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DOE OSTI2024

Instrument Control Software for Spectrophotometers

SRNL has developed instrument control software for diode array spectrophotometers that can be used for real time monitoring of dynamic systems. This software has evolved through several iterations as instruments have been developed for use in processing facilities at Savannah River Site. There are several noteworthy features of the software. The wavelength calibration is checked and updated in real time against reference emission lines that are designed into the instrument light source. Nonlinearities and offsets associated with the intensity response of the instruments are characterized, and absorbance spectra are appropriately corrected. These actions are necessary for accurate calculation of an absorbance spectrum from the intensity responses of two individual diode array detectors. The corrections also result in the spectra obtained for a particular sample by two (or more) different diode array detector pairs being nearly identical. This property assures consistent measurements at multiple locations with different instruments. It also permits the use of a single analyte calibration across many instruments without modification and without loss of accuracy

47 OTHER INSTRUMENTATION↗

NASA NTRS2011

Online Visualization and Analysis of Global Half-Hourly Infrared Satellite Data

nfrared (IR) images (approximately 11-micron channel) recorded by satellite sensors have been widely used in weather forecasting, research, and classroom education since the Nimbus program. Unlike visible images, IR imagery can reveal cloud features without sunlight illumination; therefore, they can be used to monitor weather phenomena day and night. With geostationary satellites deployed around the globe, it is possible to monitor weather events 24/7 at a temporal resolution that polar-orbiting satellites cannot achieve at the present time. When IR data from multiple geostationary satellites are merged to form a single product--also known as a merged product--it allows for observing weather on a global scale. Its high temporal resolution (e.g., every half hour) also makes it an ideal ancillary dataset for supporting other satellite missions, such as the Tropical Rainfall Measuring Mission (TRMM), etc., by providing additional background information about weather system evolution.

Liu, Zhong↗

DOE OSTI2026

SULI Report - Development of a Molten Salt Circulation Loop for in-situ Spectroscopy

This project supports the development of real time optical monitoring capabilities for molten salt reactor (MSR) environments by designing, testing, and refining a molten salt circulation loop suitable for combined laser induced breakdown spectroscopy (LIBS) and ultraviolet visible (UV Vis) absorption measurements. Online spectroscopic monitoring is increasingly important for nuclear safeguards, corrosion tracking, and material accountancy, yet MSR process fluids present substantial challenges due to their chemical complexity and hazards such as high temperatures and radiation. To address these needs, this work focuses on Phase I, the development of a room temperature aqueous circulation loop that serves as a surrogate platform for evaluating flow behavior, optical access, and component performance prior to high temperature salt operation. Initial testing identified several practical issues—including leaks, obstructions, and two-phase flow through the absorption cell—that were systematically resolved through hardware replacement, flow path redesign, and venturi pressure optimization. Relocating the flow cell upstream of the primary venturi enabled periods of stable single-phase flow, demonstrating the feasibility of integrating optical diagnostics into a circulation system. The results of Phase I provide essential design insight for Phase II, which will incorporate furnace compatible materials and LiCl KCl eutectic salt. Completion of the molten salt system will deliver a reusable testbed for evaluating multimodal spectroscopic techniques, advancing nondestructive, real time monitoring tools for future MSR and nuclear fuel cycle applications.

98 - NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL↗

DOE OSTI2026

Anomaly Detection for Online Monitoring of Thermocouple Sensors in the Advanced Test Reactor

This study explores data-driven anomaly detection methods to analyze sensor fail- ures in the Advanced Gas Reactor (AGR) nuclear fuel irradiation experiments. Specifically, we examine failures of thermocouples (TCs), which are critical for mon- itoring and controlling in-reactor temperatures during operation. Failures were pri- marily observed during abrupt power transitions and manifested as sensor drop-outs, drifts, or unexplained behavior. We applied three time-series analysis techniques— rolling mean smoothing, matrix profile, and vector auto-regression (VAR)—to de- tect anomalies in TC data prior to failure events. The rolling mean method effec- tively highlighted deviations aligned with reported failures, while the matrix profile provided partial early warning but sometimes flagged normal fluctuations during power-down periods. VAR shows potential in capturing multivariate dependencies but requires further calibration. A rare case of TC drift was also documented, which did not result in failure, underscoring the challenge of building predictive models with sparse positive examples. Our findings demonstrate that traditional statistical tools can aid anomaly detection but have limited predictive power without richer training data. We propose future directions including synthetic data generation, real- time surrogate modeling, and multi-modal feature integration. This work provides a foundation for applying robust anomaly detection frameworks to mission-critical sensor systems in experimental settings.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2021

