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DOE OSTI2020

Versailles Project on Advanced Materials and Standards interlaboratory study on intensity calibration for x-ray photoelectron spectroscopy instruments using low-density polyethylene

We report the results of a Versailles Project on Advanced Materials and Standards interlaboratory study on the intensity scale calibration of x-ray photoelectron spectrometers using low-density polyethylene (LDPE) as an alternative material to gold, silver, and copper. An improved set of LDPE reference spectra, corrected for different instrument geometries using a quartz-monochromated Al Kα x-ray source, was developed using data provided by participants in this study. Using these new reference spectra, a transmission function was calculated for each dataset that participants provided. When compared to a similar calibration procedure using the NPL reference spectra for gold, the LDPE intensity calibration method achieves an absolute offset of ~3.0% and a systematic deviation of ±6.5% on average across all participants. For spectra recorded at high pass energies (≥90 eV), values of absolute offset and systematic deviation are ~5.8% and ±5.7%, respectively, whereas for spectra collected at lower pass energies (<90 eV), values of absolute offset and systematic deviation are ~4.9% and ±8.8%, respectively; low pass energy spectra perform worse than the global average, in terms of systematic deviations, due to diminished count rates and signal-to-noise ratio. Differences in absolute offset are attributed to the surface roughness of the LDPE induced by sample preparation. We further assess the usability of LDPE as a secondary reference material and comment on its performance in the presence of issues such as variable dark noise, x-ray warm up times, inaccuracy at low count rates, and underlying spectrometer problems. In response to participant feedback and the results of the study, we provide an updated LDPE intensity calibration protocol to address the issues highlighted in the interlaboratory study. Finally, we also comment on the lack of implementation of a consistent and traceable intensity calibration method across the community of x-ray photoelectron spectroscopy (XPS) users and, therefore, propose a route to achieving this with the assistance of instrument manufacturers, metrology laboratories, and experts leading to an international standard for XPS intensity scale calibration.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Embedded sensors integrated into critical components for in situ health monitoring of steam turbines

Operational flexibility is desired in today’s coal-fired power plants to balance power grids by compensating for the variable electricity supply from renewable energy sources and distributed gensets. This demanding requirement accelerates materials degradation and makes in-situ health monitoring essential. Life monitoring of components and subsystems is thus seen as essential in assessing material and mechanical behavior to estimate system reliability, move to a conditionbased maintenance strategy and determine time to failure of the units in their actual operating conditions. Vibration monitoring can be exploited for blade tip timing to measure blade vibration amplitude and tip clearance to detect any deterioration taking place in the condition of steam turbine blades. A failure of a rotating blade can lead to severe turbine damage followed by extensive repairs and loss of power production. A blade vibration monitoring system can help early detection of abnormal blade vibration behavior. In conjunction with a health monitoring system, the vibration characteristics can be analyzed to support a pro-active maintenance and inspection schedule. While the feasibility of this inspection technique has been amply demonstrated, there is a need to install induction probes to magnetize the blade for signal output. Siemens, in partnership with Raytheon Technologies Research Corporation (RTRC), proposes a holistic approach to develop embedded sensors to utilize radio frequency for not only coupling to sensors, but as the sensing modality. The goal of this project is to “embed” the novel sensing approach by using either additively manufactured or extruded waveguides on rotating blades for recording, evaluation and monitoring of blade vibrations in Low Pressure turbines, with applications extending to aero engines

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2021

Characterization of CdZnTeSe Nuclear Detector Chemically Etched in Bromine Methanol

Semiconductor nuclear radiation detectors made from tertiary and quaternary compounds of cadmium telluride (CdTe) can operate at room temperature without cryogenic cooling. One of such materials that have become of great interest is cadmium zinc telluride selenide (CdZnTeSe). Compared to other CdTe-based materials, such as cadmium zinc telluride (CdZnTe), CdZnTeSe can be grown with much less Te inclusions and sub-grain boundary networks. Chemical etching is often used to smoothen wafer surfaces during detector fabrication. This paper presents the characterization of CdZnTeSe that is chemically etched using bromine methanol solution. Infrared imaging shows that the wafer has no sub-grain boundary networks that often limit detector performance. The current-voltage (I-V) characterization experiment gave a resistivity of 4.6 × 10 10 Ω-cm for the sample. The I-V curve was linear in the ±10 to ±50 volts range. An energy resolution of 7.2% was recorded at 100 V for the 59.6-keV gamma line of 241 Am.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2024

