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At least 451 records · Page 25

Improved Understanding of Zircaloy Hydrogen Pickup Mechanisms in BWRs. NSUF Report (Final Report)

Using an instrumented autoclave operating at 288°C and 1100 psi, electrical impedance spectroscopy (EIS) measurements were taken from three neutron irradiated fuel channel samples (Zircaloy-2 and Zircaloy-4). The three high priority fuel channel samples were tested at 288°C using a simulated PWR water with the AC frequency range extending down through 10 -4 Hz, with corresponding DC measurements to validate the resistance measurements. EIS measurements were also taken at room temperature using a simulated PWR water from four neutron irradiated fuel channel samples (Zircaloy-2 and Zircaloy-4). and four water rod samples (Zircaloy-2). EIS measurements were also performed on unirradiated Zircaloy-2 tubes that were previously oxidized in autoclaves at various temperatures for different time durations to obtain oxide layers of different thicknesses. These experiments proved to be more challenging than anticipated because of the small size of the samples, which required development of fixtures to allow valid testing of the materials, some of which are radioactive, under pressure and temperature. Equivalent circuits were used to model the data. Some samples resulted in Nyquist plots where the arcs were too close to each other resulting in the inability to separate the different oxide morphological thicknesses. Microstructural characterization in the form of optical microscopy, scanning electron microscopy and (scanning) transmission electron microscopy was performed to document the microstructural features of the oxidized Zr-2 and Zr-4 samples (oxide and metal/oxide interface) and to interpret the EIS results. At the start of this work, it was assumed that despite the laminar cracks and porosity visible in both optical and SEM, the oxide scale is dense near the metal, effectively preventing the water from contacting the metal directly. While it is generally accepted that the large laminar cracks pores allow the water to percolate into the oxide film, it is unknown just how deep it can go, and how interconnected is the porosity, which will dictate how much the porosity is connected electrically to the water within the oxide scale. The EIS results demonstrated that there is in fact a distribution of oxide thicknesses over the various samples, and within each material condition, that are communicating to the liquid. This is derived from the fact that Nyquist plots have an arc radius whose center point is often below the Z’ axis, implying that instead of a single oxide thickness, these oxides have a distribution of thicknesses. This distribution of thicknesses produces arcs that are not clearly separable in most of the samples.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Ultra-High Efficiency and Stable All-Perovskite Tandem Solar Cells

In the project period, the research team has fabricated more than 6,000 single-junction wide-bandgap (wide-E g ) and low-bandgap (low-E g ) perovskite solar cells (PSCs) and more than 2,000 all-perovskite tandem solar cells (APTSCs). The best-performing wide-E g and low-E g PSCs and APTSCs showed PCEs greater than 19%, 23%, and 30%, respectively. The average PCEs for wide-E g and low-E g PSCs and APTSCs fabricated by the benchmark processes are (18.5 ± 0.4)%, (21.9 ± 0.8)%, and (26.8 ± 2.1)%, respectively. We have demonstrated APTSCs with T 80 lifetime of more than 1,000 h, which were measured by maximum power point tracking (MPPT) under one sun operation in the air. The team has also utilized various advanced characterization techniques to study the optical and electrical properties of wide-E g and low-E g perovskite materials and devices, developing a better understanding of the unique working principle and degradation mechanism of APTSCs. The team has met most GNG decision criteria except for the stability goal of APTSCs under 85 °C/85 RH accelerated lifetime test (ALT). The shortfall of the device ALT stability is mainly limited by the intrinsic instability of Sn-Pb perovskites under illumination at elevated temperatures. The team discussed with stakeholders in the PV academic and industry about these durability concerns and concluded that this is the major technical barrier preventing the market entry of APTSCs. Future fundamental study and R&D work are needed to advance this promising technology.

