of "smart" sensor modules for monitoring the integrity and functionality (the "health") of engineering systems. Although these modules are now being designed specifically for use on rocket-engine test stands, it is anticipated that they could also readily be designed to be incorporated into health-monitoring subsystems of such diverse engineering systems as spacecraft, aircraft, land vehicles, bridges, buildings, power plants, oilrigs, and defense installations. The figure is a simplified block diagram of the "smart" sensor module. The analog sensor readout signal is processed by the ADC, the digital output of which is fed to the microprocessor. By means of a standard RS-232 cable, the microprocessor is connected to a local personal computer (PC), from which software is downloaded into a randomaccess memory in the microprocessor. The local PC is also used to debug the software. Once the software is running, the local PC is disconnected and the module is controlled by, and all output data from the module are collected by, a remote PC via an Ethernet bus. Several smart sensor modules like this one could be connected to the same Ethernet bus and controlled by the single remote PC. The software running in the microprocessor includes driver programs for operation of the sensor, programs that implement self-assessment algorithms, programs that implement protocols for communication with the external computer( s), and programs that implement evolutionary methodologies to enable the module to improve its performance over time. The design of the module and of the health-monitoring system of which it is a part reflects the understanding that the main purpose of a health-monitoring system is to detect damage and, therefore, the health-monitoring system must be able to function effectively in the presence of damage and should be capable of distinguishing between damage to itself and damage to the system being monitored. A major benefit afforded by the self-assessment algorithms is that in the output of the module, the sensor data indicative of the health of the engineering system being monitored are coupled with a confidence factor that quantifies the degree of reliability of the data. Hence, the output includes information on the health of the sensor module itself in addition to information on the health of the engineering system being monitored.

Mahajan, Ajay↗
DOE OSTI2016

Vacancy structures and melting behavior in rock-salt GeSbTe

Ge-Sb-Te alloys have been widely used in optical/electrical memory storage. Because of the extremely fast crystalline-amorphous transition, they are also expected to play a vital role in next generation nonvolatile microelectronic memory devices. However, the distribution and structural properties of vacancies have been one of the key issues in determining the speed of melting (or amorphization), phase-stability, and heat-dissipation of rock-salt GeSbTe, which is crucial for its technological breakthrough in memory devices. Using spherical aberration-aberration corrected scanning transmission electron microscopy and atomic scale energy-dispersive X-ray mapping, we observe a new rock-salt structure with high-degree vacancy ordering (or layered-like ordering) at an elevated temperature, which is a result of phase transition from the rock-salt phase with randomly distributed vacancies. First-principles calculations reveal that the phase transition is an energetically favored process. Furthermore, molecular dynamics studies suggest that the melting of the cubic rock-salt phases is initiated at the vacancies, which propagate to nearby regions. The observation of multi-rock-salt phases suggests another route for multi-level data storage using GeSbTe.

36 MATERIALS SCIENCE↗
NASA NTRSDate not supplied

Overview of Additively Manufactured TPS Proposed Flight Test and Earth Re-Entry Capsule Design