Welding of Haynes 282 to Steels to Enable Modular Rotors for Advanced Ultra Super-Critical Steam Turbines

Steam turbines for an Advanced Ultra Super Critical (AUSC) fossil fired power plant will operate at temperatures well above those of current commercial steam cycles with inlet temperatures more than 760 C , which is beyond the capabilities of alloy steels presently used for steam turbine applications and requires advanced materials. Large components such as steam turbine rotors may be made of nickel based super alloys such as Haynes 282 (H282). However, monolithic forgings of superalloys in the sizes required for large steam turbines rotors can be prohibitively expensive besides many technical challenges. To minimize cost and alleviate the related technical challenges, superalloy use needs to be limited to locations on the steam turbine rotor where strength and temperature requirements cannot be met by conventional steels. This is possible if nickel-based superalloys can be successfully welded to steels and the related technical challenges - machining parts made of dissimilar welded materials, non-destructive examination of such welds for flaw detection; and, material properties of such hybrid components – are sufficiently addressed. In this technology development project, we successfully welded H282 to plates up to ~ 75 mm (~ 3 inches) to a 3.5NiCrMoV steel of similar thickness. Advanced ultrasonic inspection technique called Phased Array Ultrasonic Testing (PAUT) was employed to examine the dissimilar H282-Steel welds, into which flat bottomed side drilled holes (SDH) of various diameters were introduced, to determine the minimum detectable feature sizes; it was shown that with PAUT SDH of dia. down to 0.5 mm could be detected in the base alloys and SDH with dia. down to 2.4 mm could be detected in the weld metal under multiple orientations successfully. An autonomous machining process monitoring system was developed and demonstrated whereby the forces acting on the cutting tool could be actively monitored as the cutting tool transitioned from H282 to Steel across the weld using which the machining parameters can be potentially altered without interruption to extend tool life. This project successfully achieved its objectives of - i. Developing a welding methodology and viable welding geometries, to successfully join H282 to steel 3.5CrMoNiV steel to enable manufacture of modular steam turbine rotors for AUSC applications (conditions of at least 760 °Celsius and 3,100 psia (pounds per square inch absolute pressure) and evaluate the material properties of the welded specimen. ii. Employ the advanced ultrasonic inspection technique to the dissimilar weld metal joint and determine the minimum detectable feature sizes. iii. Develop effective machining techniques to machine such hybrid structures with online tool force monitoring and effect machine state metrics for optimal results.

20 FOSSIL-FUELED POWER PLANTS↗

NASA NTRS2020

First-Order Runtime Verification using BDDs

Runtime Verification (RV) expedites the analyses of execution traces for detecting system errors and for statistical and quality analysis. Having started modestly, with checking temporal properties that are based on propositional (yes/no) values, the current practice of RV often involves properties that are parametrized by the data observed in the input trace. The specifications are based on various formalisms, such as automata, temporal logics, rule systems, and stream processing. Checking execution traces that are data intensive against a specification that imposes strong dependencies between the data, poses a nontrivial challenges; in particular if runtime verification has to be performed online, while many events that carry data appear within small time proximities. Towards achieving this goal, it was recently suggested to represent relations over the observed data values, based on BDDs, where data elements are enumerated and then converted into bit vectors. This representation provided a very simple and natural extension of an RV algorithm from propositional to first-order LTL, but more importantly, was shown to contribute to the memory compactness and to the speed, as was demonstrated using a corresponding implementation. We extend here the capabilities of BDD-based RV with the ability to express timing constraints, where the monitored events include (integer) clock values. We show how to efficiently operate on BDDs that represent both relations on (enumerations of) values and time dependencies, as required by the addition of the time constraints. We demonstrate our algorithm with an efficient implementation and provide experimental results.