14 SOLAR ENERGY↗

Aluminophosphate Waste Forms for Immobilizing Cations from Electrochemical Salt Wastes

This report provides experimental details and results of evaluating aluminophosphate waste forms for treating and immobilizing the salt cations from salt wastes generated during electrochemical reprocessing of used nuclear fuel. In the waste form process for these materials, chloride salt streams are reacted with NH 4 H 2 PO 4 , the chlorine is removed from the salts and driven off as NH 4 Cl (a solid condensate that can be captured), and then the product can be vitrified in conjunction with glass-forming chemicals (e.g., Fe 2 O 3 , Al 2 O 3 ) to create a high-durability waste form. This study was initiated with some literature review on aluminophosphates containing high alkali oxide content and some of this information is summarized in this report. Following literature review, three new samples were synthesized where two contained Fe 2 O 3 +Al 2 O 3 (i.e., samples G3 and G5 ) and one was only Al 2 O 3 (Fe 2 O 3 -free) (i.e., sample G6 ). In addition to these samples, G1 was also made, which is the baseline reference waste form referred to as DPF5-336 (made without Al 2 O 3 ). Samples G1, G3, G5, and G6 had phases of Li 3 Fe 2 (PO 4 ) 3 (likely), monazite (below XRD detection limits), AlPO 4 , and AlPO 4 , respectively. Characterizations on these materials included optical images, scanning electron microscopy, energy dispersive X-ray spectroscopy, and X-ray diffraction. These samples were shipped to Argonne National Laboratory for chemical durability testing. Depending on how the samples perform in these tests, an additional phase of aluminophosphate formulations could be designed and tested. This report completes the milestone M4FT-23PN030104041 with details provided in Appendix B.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Noble Liquid Test Facility at Fermilab

The Noble Liquid Test Facility (NLTF) at Fermilab is a liquid argon detector R\&D facility open to the national and international HEP community. The facility consists of 4 permanent cryostats, ranging from 250L up to 3000L, open space for small open dewar testing, and an optical test stand facility capable of measuring the optical properties of materials and characterizing photon detectors. NLTF’s strongest advantage is its capability to provide ultra-pure LAr in a reliable manner. Its inline filters are capable of filtering all of the three biggest contaminants for standard LAr detectors, O$_2$ and H$_2$O down to $< 1$ppb and N$_2$ $< 1$ppm. This is critical for the users of the test stands as small levels of impurities can dramatically change the efficiency of LArTPCs for the collection of charge and light. The smallest cryostat is mainly used for material testing, a service provided to the international HEP community interested in understanding how the introduction of a specific material might affect the electron lifetime in LAr. The test stands can be equipped with a purity monitor, which allows measuring the electron lifetime in real time, as well as gas sampling and analyzing, and in the near future, local recirculation and filtering. The facility has hosted many successful R\&D projects, which have published their results in well-known journals and talks. A few examples of such projects are: NIR light production in LAr and GAr, the characterization of VUV metalenses, the testing of new filter media capable of filtering N$_2$ from LAr, high voltage studies and direct charge amplification in LAr, and various doping studies.

Blaszczyk, Flor María [Fermilab]↗

Cascade Dielectrophoretic Separation for Selective Enrichment of Polyhydroxybutyrate (PHB)-Producing Cyanobacterium Synechocystis sp. PCC 6803

Maintaining favorable biological productivities in photosynthetic biomanufacturing systems, especially when the risk of contamination with competing microbes is high, remains a challenge to achieve while maintaining economic feasibility. This study presents a dielectrophoresis (DEP)-based microfluidic approach for isolating a desired strain within a co-culture. The cyanobacterium Synechocystis sp. PCC 6803 (a strain capable of producing the bioplastic precursor polyhydroxybutyrate, or PHB) was enriched from mixed cultures containing the competing cyanobacterium Synechococcus elongatus PCC 7942 (which does not naturally produce PHB). A DEP cascade electrode system was established to increase purification efficiency through sequential enrichment, which leveraged inherent differences in cell morphology and dielectric properties, to achieve the selective separation of these strains under physiological conditions. A substantial increase in the relative abundance of PHB-producing cells was assessed by optical microscopy and flow cytometry characterization, confirming more than five-fold reduction of the Synechococcus fraction in the refined cell mix. The presented electrokinetic platform offers a scalable and effective approach for selectively enhancing desired microbial components within microbial biomanufacturing systems, leading towards improved product yields.