A flight mechanics overview is presented of an Earth flight test designed to investigate a novel, 3D printed thermal protection system (TPS) that is currently in development at NASA as part of the Additive Manufacturing of Thermal Protection Systems project. The project is pioneering a method to print a thermal protection system onto an entry vehicle forebody one layer at a time. This method reduces labor and complexity as compared to traditional manufacturing methods while increasing mission-dependent customization of through-depth materials properties. The flight test has three objectives. First, subject the forebody stagnation point of a capsule equipped with additively manufactured TPS (AMTPS) material to peak heat fluxes in excess of 100 $W/cm^2$. Second, capture in-flight data to enable flight reconstruction and AMTPS material thermal response model improvement. Third, recover the capsule with data storage and forebody AMTPS intact to enable post-flight inspection and analysis of AMTPS performance. The flight test trajectory is designed to achieve a peak stagnation point, cold-wall, entry heat flux of 135~$W/cm^2$. Flight mechanics simulations are performed using the Program to Optimize Simulated Trajectories II (POST2) and Monte-Carlo analysis yields statistical percentiles on vehicle performance at key points along the trajectory. Based on the flight mechanics analysis presented in this paper, a prototype capsule was designed, partially fabricated, and underwent preliminary component stress testing in preparation for fabrication of the flight unit capsule. The capsule outer mold line is a modified version of the heritage Mars Microprobe geometry. The capsule has a 0.356~m diameter, a 30~kg mass, and a hypersonic ballistic coefficient of 300~$kg/m^2$. Sensor selection is guided by flight dynamics simulations with the goal of resolving the re-entry heating pulse. On-board instrumentation include forebody and aftbody pressure sensors and thermocouples, a 9-axis IMU, a GPS receiver, and an Iridium satellite modem, all of which collect and store data throughout flight via on-board avionics systems. A two-stage parachute system is designed to decelerate the capsule to touchdown velocities that will not result in significant fracture or deformation of the charred AMTPS material at ground impact.

Flight Mechanics↗
DOE OSTI2017

Development and use of a switchgrass ( Panicum virgatum L.) transformation pipeline by the BioEnergy Science Center to evaluate plants for reduced cell wall recalcitrance

Here, the mission of the BioEnergy Science Center (BESC) was to enable efficient lignocellulosic-based biofuel production. One BESC goal was to decrease poplar and switchgrass biomass recalcitrance to biofuel conversion while not affecting plant growth. A transformation pipeline (TP), to express transgenes or transgene fragments (constructs) in these feedstocks with the goal of understanding and decreasing recalcitrance, was considered essential for this goal. Centralized data storage for access by BESC members and later the public also was essential. A BESC committee was established to codify procedures to evaluate and accept genes into the TP. A laboratory information management system (LIMS) was organized to catalog constructs, plant lines and results from their analyses. One hundred twenty-eight constructs were accepted into the TP for expression in switchgrass in the first 5 years of BESC. Here we provide information on 53 of these constructs and the BESC TP process. Eleven of the constructs could not be cloned into an expression vector for transformation. Of the remaining constructs, 22 modified expression of the gene target. Transgenic lines representing some constructs displayed decreased recalcitrance in the field and publications describing these results are tabulated here. Transcript levels of target genes and detailed wall analyses from transgenic lines expressing six additional tabulated constructs aimed toward modifying expression of genes associated with wall structure (xyloglucan and lignin components) are provided. Altered expression of xyloglucan endotransglucosylase/hydrolases did not modify lignin content in transgenic plants. Simultaneous silencing of two hydroxycinnamoyl CoA:shikimate hydroxycinnamoyl transferases was necessary to decrease G and S lignin monomer and total lignin contents, but this reduced plant growth. A TP to produce plants with decreased recalcitrance and a LIMS for data compilation from these plants were created. While many genes accepted into the TP resulted in transgenic switchgrass without modified lignin or biomass content, a group of genes with potential to improve lignocellulosic biofuel yields was identified. Results from transgenic lines targeting xyloglucan and lignin structure provide examples of the types of information available on switchgrass lines produced within BESC. This report supplies useful information when developing coordinated, large-scale, multi-institutional reverse genetic pipelines to improve crop traits.