Specifications of Cladding Diameter Measurements Conducted at AGHCF

Fuel element diameter data was collected on-site at the Alpha-Gamma Hot Cell Facility (AGHCF) before and after out-of-pile furnace transient tests of fuel elements. Available data records have been collected and preserved in the Out-of-Pile Transient Database (OPTD). This data is used to determine the transient-induced changes in fuel element diameter, or cladding strain, for the Whole Pin Furnace (WPF) tests. Fuel element diameter was measured by contact profilometry along the length of the fuel pin at specified rotational orientations and/or by a manually operated micrometer at several discrete axial locations along the pin. The Alpha-Gamma Hot Cell Facility Operations Manual details the way the facility operated, organizational and oversight responsibilities, and procedures for examination of samples. The working version of the manual at the time of the whole pin furnace tests and the test pin examinations is Doc. No. IPS-2-00-00, dated June 1989. This specification was developed using the operations manual and recovered measurement records in consultation with subject matter experts (SMEs). The measurement methods, format of the available post-test examination (PTE) data, and recommended methods for use and interpretation of that data are summarized. Section 2 describes the available diameter measurement data for the WPF tests with guidance for interpretation and usage, and Section 3 describes the instrument measurement procedures and calibration methods.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2020

Development and evaluation of a list mode neutron coincidence collar for spatial response measurements of fresh fuel assemblies

A traditional safeguards neutron coincidence counting system, the Neutron Coincidence Collar, has been modified to incorporate individual preamplifiers on each of its 18 3He tubes in active interrogation mode. When used with list mode data acquisition (LMDA) and analysis, a signal from each 3He tube can be recorded and analyzed to allow a spatial response measurement to be performed on an item based on count rate and 3He tube location within the system. The ultimate goal of this project is to demonstrate the capabilities of a list mode response matrix for the nondestructive assay of fresh nuclear fuel assemblies. To enable partial defect detection of fuel pin locations and absences within an assembly, the project aims to extend well-established correlated neutron analysis techniques on a preexisting Neutron Coincidence Collar by extracting a greater number of useful signatures from the system than are currently generated. LMDA, combined with the addition of multiple preamplifiers, facilitates this capability by increasing the number of simultaneous signals that can be measured; this allows an in-depth analysis of neutron coincidence events to determine a fissioning item’s location based on the measured doubles count rate in various channel logic coincidence combinations. All of this can be done from a single measurement pulse train in offline analysis, which is the major benefit provided by LMDA. Through various stages of development and testing, a Mirion Technologies model JCC-71 Neutron Coincidence Collar has been successfully retrofit with modern electronics designed in-house at Oak Ridge National Laboratory, matching preexisting JAB-01 electronics performance, while maintaining the original system footprint. This paper presents these various stages of development and experimental evaluation of the proof of concept system.

Moore, Angela S.↗

DOE OSTI2023

The Global DAS Month of February 2023

During February 2023, a total of 32 individual distributed acoustic sensing (DAS) systems acted jointly as a global seismic monitoring network. The aim of this Global DAS Month campaign was to coordinate a diverse network of organizations, instruments, and file formats to gain knowledge and move toward the next generation of earthquake monitoring networks. During this campaign, 156 earthquakes of magnitude 5 or larger were reported by the U.S. Geological Survey and contributors shared data for 60 min after each event’s origin time. Participating systems represent a variety of manufacturers, a range of recording parameters, and varying cable emplacement settings (e.g., shallow burial, borehole, subaqueous, and dark fiber). Monitored cable lengths vary between 152 and 120,129 m, with channel spacing between 1 and 49 m. The data has a total size of 6.8 TB, and are available for free download. Finally, organizing and executing the Global DAS Month has produced a unique dataset for further exploration and highlighted areas of further development for the seismological community to address.