60 APPLIED LIFE SCIENCES↗

Best Practices for Measuring the Modulation Transfer Function of Video Endoscopes

Endoscopes are crucial for assisting in surgery and disease diagnosis, including the early detection of cancer. The effective use of endoscopes relies on their optical performance, which can be characterized with a series of metrics such as resolution, vital for revealing anatomical details. The modulation transfer function (MTF) is a key metric for evaluating endoscope resolution. However, the 2020 version of the ISO 8600-5 standard, while introducing an endoscope MTF measurement method, lacks empirical validation and excludes opto-electronic video endoscopes, the largest family of endoscopes. Measuring the MTF of video endoscopes requires tailored standards that address their unique characteristics. This paper aims to expand the scope of ISO 8600-5:2020 to include video endoscopes, by optimizing the MTF test method and addressing parameters affecting measurement accuracy. We studied the effects of intensity and uniformity of image luminance, chart modulation compensation, linearity of image digital values, auto gain control, image enhancement, image compression and the region of interest dimensions on images of slanted-edge test charts, and thus the MTF based on these images. By analyzing these effects, we provided recommendations for setting and controlling these factors to obtain accurate MTF curves. Our goal is to enhance the standard’s relevance and effectiveness for measuring the MTF of a broader range of endoscopic devices, with potential applications in the MTF measurement of other digital imaging devices.

47 OTHER INSTRUMENTATION↗

Diel cycle impacts on the chemical and light absorption properties of organic carbon aerosol from wildfires in the western United States

Abstract. Organic aerosol (OA) emissions from biomass burning have been the subject of intense research in recent years, involving a combination of field campaigns and laboratory studies. These efforts have aimed at improving our limited understanding of the diverse processes and pathways involved in the atmospheric processing and evolution of OA properties, culminating in their accurate parameterizations in climate and chemical transport models. To bring closure between laboratory and field studies, wildfire plumes in the western United States were sampled and characterized for their chemical and optical properties during the ground-based segment of the 2019 Fire Influence on Regional to Global Environments and Air Quality (FIREX-AQ) field campaign. Using a custom-developed multiwavelength integrated photoacoustic-nephelometer spectrometer in conjunction with a suite of instruments, including an oxidation flow reactor equipped to generate hydroxyl (OH⚫) or nitrate (NO3⚫) radicals to mimic daytime or nighttime oxidative aging processes, we investigated the effects of multiple equivalent hours of OH⚫ or NO3⚫ exposure on the chemical composition and mass absorption cross-sections (MAC(λ)) at 488 and 561 nm of OA emitted from wildfires in Arizona and Oregon. We found that OH⚫ exposure induced a slight initial increase in absorption corresponding to short timescales; however, at longer timescales, the wavelength-dependent MAC(λ) decreased by a factor of 0.72 ± 0.08, consistent with previous laboratory studies and reports of photobleaching. On the other hand, NO3⚫ exposure increased MAC(λ) by a factor of up to 1.69 ± 0.38. We also noted some sensitivity of aerosol aging to different fire conditions between Arizona and Oregon. The MAC(λ) enhancement following NO3⚫ exposure was found to correlate with an enhancement in CHO1N and CHOgt1N ion families measured by an Aerodyne aerosol mass spectrometer.

54 ENVIRONMENTAL SCIENCES↗

Characterization of Octuopole Elements for IOTA

The Integrable Optics Test Accelerator (IOTA) is a research storage ring constructed and operated at Fermilab to demonstrate the advantages of nonlinear integrable lattices. One of the nonlinear lattice configurations with one integral of motion is based on a string of short octupoles. The results of the individual magnets characterizations, which were necessary to determine their multipole composition and magnetic centers, are presented. This information was used to select and align the best subset of octupoles for the IOTA run 4.