09 BIOMASS FUELS↗
DOE OSTI2024

Enhancing Cloud Cybersecurity: Prescriptive Controls for Operational Technology

This whitepaper provides strategic insights and recommendations into security cloud-based solutions for electric utilities, encompassing operational technology (OT), virtual power plants (VPP), distributed energy resources (DERs), applications, networks, and data storage as they transition to and leverage cloud infrastructure through managed service providers (MSPs) and cloud service providers (CSPs). Principles derived from established frameworks serve as a foundation for best practices across cybersecurity projects and remove the constraints of settling on a single framework. For organizations that prefer not to integrate a specific framework altogether, elements of the proposed approach could be adopted or tailored to best fit defined requirements and expected functionalities. The Cirrus assessment, a utility cloud feasibility tool, and the roadmap it provides serve as a precursor to this paper, which seeks to be a valuable resource for defining next steps following cloud technology integration feasibility appraisal. With its comprehensive approach to adoption, the Cirrus framework offers strategic guidance on responsibly preparing for or deploying a utility cloud solution. The previously published whitepaper, “Use Case-Informed Framework for Utility Cloud Migration,” details the guiding strategy, research, and deployment of cloud solutions within electric and interconnected grid systems. Before implementing the controls suggested in this document, it is recommended that stakeholders complete Cirrus's cloud integration assessment and pair the results with their unique cybersecurity controls to form a comprehensive cloud-based utility cybersecurity plan. The Cirrus outcome will consider a series of future architectures for the grid before and after the energy transition and evaluate the arguments for and against cloud applications for each electric and interconnected grid layer. This document is a companion to the original whitepaper, "Use Case-Informed Framework for Utility Cloud Migration" to further identify and recommend security controls based on Cirrus’s cloud integration assessment output. The following whitepaper outlines the cybersecurity controls that secure cloud-service models pertinent to the electric sector using the predefined categories identify, protect, detect, and respond and recover. The objective is to outline prescriptive security controls based on the type of architecture and data stored in the cloud. The focus includes dissecting the shared responsibility model and elucidating what on-premises Infrastructure as a Service (IaaS), Platform as a Service (PaaS), and Software as a Service (SaaS) entail. A pivotal consideration in this context is allocating responsibility for foundational cybersecurity aspects—having used Cirrus for the cloud integration assessment. The ensuing controls detailed herein also represent a checklist of controls necessary for a secure cloud transition, equipping utilities with the knowledge to navigate this digital transformation with confidence and strategic foresight in a safe and responsible manner.

42 ENGINEERING↗
DOE OSTI2016

Investigation of Natural Circulation Instability and Transients in Passively Safe Small Modular Reactors