58 GEOSCIENCES↗

DOE OSTI2026

Automation of Nanoparticle Synthesis Processes in a Plasma Environment Using LabVIEW

This work presents an automated control system for the synthesis of nanomaterials by plasma-enhanced chemical vapor deposition (PECVD), implemented using the LabVIEW software environment. The main objective of the study is to develop an integrated hardware-software platform that enables sequential control of the key stages of the PECVD process, including vacuum chamber preparation, pressure monitoring, working gas supply, plasma ignition, power matching, cyclic nanomaterial growth, and optical monitoring of nanoparticles in the plasma environment. The use of LabVIEW made it possible to integrate actuator control, experimental parameter acquisition, and realtime process visualization within a single automated system. The automated cycle begins with evacuation of the reaction chamber to a predefined base pressure. Transition to the next stage is permitted only after the specified pressure threshold has been reached, ensuring reproducible initial conditions for each experiment. The program then controls the supply of the working gas through mass flow controllers (MFCs). In this work, two gas-flow control modes were considered: analog control using a 0-5 V voltage signal and digital communication via RS-232 interface. It was shown that the analog approach requires accurate scaling of the control voltage, since applying 5 V corresponds to full-scale opening of the controller and results in the maximum gas flow. In contrast, the RS232 interface enables the gas flow rate to be specified directly in sccm, improving the accuracy, flexibility, and convenience of gas-environment control. After pressure stabilization, LabVIEW initiates RF plasma ignition and executes the RF matching algorithm aimed at minimizing reflected power and improving the stability of the plasma process. A separate software module implements the cyclic nanomaterial growth mode, in which the plasma-on time, plasma duration, and total number of synthesis cycles are predefined. This approach makes it possible to control material accumulation on the substrate and to correlate the process parameters with the morphological characteristics of the resulting nanostructures. The final module of the system is designed for optical monitoring of the nanoparticle cloud density in dusty plasma. For this purpose, the change in the intensity of laser radiation passing through the plasma region is recorded using a photodetector and a Keithley 2401 measuring unit connected to LabVIEW via RS-232 interface. The difference between the initial and modified optical signal intensity is used as a diagnostic parameter characterizing the formation and temporal evolution of nanoparticles. The developed system demonstrates that LabVIEW can be effectively applied not only for the automation of individual instruments, but also for the implementation of a complete digital control cycle for PECVD-based nanomaterial synthesis.

PECVD↗

DOE OSTI2022

Feasibility Study of Millimeter Wave Radars For Safeguards Applications

Containment and surveillance are fundamental measures in nuclear safeguards. Techniques such as video surveillance and laser curtain for containment provide effective monitoring in areas where maintaining continuity of knowledge is required. These systems, however, can be susceptible to loss of monitoring capabilities under certain environmental conditions such as poor visibility (i.e. low light conditions, smoke, fog, etc.) or extended power loss past the duration that the backup power system is designed for. Brookhaven National Laboratory has been investigating the feasibility of millimeter waves (mmWave) as a new perimeter seal in which radio frequency waves in the range of 60-64 GHz are used to detect and monitor objects of interest. Signals in this frequency range are not susceptible to environmental conditions. For proof-of-concept tests, mmWave sensors from Texas Instruments (TI), specificallyIWR6843, are used in a test bed at BNL's Waste Management facility to simulate the operations at nuclear facilities. The unique design of TI mmWave sensors requires less memory and power consumption compared to counterpart systems. These devices are capable of exporting 3D point-cloud data, which is visualized graphically and compared to videos recorded at the same time to validate the performance of the mmWave sensor. A set of experiments were planned to test the feasibility of the mmWave in this application, including monitoring static containers in a storage area and detecting intrusions at the boundaries of the area. In addition, the experiments also identify potential blind spots relative to sensor position and utilize multiple operating sensors simultaneously to reduce or eliminate such blind spots. The optimal positioning of multiple sensors was determined for the experimental room configuration. In this paper, we will discuss the details of this novel perimeter sealing concept and present the test results.