43 PARTICLE ACCELERATORS↗

Determining the tilt of the Raman laser beam using an optical method for atom gravimeters

The tilt of a Raman laser beam is a major systematic error in precision gravity measurement using atom interferometry. The conventional approach to evaluating this tilt error involves modulating the direction of the Raman laser beam and conducting time-consuming gravity measurements to identify the error minimum. In this work, we demonstrate a method to expediently determine the tilt of the Raman laser beam by transforming the tilt angle measurement into characterization of parallelism, which integrates the optical method of aligning the laser direction, commonly used in freely falling corner-cube gravimeters, into an atom gravimeter. A position-sensing detector (PSD) is utilized to quantitatively characterize the parallelism between the test beam and the reference beam, thus measuring the tilt precisely and rapidly. After carefully positioning the PSD and calibrating the relationship between the distance measured by the PSD and the tilt angle measured by the tiltmeter, we achieved a statistical uncertainty of less than 30 µrad in the tilt measurement. Furthermore, we compared the results obtained through this optical method with those from the conventional tilt modulation method for gravity measurement. The comparison validates that our optical method can achieve tilt determination with an accuracy level of better than 200 µrad, corresponding to a systematic error of 20 µGal in g measurement. This work has practical implications for real-world applications of atom gravimeters.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Characterization of the Hamamatsu 8-inch R14688-100 PMT

Large-scale optical neutrino and dark-matter detectors rely on large-area photomultiplier tubes (PMTs) for cost-effective light detection. The new R14688-100 8-inch PMT developed by Hamamatsu provides state-of-the-art timing resolution of around 1 ns (FWHM), which can help improve vertex reconstruction and enable Cherenkov and scintillation light separation in scintillation-based detectors. This PMT also provides excellent charge resolution, allowing for precision photoelectron counting and improved energy reconstruction. The Eos experiment is the first large-scale optical detector to utilize these PMTs. Here, in this manuscript, we present a characterization of the R14688-100 single photoelectron response, such as the transit-time spreads, the dark-rates, and the afterpulsing. The single photoelectron response measurements are performed for the 206 PMTs that will be used in Eos.

47 OTHER INSTRUMENTATION↗

A laserball calibration device for the SNO+ scintillator phase

Located 2 km underground in SNOLAB, Sudbury, Canada, SNO+ is a large scale liquid scintillator experiment that primarily aims to search for neutrinoless double beta decay. Whilst SNO+ has light and radioactive calibration sources external to the inner volume, an internally deployed optical source is necessary for the full characterization of the detector model. A laser diffuser ball developed for SNO has previously demonstrated to be an effective optical calibration device for both SNO and SNO+ water phase. Since the introduction of liquid scintillator for SNO+, the material compatibility, cleanliness, and radiopurity requirements of any materials in contact with the internal medium have increased. Improving on the original SNO laserball design, a new laserball calibration device has been developed for the SNO+ scintillator phase with the goal of measuring the optical properties of the detector and performing routine PMT gain and timing calibrations. Simulations have been written to model the diffusion properties to optimise optical and temporal performance for calibration. Prototype laserballs have been built and characterised, demonstrating sub-ns timing resolution and a quasi-isotropic light distribution.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

pH dependence of brown-carbon optical properties in cloud water

Abstract. Light-absorbing organic species present in aerosols, collectively called brown carbon (BrC), have important but highly uncertain effects on climate. Clouds likely represent a significant medium for secondary BrC production and for bleaching reactions, though the relative importance of the formation and loss processes in clouds is unknown at present. The acidity (or pH) of atmospheric particles and clouds affects the optical properties of BrC and bleaching rates. Given the wide variability of pH in the atmosphere (pH in particles and clouds ranges from −1 to 8), the optical properties of BrC and its bleaching behavior are expected to vary significantly, and the link between pH and BrC is yet another uncertainty in attempts to constrain its climate forcing effects. In this work, we characterize the pH dependence of BrC optical properties – including light absorption at 365 nm (Abs365), the mass absorption coefficient (MAC365), and the absorption Ångström exponent (AAE) – in bulk cloud water sampled from the summit of Whiteface Mountain, NY. In all samples (n=17), Abs365 and MAC365 increased linearly with increasing pH, highlighting the importance of reporting pH in studies of BrC in aqueous media. There was strong variability in the sensitivity of Abs365 to pH, with normalized slopes that ranged from 5.1 % to 17.2 % per pH unit. The normalized slope decreased strongly with increasing cloud water [K+], suggesting that the non-biomass-burning BrC has optical properties that are more sensitive to pH than BrC associated with biomass burning. AAE also showed a distinct pH dependence as it was relatively flat between pH 1.5–5 and then decreased significantly above pH 5. The cloud water composition was used to inform thermodynamic predictions of aerosol pH upwind and/or downwind of Whiteface Mountain and the subsequent changes in BrC optical properties. Overall, these results show that, in addition to secondary BrC production, photobleaching, and the altitudinal distribution, the climate forcing of BrC is quite strongly affected by its pH-dependent absorption.