The NEUP funded project, NEUP-3496, aims to experimentally investigate two-phase natural circulation flow instability that could occur in Small Modular Reactors (SMRs), especially for natural circulation SMRs. The objective has been achieved by systematically performing tests to study the general natural circulation instability characteristics and the natural circulation behavior under start-up or design basis accident conditions. Experimental data sets highlighting the effect of void reactivity feedback as well as the effect of power ramp-up rate and system pressure have been used to develop a comprehensive stability map. The safety analysis code, RELAP5, has been used to evaluate experimental results and models. Improvements to the constitutive relations for flashing have been made in order to develop a reliable analysis tool. This research has been focusing on two generic SMR designs, i.e. a small modular Simplified Boiling Water Reactor (SBWR) like design and a small integral Pressurized Water Reactor (PWR) like design. A BWR-type natural circulation test facility was firstly built based on the three-level scaling analysis of the Purdue Novel Modular Reactor (NMR) with an electric output of 50 MWe, namely NMR-50, which represents a BWR-type SMR with a significantly reduced reactor pressure vessel (RPV) height. The experimental facility was installed with various equipment to measure thermalhydraulic parameters such as pressure, temperature, mass flow rate and void fraction. Characterization tests were performed before the startup transient tests and quasi-steady tests to determine the loop flow resistance. The control system and data acquisition system were programmed with LabVIEW to realize the realtime control and data storage. The thermal-hydraulic and nuclear coupled startup transients were performed to investigate the flow instabilities at low pressure and low power conditions for NMR-50. Two different power ramps were chosen to study the effect of startup power density on the flow instability. The experimental startup transient results showed the existence of three different flow instability mechanisms, i.e., flashing instability, condensation induced flow instability, and density wave oscillations. In addition, the void-reactivity feedback did not have significant effects on the flow instability during the startup transients for NMR-50. ii Several initial startup procedures with different power ramp rates were experimentally investigated to eliminate the flow instabilities observed from the startup transients. Particularly, the very slow startup transient and pressurized startup transient tests were performed and compared. It was found that the very slow startup transients by applying very small power density can eliminate the flashing oscillations in the single-phase natural circulation and stabilize the flow oscillations in the phase of net vapor generation. The initially pressurized startup procedure was tested to eliminate the flashing instability during the startup transients as well. The pressurized startup procedure included the initial pressurization, heat-up, and venting process. The startup transient tests showed that the pressurized startup procedure could eliminate the flow instability during the transition from single-phase flow to two-phase flow at low pressure conditions. The experimental results indicated that both startup procedures were applicable to the initial startup of NMR. However, the pressurized startup procedures might be preferred due to short operating hours required. In order to have a deeper understanding of natural circulation flow instability, the quasi-steady tests were performed using the test facility installed with preheater and subcooler. The effect of system pressure, core inlet subcooling, core power density, inlet flow resistance coefficient, and void reactivity feedback were investigated in the quasi-steady state tests. The experimental stability boundaries were determined between unstable and stable flow conditions in the dimensionless stability plane of inlet subcooling number and Zuber number. To predict the stability boundary theoretically, linear stability analysis in the frequency domain was performed at four sections of the natural circulation test loop. The flashing phenomena in the chimney section was considered as an axially uniform heat source. And the dimensionless characteristic equation of the pressure drop perturbation was obtained by considering the void fraction effect and outlet flow resistance in the core section. The theoretical flashing boundary showed some discrepancies with previous experimental data from the quasi-steady state tests. In the future, thermal non-equilibrium was recommended to improve the accuracy of flashing instability boundary. As another part of the funded research, flow instabilities of a PWR-type SMR under low pressure and low power conditions were investigated experimentally as well. The NuScale reactor design was selected as the prototype for the PWR-type SMR. In order to experimentally study the natural circulation behavior of NuScale iii reactor during accidental scenarios, detailed scaling analyses are necessary to ensure that the scaled phenomena could be obtained in a laboratory test facility. The three-level scaling method is used as well to obtain the scaling ratios derived from various non-dimensional numbers. The design of the ideally scaled facility (ISF) was initially accomplished based on these scaling ratios. Then the engineering scaled facility (ESF) was designed and constructed based on the ISF by considering engineering limitations including laboratory space, pipe size, and pipe connections etc. PWR-type SMR experiments were performed in this well-scaled test facility to investigate the potential thermal hydraulic flow instability during the blowdown events, which might occur during the loss of coolant accident (LOCA) and loss of heat sink accident (LOHS) of the prototype PWR-type SMR. Two kinds of experiments, normal blowdown event and cold blowdown event, were experimentally investigated and compared with code predictions. The normal blowdown event was experimentally simulated since an initial condition where the pressure was lower than the designed pressure of the experiment facility, while the code prediction of blowdown started from the normal operation condition. Important thermal hydraulic parameters including reactor pressure vessel (RPV) pressure, containment pressure, local void fraction and temperature, pressure drop and natural circulation flow rate were measured and analyzed during the blowdown event. The pressure and water level transients are similar to the experimental results published by NuScale [51], which proves the capability of current loop in simulating the thermal hydraulic transient of real PWR-type SMR. During the 20000s blowdown experiment, water level in the core was always above the active fuel assemble during the experiment and proved the safety of natural circulation cooling and water recycling design of PWR-type SMR. Besides, pressure, temperature, and water level transient can be accurately predicted by RELAP5 code. However, the oscillations of natural circulation flow rate, water level and pressure drops were observed during the blowdown transients. This kind of flow oscillations are related to the water level and the location upper plenum, which is a path for coolant flow from chimney to steam generator and down comer. In order to investigate the transients start from the opening of ADS valve in both experimental and numerical way, the cold blow-down experiment is conducted. For the cold blowdown event, different from setting both reactor iv pressure vessel (RPV) and containment at high temperature and pressure, only RPV was heated close to the highest designed pressure and then open the ADS valve, same process was predicted using RELAP5 code. By doing cold blowdown experiment, the entire transients from the opening of ADS can be investigated by code and benchmarked with experimental data. Similar flow instability observed in the cold blowdown experiment. The comparison between code prediction and experiment data showed that the RELAP5 code can successfully predict the pressure void fraction and temperature transient during the cold blowdown event with limited error, but numerical instability exists in predicting natural circulation flow rate. Besides, the code is lack of capability in predicting the water level related flow instability observed in experiments.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗
DOE OSTI2020