98 NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL P↗

DOE OSTI2023

A liquid metal dropper for experiments on the wettability of liquid metals on plasma facing components

A liquid metal dropper has been developed as a part of the Ion-Gas-Neutral Interactions with Surfaces 2 (IGNIS-2) facility at The Pennsylvania State University. The dropper has the capability of directly applying drops to candidate plasma facing materials for nuclear fusion reactors to enable measurements of their liquid metal wetting properties. The results presented here are specific to the use of lithium in the dropper. This paper discusses the design choices of the liquid metal dropper and its chamber, including the heating and temperature control and the dropper’s motorized operation. Lithium drops of masses ranging from 0.05 g up to 0.13 g, equivalent to drop diameters between 5.6 mm to 1 cm, have been consistently dispensed by the dropper. A new algorithm is developed and used to automate the analysis of the contact angle between the liquid drops and substrate material for efficient analysis of video data recorded to study the wetting properties of candidate plasma-facing components.

Instruments & Instrumentation↗

DOE OSTI2020

Comparison of DTRA/NACT Next Generation Digitizer Evaluations

Sandia National Laboratories has tested and evaluated three digitizers, the Affinity, manufactured by Guralp Systems, the Centaur, manufactured by Nanometrics, and the Q330M+, manufactured by Quanterra, a division of Kinemetrics. These digitizers are used to record sensor output for seismic and infrasound monitoring applications. The purpose of this document is to highlight various results and observations collected during comprehensive evaluations conducted on each unit.

42 ENGINEERING↗

DOE OSTI2025

Production of alternate realizations of DESI fiber assignment for unbiased clustering measurement in data and simulations

A critical requirement of spectroscopic large scale structure analyses is correcting for selection of which galaxies to observe from an isotropic target list. This selection is often limited by the hardware used to perform the survey which will impose angular constraints of simultaneously observable targets, requiring multiple passes to observe all of them. In SDSS this manifested solely as the collision of physical fibers and plugs placed in plates. In DESI, there is the additional constraint of the robotic positioner which controls each fiber being limited to a finite patrol radius. A number of approximate methods have previously been proposed to correct the galaxy clustering statistics for these effects, but these generally fail on small scales. To accurately correct the clustering we need to upweight pairs of galaxies based on the inverse probability that those pairs would be observed (Bianchi & Percival 2017). This paper details an implementation of that method to correct the Dark Energy Spectroscopic Instrument (DESI) survey for incompleteness. To calculate the required probabilities, we need a set of alternate realizations of DESI where we vary the relative priority of otherwise identical targets. These realizations take the form of alternate Merged Target Ledgers (AMTL), the files that link DESI observations and targets. We present the method used to generate these alternate realizations and how they are tracked forward in time using the real observational record and hardware status, propagating the survey as though the alternate orderings had been adopted. We detail the first applications of this method to the DESI One-Percent Survey (SV3) and the DESI year 1 data. We include evaluations of the pipeline outputs, estimation of survey completeness from this and other methods, and validation of the method using mock galaxy catalogs.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2020