Peled, Doron↗

NASA NTRS2018

Initial Approach to Collect Small Unmanned Aircraft System Off-Nominal Operational Situations Data

NASA is developing the Unmanned Aircraft System Traffic Management research platform to safely integrate small unmanned aircraft operations in large-scale at low-altitudes. As a part of this effort, small unmanned aircraft system off-nominal operational situations data collection process has been developed to take lessons learned and to reinforce operational compliance. In this paper, descriptions of variables used for digital data collection and an online report form for collection of observational data from the operators (contextual data) are provided. They are used to collect off-nominal data from the Unmanned Aircraft System Traffic Management National Campaign in 2017. The digital data show that 2 out of 118 campaign operations (1.7%) encountered loss of navigation. Since the campaign aircraft used Global Positioning System for navigation, it is likely that unobstructed view of the sky at the campaign locations contributed to this small number. Also, 4 out of 47 operations (8.5%) encountered loss of communications. A relatively short distance between ground control system and aircraft, ranging from 2300 feet to 4200 feet, likely contributed to this small number. There was no data to identify the loss of communications condition, aircraft received signal strength, for the remaining 71 operations suggesting that some operators may not be monitoring unmanned aircraft communications system performance or monitoring it with different parameters. For the contextual data, due to the low number of total reports during the campaign, no significant trends emerged. This is an initial attempt to collect contextual data from small unmanned aircraft operators about off-nominal situations, and changes will be made to the future data collection to improve the amount and quality of the information.

unmanned aviation systems traffic management (UTM)↗

NASA NTRS2018

Initial Approach to Collect Small Unmanned Aircraft System Off-Nominal Operational Situations Data

Jung, Jaewoo↗

DOE OSTI2023

Proactive Intrusion Detection and Mitigation System

SAND2023-05661O The proactive intrusion detection and mitigation system (PIDMS) provides grid-edge situational awareness for cybersecurity defense by capturing real-time distributed energy resource (DER) network traffic and performance data with a novel approach that improves the detection and prevention of cyber-physical attacks. The PIDMS addresses the grid-edge security gap with real-time analysis of both network traffic and photovoltaic performance data to deliver a novel, cyber-physical intrusion detection system (IDS) approach that increases the accuracy and effectiveness of detection and mitigation. This hybrid IDS analysis enables dual monitoring that increases the workload of the adversary; both cyber and physical data would have to be simultaneously spoofed to evade detection. Furthermore, monitoring and analyzing cyber data are insufficient in some cases. For example, in an insider threat aimed at disrupting inverter grid-support functions where proper credentials and authentication are achieved, only the altered PV performance would indicate abnormal behavior. All in all, the PIDMS provides novel capabilities for: • Distributed, real-time cyber-physical detection and mitigation analysis • Cybersecurity defense for grid-edge systems • Analysis framework that can provide situational awareness across the transmission, distribution, and DER systems The PIDMS sensor is designed to collect cyber-physical data, process the data using machine-learning algorithms, detect abnormal events, and deploy mitigations. With these goals, the main functional PIDMS objectives are: • Capability to collect cyber-physical data • Onboard storage of cyber-physical data • Peer-to-peer communication • Computationally efficient machine-learning algorithms • Online cyber-physical data analysis • Alerting/visualization capabilities • Mitigation deployment capability with bump-in-the-wire (BITW) implementation Each of these functional objectives enable PIDMS to perform effective cyber-physical intrusion detection and mitigation. Sandia National Laboratories is a multimission laboratory managed and operated by National Technology & Engineering Solutions of Sandia, LLC, a wholly owned subsidiary of Honeywell International Inc., for the U.S. Department of Energy’s National Nuclear Security Administration under contract DE-NA0003525.