Acceleration of Crystallization Kinetics in Ge‐Sb‐Te‐Based Phase‐Change Materials by Substitution of Ge by Sn

Abstract Thin films of (Ge 1– x Sn x ) 8 Sb 2 Te 11 are prepared to study the impact of Sn‐substitution on properties relevant for application in phase‐change memory, a next‐generation electronic data storage technology. It is expected that substitution decreases the crystallization temperature, but it is not known how the maximum crystallization rate is affected. Ge 8 Sb 2 Te 11 is chosen from the (GeTe) y (Sb 2 Te 3 ) 1– y system of phase‐change materials as a starting point due to its higher crystallization temperature as compared to the common material Ge 2 Sb 2 Te 5 . In situ X‐ray diffraction at 5 K min −1 heating rate is performed to determine the crystallization temperature and the resulting structure. To measure the maximum crystallization rate, femtosecond optical pulses that heat the material repetitively and monitor the resulting increase of optical reflectance are used. Glasses over the entire composition range are prepared using a melt‐quenching process. While at x = 0, 97, subsequent pulses are required for crystallization, one single pulse is enough to achieve the same effect at x = 0.5. The samples are further characterized by optical ellipsometry and calorimetry. The combined electrical and optical contrast and the ability to cycle between states with single femtosecond pulses renders Ge 4 Sn 4 Sb 2 Te 11 promising for photonics applications.

Zalden, Peter↗
DOE OSTI2020

Giant Domain Wall Conductivity in Self‐Assembled BiFeO 3 Nanocrystals

Abstract Ever‐increasing demand on electronic devices with ultrahigh‐density non‐volatile data storage has attracted great interest in novel ferroelectric memories based on conductive ferroelectric domain walls. Embedded in an insulating material, ferroelectric domain walls have the capability of being (re)created, displaced, erased, and altered in their spatial configurations and electronic characteristics. However, the domain wall conductivities are in most cases not yet sufficiently high to ensure the current density required to drive read‐out circuits operating at high speeds. In this work, a giant domain wall current (>10 µA) of a single charged domain wall is obtained through conductive atomic force microscopy with a bias field of 4 V. This is achieved in self‐assembled BiFeO 3 nanocrystals grown by sol‐gel method on Nb‐doped SrTiO 3 substrates. Local configurations of domains and domain wall types are studied using vector piezoresponse force microscopy and high‐resolution transmission electronic microscopy. The enhancement of the wall current is shown to be due to the formation of conducting pathways of charged defects accumulated along domain walls and traversing the nanocrystals. The diverse domain walls can be manipulated by electric field in a perpendicular architecture. The perpendicular array structure of BiFeO 3 nanocrystals should have great potentials for developing perpendicular nanoelectronic prototypes.