AEROICESTUDY-Colorado State University Ice Spectrometer

The dataset comprises measures, using Colorado State University's Ice Spectrometer (IS, an immersion freezing device with a range from 0 °C down to -26 to -29 °C) of atmospheric ice nucleating particle (INP) concentrations taken at ARM's Southern Great Plains (SGP) Site Guest Instrument Facility (GIF), in Lamont, Oklahoma, during the Aerosol-Ice Formation Closure Pilot Study (AEROICESTUDY). A filter sampler was mounted approximately 6 m above ground level atop the GIF rooftop platform. Single-use filter units open to the atmosphere fitted with pre-cleaned and pre-sterilized, 47-mm diameter Nuclepore polycarbonate filters were used. Filters were typically drawn for either a full day period (9AM-5PM CDT) or broken up into morning (9AM-12PM CDT) and afternoon (1PM-5PM CDT) periods. Additionally, 4 overnight filters were taken (6PM-8AM CDT). The volume of air filtered was typically between 3000 and 8000 standard liters for daily samples. After collection, filters were stored at -20 °C until processed. Initial processing to obtain spectra of INP number concentration active via the immersion freezing mechanism versus temperature was conducted using CSU's IS instrument (McCluskey et al., 2018). For measurement of INPs, collected aerosol particles were re-suspended in 8 mL of 0.1 µm-filtered deionized (DI) water. Aliquots of each suspension, and serial dilutions, were dispensed into trays which were fit into aluminum blocks in the IS. Samples were cooled at 0.33 °C per min and the freezing temperatures of wells recorded automatically. Cumulative INP concentrations were determined by first calculating the INPs per mL of suspension based on Vali (1971) and then converting to concentration per standard liter of air using the proportion of the total liquid sample dispensed and the air sample volumes. Two-tailed, 95% confidence intervals for binomial sampling were based on Equation 2 from Agresti and Coull (1998). Aliquots of suspensions from selected samples were also heat treated (95 °C for 20 min) to denature and deactiv

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2024

Analysis of Temperature Effects on GS-13 Short Period Sensors Utilizing Sandia's Seismic Sensor Temperature Testbed

Sandia National Laboratories has fabricated a Seismic Sensor Temperature Testbed (SSTT) suitable for exposing sensors under test to a range of reasonably stable temperatures while a co-located reference sensor is maintained at room temperature. The testbed has proven sufficiently quiet to allow recording of high-coherence signals from regional earthquakes in the passband of the seismometers, allowing a direct comparison of signals between the sensors under test and the reference sensor.

47 OTHER INSTRUMENTATION↗

DOE OSTI2024

Subdecadal Holocene Warm-Season Temperature Variability in Central Europe Recorded by Biochemical Varves

Paleoclimate data provide important information about the character of natural climate variability. However, records with sufficient length and resolution to resolve high-frequency (decadal-scale) variability across the Holocene are scarce. We present a 10,800-year reconstruction of spring and summer temperature at three-year resolution based on biochemical varves from Lake $\dot{Z}abi$$\acute{n}skie$, Poland. The reconstruction is based on Ca/Ti ratio, which are significantly correlated with instrumental spring and summer temperature spanning 240 years. Major climate events of the Holocene period are represented in the reconstruction, including the Holocene Thermal Maximum, 8.2 ka Event, Medieval Climate Anomaly, and Little Ice Age. A low-frequency 8,000-year decreasing trend in warm-season temperatures is driven by declining summer insolation. Temperature variability is highest during the early Holocene, likely related to warmer and drier conditions. The rate of warming during the past 90 years is extremely unusual, if not unprecedented for the Holocene, based on our reconstruction.

58 GEOSCIENCES↗

DOE OSTI2022

Classification of Ultrasonic Weld Quality using Acoustic Signatures Acquired During Manufacture

Ultrasonic welding is a process is based on generating a solid-state bond between two metals by applying moderate pressure and high intensity sound waves (20-70 kHz frequencies) at their interface. During the solid-state process numerous material, surface, instrument, and environmental factors contribute to bond formation, strength, and durability. The inherent difficulty of measuring and controlling each of these factors has, to date, made predicting bond quality elusive. In this work, a Sonics model MWB20 ultrasonic spot welder with integral base, was used to produce a variety of welds of different metal foils under varying weld conditions. Acoustic measurements were recorded throughout the measurement process. Subsequent analysis of the signals using metrics that approximate the energy dispersed during the weld proved to successfully predict weld quality. Two metrics based on normalized energy differential and Renyi entropy were developed into Python and C++ scripts for direct analysis of weld acoustic data.