Jones, Christian↗

DOE OSTI2023

Robust Real-Time Modeling of Distribution Systems with Data-Driven Grid-Wise Observability (Final Technical Report)

The overall objective of this project is to leverage existing and emerging sensor measurements to develop data-driven observability enhancement algorithms as well as robust state estimation and parameter identification techniques to enable real-time grid-wise monitoring and modeling of loads and distributed energy resources (DERs). The project resulted in a holistic framework with the following key components: 1) data-driven and machine learning-based grid-edge visibility enhancement, 2) robust branch-current-based state estimation (BCSE), and 3) robust real-time steady-state and dynamic-state modeling of loads and DERs. The research outcomes have provided utility companies better network visibility, higher-fidelity load/DER models, and more accurate assessment of DERs’ impacts, thus, facilitating the integration of renewable energy sources. The synergistic collaborative project among Iowa State University (ISU), Argonne National Laboratory (ANL), Electric Power Research Center (EPRC), SIEMENS Industry, Alliant Energy, Cedar Falls Utilities (CFU), and Maquoketa Valley Electric Cooperative (MVEC) to leverage the team’s extensive expertise and experience in power distribution systems, state estimation, online modeling and identification, and DER integrations. The proposed frameworks have been verified with industry adopted software and attempted integrated with existing tool wherever possible

24 POWER TRANSMISSION AND DISTRIBUTION↗

NASA NTRS2018

Identification of Safety Metrics for Airport Surface Operations

A large fraction of safety incidents occurs on the ground during airport surface operations. Although these incidents are mostly non-fatal with a few exceptions, they are high profile incidents that remain a source of concern for the National Transportation Safety Board (NTSB), the Federal Aviation Administration (FAA), major airlines, and other stakeholders of the National Airspace System (NAS). These incidents have historically been mitigated by implementing changes to regulations, policies, and procedures over time. This approach has minimized but not eliminated the risk of occurrence of safety incidents. It is thus important to develop integrated techniques to assess, model, and prevent these incidents by analyzing the risk and likelihood of occurrence and communicating results of the analysis to decision-making personnel who can mitigate and prevent incidents in real time. The work presented in this paper builds on a previously developed architecture for safety, Real-Time Safety Monitoring (RTSM), to enable monitoring and prediction of the safety of the NAS. In the RTSM framework, hazards to flight are translated to safety metrics such as wake vortex encounters or loss of separation, that can be modeled and analyzed offline and also predicted and monitored in real time (online). The intent of this paper is to integrate predictable incidents that occur during surface and ground operations into the safety portfolio of the RTSM project by (i) identifying suitable information sources from which ground incidents can be studied, (ii) developing safety metrics correlated with surface operations, and (iii) recommending suitable data sources that can be quantified and used for the computation of pertinent safety metrics.

safety↗

DOE OSTI2024

First Phase Consensus Roadmap for Development of Condition-Based Cable Reliability Assurance

The objective of this work was to develop a first phase consensus roadmap for condition-based qualification (CBQ) of electrical cables. With CBQ, qualification of Class 1E electrical cables moves from a time-based approach to a condition-based approach, which is anticipated to be safer in terms of reliability and conservatism, and more cost effective in the long run. However, due to barriers, the CBQ approach has not yet been adopted by U.S. nuclear power plants (NPPs). Based upon a review of current work evaluating CBQ, the limitation of available condition monitoring technology seems to be the largest barrier. The importance of condition monitoring, or more specifically selecting appropriate condition indicators, during CBQ cannot be understated. However, selecting appropriate condition indicators is challenged by techniques that are destructive and only evaluate cable degradation locally. Further, arguably, no one identified condition indicator fully establishes cable condition. Thus, additional work is necessary to evaluate potential condition indicators towards CBQ. In addition to the requirements of IEC/IEEE Std. 60780-323, ideal condition indicators should include a) both destructive and non-destructive approaches, b) both local and global measurements, c) real-time (i.e., online) monitoring that trends with degradation, d) enable correlation with qualified levels of degradation, and e) be established within a repository of condition indicators with applicable materials and/or components and their acceptance criteria. Additional work is needed in development of technology and methodology prior to adoption of CBQ, especially for extending qualified life of installed components. Education and early experience by the industry and regulators will be required for this change in approach as an alternative to re-analysis. A series of workshops that bring together stakeholders to identify and address gaps will be needed. The longstanding cooperative working group of cable researchers from the U.S. Department of Energy, the Electric Power Research Institute, and the Nuclear Regulatory Commission forms a valuable starting point for development of a consensus roadmap to condition-based qualification approach as a viable options for qualification of cable systems in U.S. light water reactors.