Liu, Lisha↗
DOE OSTI2025

In Situ Study of Resistive Switching in a Nitride‐Based Memristive Device

Abstract Resistive switching (RS) devices with ultra‐low‐voltage threshold and reliable switching repeatability exhibits great potential applications in energy‐efficient data storage and neuromorphic computing. Understanding switching mechanisms at nanoscale is critical to design RS devices with improved performance. In this work, a lamella memristive device using focused ion beam (FIB) method based on the metal/TiO x /TiN/Si structure device is fabricated. In situ transmission electron microscopy (TEM) and current–voltage ( I–V ) characteristic demonstrate that the lamella device shows a volatile RS behavior with a threshold switching at ≈ ± 0.4 V. In situ scanning transmission electron microscopy (STEM) experiments with electron energy loss spectroscopy (EELS) reveal that the charge carriers such as oxygen vacancies migrate under positive/negative DC bias and modulate Schottky barriers at the top and bottom metal/semiconductor interfaces. The RS mechanism of the lamella device is based on the Schottky barriers modulation and Joule heating assisted electric field triggered thermal runaway (FTTR) occurred at the metal/semiconductor interfaces. The fundamental insights gained from this study presents a perspective on interface‐type RS devices processing and opens up new technological opportunities of fabricating ultra‐low‐energy memristive devices.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Chemical Tuning Meets 2D Molecular Magnets

Two-dimensional (2D) magnets provoke a surge of interest in large anisotropy in reduced dimensions and are promising for next-generation information technology where dynamic magnetic tuning is essential. Until recently, the crucial metal-organic magnet Cr(pyz) 2 ∙xLiCl∙yTHF with considerable high coercivity and high-temperature magnetic order opens up a new platform to control magnetism in metal-organic materials at room temperature. Here we report an in-situ chemical tuning route to realize the controllable transformation of low-temperature magnetic order into room-temperature hard magnetism in Cr(pyz) 2 ∙xLiCl∙yTHF. The chemical tuning via electrochemical lithiation and solvation/desolvation exhibits continuously variable magnetic features from cryogenic magnetism to the room-temperature optimum performance of coercivity (H c ) of 8500 Oe and energy product of 0.6 MGOe. Such chemically flexible tunability of room-temperature magnetism is ascribed to the different degrees of lithiation and solvation that modify the stoichiometry and Cr-pyrazine coordination framework. Furthermore, the additively manufactured hybrid magnets show air stability and electromagnetic induction, providing potential applications. Our findings here suggest chemical tuning as a universal approach to control the anisotropy and magnetism of 2D hybrid magnets at room temperature, promising for data storage, magnetic refrigeration, and spintronics.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Sub‐Nanosecond Reconfiguration of Ferroelectric Domains in Bismuth Ferrite

Abstract Domain switching is crucial for achieving desired functions in ferroic materials that are used in various applications. Fast control of domains at sub‐nanosecond timescales remains a challenge despite its potential for high‐speed operation in random‐access memories, photonic, and nanoelectronic devices. Here, ultrafast laser excitation is shown to transiently melt and reconfigure ferroelectric stripe domains in multiferroic bismuth ferrite on a timescale faster than 100 picoseconds. This dynamic behavior is visualized by picosecond‐ and nanometer‐resolved X‐ray diffraction and time‐resolved X‐ray diffuse scattering. The disordering of stripe domains is attributed to the screening of depolarization fields by photogenerated carriers resulting in the formation of charged domain walls, as supported by phase‐field simulations. Furthermore, the recovery of disordered domains exhibits subdiffusive growth on nanosecond timescales, with a non‐equilibrium domain velocity reaching up to 10 m s −1 . These findings present a new approach to image and manipulate ferroelectric domains on sub‐nanosecond timescales, which can be further extended into other complex photoferroic systems to modulate their electronic, optical, and magnetic properties beyond gigahertz frequencies. This approach could pave the way for high‐speed ferroelectric data storage and computing, and, more broadly, defines new approaches for visualizing the non‐equilibrium dynamics of heterogeneous and disordered materials.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Artificial Intelligence Guided Studies of van der Waals Magnets