36 MATERIALS SCIENCE↗

DOE OSTI2021

CACTI ARM Mobile Facility (AMF) Measurements of Ice Nucleating Particles

The dataset comprises measures, using Colorado State University's Ice Spectrometer (IS, an immersion freezing device with a range from 0°C down to -26 to -29°C) of atmosperic ice nucleating particle (INP) concentrations taken on ARM's Mobile Facility (AMF-1) Aerosol Observing System, near Villa Yacanto in central Argentina, during the Cloud, Aerosol, and Complex Terrain Interactions (CACTI) Experiment. A filter sampler was mounted on the AOS trailer (2 m below the AOS inlet). Single-use filter units open to the atmosphere fitted with pre-cleaned and pre-sterilized, 47-mm dia. Nuclepore polycarbonate filters were used. Filters were typically drawn for an 8-hour period, totaling 6000 liters sampled on average. After collection, filters were stored at -20°C until processed. Initial processing to obtain spectra of INP number concentration active via the immersion freezing mechanism versus temperature was conducted using CSU's IS instrument (McCluskey et al., 2018). For measurment of INPs, collected aerosol particles were re-suspended in 7-8 mL of 0.1 µm-filtered deionized (DI) water. Aliquots of each suspension, and serial dilutions, were dispensed into trays which were fit into aluminum blocks in the IS. Samples are cooled at 0.33°C min-1 and the freezing temperatures of wells recorded automatically. Cumulative INP concentrations were determined by first calculating the INPs per mL of suspension based on Vali (1971) and then converting to concentration per standard liter of air using the proportion of the total liquid sample dispensed and the air sample volumes. An aliquot of suspension fro selected samples were also heat treated (95°C for 20 min) to denature and deactivate biological INPs, and another aliquot digested in 10% H2O2 at 95°C under UV-B to remove all organic carbon INPs. McCluskey, C. S., J. Ovadnevaite, M. Rinaldi, J. Atkinson, F. Belosi, D. Ceburnis, S. Marullo, T. C. J. Hill, U. Lohmann, Z. A. Kanji, C. O’Dowd, S. M. Kreidenweis, P. J. DeMott, 2018: Marine and Terrestrial Organic Ice Nucleating Particles in Pristine Marine to Continentally-Influenced Northeast Atlantic Air Masses, Journal of Geophysical Research: Atmospheres, 123, 6196–6212, https://doi.org/10.1029/2017JD028033. Vali, G., 1971: Quantitative evaluation of experimental results on the heterogeneous freezing nucleation of supercooled liquids. J. Atmos. Sci., 28, 402–409.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2024

Size resolved particle hygroscopcity for 30, 60, and 90 nm particles collected at the EPCAPE Mount Soledad site from 04/20/2023 to 06/15/2023

Contains both the growth factor probability density function (probability is out of 200) and the average growth factors calculated by the Gysel inversion. The instrument measured three different diameters 30 nm, 60nm and 90nm each diameter was selected for an hour. During that hour, five 12-minute scans were taken scanning growth factors from 0.5-3.0. RH was consistently kept at 85%. Calibrations of the instrument with NaCl were performed on 4/26/2023 from 11:20 to 14:20, on 5/16/2023 from 11:40 to 16:00, and on 5/30/2023 from 10:20 to 14:20. Calibrations with (NH4)2SO4 were performed on 5/8/2023 from 11:45 to 14:40, on 5/23/2023 from 11:20 to 3:00, and on 6/14/2023 from 13:00 to 16:00. Time is recorded in seconds since 1/1/1904.

30 nm particle hygroscopicity↗

DOE OSTI2020

Cloud Particle Imager (CPI) and 3-View Cloud Particle Imager (3V-CPI) Instrument Handbook

The cloud particle imager (CPI) is a U.S. Department of Energy (DOE) Atmospheric Radiation Measurement (ARM) user facility instrument for measuring the concentration and size of cloud droplet and ice crystals. Hydrometeors entering the tube will be detected by a system of two continuous wave lasers that are perpendicular to each other, monitoring the sample volume. When a hydrometeor obscures both laser beams it is inside the sample volume and a third laser is triggered to illuminate the hydrometeor and a camera records a two-dimensional image. The CPI records images with a resolution of 2.3 μm. Since the camera has 1024 x 1024 pixels, the maximum detectable size is 2.3 mm x 2.3 mm.

54 ENVIRONMENTAL SCIENCES↗