42 ENGINEERING↗

NASA NTRS2018

Identification of Safety Metrics for Airport Surface Operations

A large fraction of safety incidents occurs on the ground during airport surface operations. Although these incidents are mostly non-fatal with a few exceptions, they are high profile incidents that remain a source of concern for the National Transportation Safety Board (NTSB), the Federal Aviation Administration (FAA), major airlines, and other stakeholders of the National Airspace System (NAS). These incidents have historically been mitigated by implementing changes to regulations, policies, and procedures over time. This approach has minimized but not eliminated the risk of occurrences. It is thus important to develop integrated techniques to assess, model, and prevent these incidents by analyzing the risk and likelihood of occurrence and communicating results of the analysis to decision-making personnel who can mitigate and prevent incidents in real time. The research presented in this report builds on prior work of researchers at the NASA Ames Research Center who developed an automated framework, Real-Time Safety Monitoring (RTSM), to enable monitoring and prediction of the safety of the NAS. In the RTSM framework, hazards to flight are translated to safety metrics such as wake vortex encounters or loss of separation, that can be modeled and analyzed offline and also predicted and monitored in real time (online). The intent of this report is to integrate predictable incidents that occur during surface and ground operations into the safety portfolio of the RTSM project by (i) identifying suitable information sources from which ground incidents can be studied, (ii) developing safety metrics correlated with surface operations, and (iii) recommending suitable data sources that can be quantified and used for the computation of pertinent safety metrics.

ground operations↗

NASA NTRS2012

NASA Tech Briefs, October 2012

Topics discussed include: Detection of Chemical Precursors of Explosives; Detecting Methane From Leaking Pipelines and as Greenhouse Gas in the Atmosphere; Onboard Sensor Data Qualification in Human-Rated Launch Vehicles; Rugged, Portable, Real-Time Optical Gaseous Analyzer for Hydrogen Fluoride; A Probabilistic Mass Estimation Algorithm for a Novel 7-Channel Capacitive Sample Verification Sensor; Low-Power Architecture for an Optical Life Gas Analyzer; Online Cable Tester and Rerouter; A Three-Frequency Feed for Millimeter-Wave Radiometry; Capacitance Probe Resonator for Multichannel Electrometer; Inverted Three-Junction Tandem Thermophotovoltaic Modules; Fabrication of Single Crystal MgO Capsules; Inflatable Hangar for Assembly of Large Structures in Space; Mars Aqueous Processing System; Hybrid Filter Membrane; Design for the Structure and the Mechanics of Moballs; Pressure Dome for High-Pressure Electrolyzer; Cascading Tesla Oscillating Flow Diode for Stirling Engine Gas Bearings; Compact, Low-Force, Low-Noise Linear Actuator; Ultra-Compact Motor Controller; Extreme Ionizing-Radiation-Resistant Bacterium; Wideband Single-Crystal Transducer for Bone Characterization; Fluorescence-Activated Cell Sorting of Live Versus Dead Bacterial Cells and Spores; Nonhazardous Urine Pretreatment Method; Laser-Ranging Transponders for Science Investigations of the Moon and Mars; Ka-Band Waveguide Three-Way Serial Combiner for MMIC Amplifiers; Structural Health Monitoring with Fiber Bragg Grating and Piezo Arrays; Low-Gain Circularly Polarized Antenna with Torus-Shaped Pattern; Stereo and IMU- Assisted Visual Odometry for Small Robots; Global Swath and Gridded Data Tiling; GOES-R: Satellite Insight; Aquarius iPhone Application; Monitoring of International Space Station Telemetry Using Shewhart Control Charts; Theory of a Traveling Wave Feed for a Planar Slot Array Antenna; Time Manager Software for a Flight Processor; Simulation of Oxygen Disintegration and Mixing With Hydrogen or Helium at Supercritical Pressure; A Superfluid Pulse Tube Refrigerator Without Moving Parts for Sub-Kelvin Cooling; Sapphire Viewports for a Venus Probe; The Mobile Chamber; Electric Propulsion Induced Secondary Mass Spectroscopy; and Radiation-Tolerant DC-DC Converters.