A materials informatics framework to explore a large number of candidate van der Waals (vdW) materials is developed. In particular, in this study a large space of monolayer transition metal halides is investigated by combining high-throughput density functional theory calculations and artificial intelligence (AI) to accelerate the discovery of stable materials and the prediction of their magnetic properties. Here, the formation energy is used as a proxy for chemical stability. Semi-supervised learning is harnessed to mitigate the challenges of sparsely labeled materials data in order to improve the performance of AI models. This approach creates avenues for the rapid discovery of chemically stable vdW magnets by leveraging the ability of AI to recognize patterns in data, to learn mathematical representations of materials from data and to predict materials properties. Using this approach, previously unexplored vdW magnetic materials with potential applications in data storage and spintronics are identified.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Revealing the Effects of Trace Oxygen Vacancies on Improper Ferroelectric Manganite with In Situ Biasing

Abstract Multiferroic materials, which exhibit multiple orderings, are promising for next generation data‐storage device applications. YMnO 3 , in particular, because of the coexistence of the ferroelectricity and (anti)ferromagnetism within one single material, has drawn special attentions to application‐based research. However, the role of defect chemistry related to the behaviors of the ferroelectric polarization has been seldomly studied due to its complexity. In this work, a novel switching behavior of multiferroic YMnO 3 single crystal is reported using in situ biasing and Landau based numerical calculation. It is revealed that the domain switching only happens at the topmost surface, which can be well explained by the electric field redistribution due to the trace amount of oxygen vacancies. These in situ observations demonstrate that defect chemistry plays an important role in domain switching and can be utilized as an additional parameter for controlling the distribution of electric field within the multiferroic materials.

Cheng, Shaobo↗
DOE OSTI2019

Unraveling Ferroelectric Polarization and Ionic Contributions to Electroresistance in Epitaxial Hf 0.5 Zr 0.5 O 2 Tunnel Junctions

Tunnel devices based on ferroelectric Hf 0.5 Zr 0.5 O 2 (HZO) barriers hold great promises for emerging data storage and computing technologies. The resistance state of the device can be changed through use of a suitable writing voltage. However, the microscopic mechanisms leading to the resistance change are an intricate interplay between ferroelectric polarization controlled barrier properties and defect-related transport mechanisms. Herein, the fundamental role of the microstructure of HZO films determining the balance between those contributions is demonstrated. The HZO film presents coherent or incoherent grain boundaries, associated to the coexistance of monoclinic and orthorhombic phases, which are dictated by the mismatch with the substrates for epitaxial growth. These grain boundaries are the toggle that allows to obtain either large (up to ≈450%) and fully reversible genuine polarization controlled electroresistance when only the orthorhombic phase is present or an irreversible and extremely large (≈10 3 –10 5 %) electroresistance when both phases coexist.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Reduced Stochastic Resistive Switching in Organic-Inorganic Hybrid Memristors by Vapor-Phase Infiltration

We report resistive random-access memory (RRAM) is promising for next-generation data storage and non-von Neumann computing hardware. However, tuning device switching characteristics and particularly, controlling their stochastic variation remain as critical challenges. Here, new organic-inorganic hybrid RRAM media are reported whose bipolar switching characteristics and stochasticity can be controlled by vapor-phase infiltration (VPI), an ex situ hybridization technique derived from atomic layer deposition. Hybrid RRAMs based on AlO x -infiltrated SU-8 feature facile tunability of device switching voltages, off-state current, and on-off ratio by adjusting the amount of infiltrated AlO x in the hybrid. Furthermore, a significant reduction in the stochastic, cycle-to-cycle variations of switching parameters is enabled by AlO x infiltration, driven by the infiltration-induced changes in mechanical, dielectric, and chemical properties of organic medium and their influence on the dimension and formation characteristics of conductive filaments. Finally, multi-level analog switching potentially useful for neuromorphic applications are demonstrated, along with direct, one-step device patterning exploiting the negative-tone resist feature of SU-8. With the demonstrated control over switching characteristics and stochastic variation, combined with analog switching and one-step patterning capabilities, the results not only present a novel hybrid medium for RRAM applications but also showcase the utility of VPI for developing new, high-performance hybrid RRAM devices.

77 NANOSCIENCE AND NANOTECHNOLOGY↗