Source record↗

NASA NTRS2004

Vibration-Based Data Used to Detect Cracks in Rotating Disks

Rotor health monitoring and online damage detection are increasingly gaining the interest of aircraft engine manufacturers. This is primarily due to the fact that there is a necessity for improved safety during operation as well as a need for lower maintenance costs. Applied techniques for the damage detection and health monitoring of rotors are essential for engine safety, reliability, and life prediction. Recently, the United States set the ambitious goal of reducing the fatal accident rate for commercial aviation by 80 percent within 10 years. In turn, NASA, in collaboration with the Federal Aviation Administration, other Federal agencies, universities, and the airline and aircraft industries, responded by developing the Aviation Safety Program. This program provides research and technology products needed to help the aerospace industry achieve their aviation safety goal. The Nondestructive Evaluation (NDE) Group of the Optical Instrumentation Technology Branch at the NASA Glenn Research Center is currently developing propulsion-system-specific technologies to detect damage prior to catastrophe under the propulsion health management task. Currently, the NDE group is assessing the feasibility of utilizing real-time vibration data to detect cracks in turbine disks. The data are obtained from radial blade-tip clearance and shaft-clearance measurements made using capacitive or eddy-current probes. The concept is based on the fact that disk cracks distort the strain field within the component. This, in turn, causes a small deformation in the disk's geometry as well as a possible change in the system's center of mass. The geometric change and the center of mass shift can be indirectly characterized by monitoring the amplitude and phase of the first harmonic (i.e., the 1 component) of the vibration data. Spin pit experiments and full-scale engine tests have been conducted while monitoring for crack growth with this detection methodology. Even so, published data are extremely limited, and the basic foundation of the methodology has not been fully studied. The NDE group is working on developing this foundation on the basis of theoretical modeling as well as experimental data by using the newly constructed subscale spin system shown in the preceding photograph. This, in turn, involved designing an optimal sub-scale disk that was meant to represent a full-scale turbine disk; conducting finite element analyses of undamaged and damaged disks to define the disk's deformation and the resulting shift in center of mass; and creating a rotordynamic model of the complete disk and shaft assembly to confirm operation beyond the first critical concerning the subscale experimental setup. The finite element analysis data, defining the center of mass shift due to disk damage, are shown. As an example, the change in the center of mass for a disk spinning at 8000 rpm with a 0.963-in. notch was 1.3 x 10(exp -4) in. The actual vibration response of an undamaged disk as well as the theoretical response of a cracked disk is shown. Experiments with cracked disks are continuing, and new approaches for analyzing the captured vibration data are being developed to better detect damage in a rotor. In addition, the subscale spin system is being used to test the durability and sensitivity of new NDE sensors that focus on detecting localized damage. This is designed to supplement the global response of the crack-detection methodology described here.

Gyekenyesi, Andrew L.↗

DOE OSTI2023

Effects of small marine energy deployments on oceanographic systems

The placement and operation of marine energy deployments in the ocean have the potential to change flow patterns, decrease wave heights, and/or remove energy from the oceanographic system. Changes in oceanographic systems resulting from harvesting marine energy, particularly tidal and wave energy, may be of concern. These changes include alterations in nearfield and farfield physical processes, as well as potential secondary environmental effects such as changes in sediment transport patterns, biological processes, or coastal erosion. Knowledge of changes in oceanographic systems associated with marine energy is primarily available from numerical modeling studies, informed by some laboratory tests and very few field measurements. A literature review was conducted using the Tethys knowledge base and other online sources, building on conclusions from the Ocean Energy Systems-Environmental State of the Science report. Potential changes in oceanographic systems that may be caused by marine energy differ between tidal and wave devices because of different extraction mechanisms and siting locations. Numerical models show that tidal extraction on the order of hundreds of megawatts or with significant channel blockage is required to create changes in oceanographic processes that exceed natural variability. Effects from wave energy extraction in arrays are localized and dependent on array spacing and proximity to the shore. Here the available evidence supports the conclusion that the risk of significant environmental effects from such changes could be retired (i.e., less investigation required for every project) for small deployments—those representative of the state of the industry in 2021. Determining changes in oceanographic systems to be low risk for small deployments can thereby streamline environmental consenting by reducing monitoring needs at this early stage in the industry.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2021

In-situ Photophysical Monitors and Corrective Algorithms for Photovoltaic Film Deposition and Rapid Thermal Processing in Scalable Roll-to-Roll Manufacturing

This project evaluated three photophysics-based approaches for in situ process monitoring of the scalable deposition of perovskite photovoltaic films. Based on stakeholder input and the results of laboratory trials and literature analysis, two techniques, angle resolved elastic light scattering (ARLS) and time-resolved photoluminescence (TRPL) were prototyped and demonstrated with a mixture of simulation, offline and online tests. Also, a hybrid gas flow and humidity control enclosure was constructed and demonstrated to stabilize the ambient conditions around the slot die deposition process and were demonstrated to meet the target humidity control in situ. Due in part to a delayed start and COVID-related lab restrictions and personnel changes, some of the milestones were not met. In spite of these challenges, however, both techniques were prototyped through several iterations and demonstrated significant promise for rapid in line perovskite characterization within the targeted characterization time windows and these techniques are under further development for use in DE-FOA000235:2357-1586. The TRPL system was fully mounted and demonstrated on the scaled slot die roll to roll and sheet coating systems at the Washington Clean Energy Testbeds (WCET). Motivated by significant internal and stakeholder interest, the successful prototyping achieved here, the ongoing need for in-situ characterization for the scale-up of perovskite manufacturing, and the benefits of in situ photophysical characterization for future funded process development research, we are continuing with the principle aims of the project to develop effect in situ photophysical probes for fast analysis of the optoelectronic and structural quality of sheet based and roll to roll process perovskites. TRPLS and ARLS probes proposed in the project are to be completed with external support from the Washington Research Foundation at the WCET. We are currently actively engaged in the acquisition of components and plan to complete and test the probes within three months. It is our intention that these probes will then be used in ongoing perovskite development with our research and commercialization partners including First Solar and other member of the US MAP consortium in future funded development work.

14 SOLAR ENERGY↗

DOE OSTI2024

Online Monitoring of Catalytic Processes by Fiber-Enhanced Raman Spectroscopy

An innovative solution for real-time monitoring of reactions within confined spaces, optimized for Raman spectroscopy applications, is presented. This approach involves the utilization of a hollow-core waveguide configured as a compact flow cell, serving both as a conduit for Raman excitation and scattering and seamlessly integrating into the effluent stream of a cracking catalytic reactor. The analytical technique, encompassing device and optical design, ensures robustness, compactness, and cost-effectiveness for implementation into process facilities. Notably, the modularity of the approach empowers customization for diverse gas monitoring needs, as it readily adapts to the specific requirements of various sensing scenarios. As a proof of concept, the efficacy of a spectroscopic approach is shown by monitoring two catalytic processes: CO 2 methanation (CO 2 + 4H 2 → CH 4 + 2H 2 O) and ammonia cracking (2NH 3 → N 2 + 3H 2 ). Leveraging chemometric data processing techniques, spectral signatures of the individual components involved in these reactions are effectively disentangled and the results are compared to mass spectrometry data. This robust methodology underscores the versatility and reliability of this monitoring system in complex chemical environments.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