54 ENVIRONMENTAL SCIENCES↗

Durable and Low-Cost Fractal Structured Multifunctional Coatings for Next-Generation CSP

Fractal coatings on various low-cost and high-temperature metallic substrates such as SS316, SS347, In800H, In740H, In625, Haynes 230, etc. were fabricated employing our patented novel electrodeposition process at various deposition potentials and deposition times, as well as chemical etching. The best combination of the materials and processing conditions were co-optimized for the reliable and repeatable fabrication of the multifunctional coatings. Surface morphologies were examined using SEM and AFM, and fractal characterization was done using a 3D optical surface profiler. Fractal dimension was used to identify successful fabrication and material parameters. The mechanical durability of the coatings was evaluated using several standardized tests, such as sand abrasion (ASTM D968) and adhesion (ASTM D3359), to fully characterize and demonstrate the mechanical durability of the fabricated surfaces. HTF immersion tests on the fractal multifunctional coatings were conducted based on a modification of the ASTM D870, which is established for static water immersion testing. To calculate the corrosion rates and descaled weight loss of the samples subjected to thermal exposure for different time durations (100 h, 300 h, 500 h, and optionally 750 h) to estimate the corrosion rate. While protecting the substrates from corrosion is an important goal, an allied goals is also to examine the post-corrosion temperature stability and properties of the molten salts themselves due to the dissolution of the constituents of the alloys and the corrosion products from the coatings that cause “fouling” of the molten salts. Fouling characteristics of the different molten salt HTFs exposed to coated and uncoated substrates were investigated. Finally, considering a prototype molten salt/sCO2 heat exchanger, cost/performance model is developed to demonstrate that the coatings on low-cost alloys such as stainless steel provide lower levelized cost of heat exchanger compared to high nickel content Ha230.

14 SOLAR ENERGY↗

Probing Nanocrystal Optical Properties in the Limit of Single Nanocrystals

The Bawendi lab has been at the forefront of the synthesis and characterization of the fundamental photo-physics of quantum confined systems for the past three decades. During this DoE project, our progress has been enabled by both our expertise in single nanocrystal (NC) photoluminescence (PL) spectroscopy as well as our extensive knowledge of the synthetic optimization of various NC semiconductors - all of this forming an efficient feedback loop between characterization and synthesis. Our research in this project has focused on the development and application of novel single emitter optical tools for the characterization of colloidal quantum dots (CQDs) which are semiconducting NCs with size-tunable quantum confined electronic structure. CQDs have had a significant commercial impact as display technologies. They are also commercially available as fluorescent biological markers. CQDs are being investigated as a potential material for photovoltaic or optical sensing applications and as emerging optical quantum materials. We have focused on the fundamental understanding of the optical properties of NCs through the development of novel spectroscopic methods at the single emitter level, including understanding how synthetic and environmental heterogeneities influence NC properties. A major advance in our research has been the development of novel photon resolved correlation spectroscopies that allow us to extract the physics of photo-excited single NCs with unprecedented time and spectral resolution from the photon stream of individual NCs.

36 MATERIALS SCIENCE↗

LLNL FY22 Aging and Lifetimes Exit Criteria (Milestone 8118, GC#5)

This report introduces a novel characterization tool that can rapidly collect in-situ time-dependent oxide thickness and hydride growth data together with spatial data using while-light interferometry. White-light interferometry is a non-destructive and non-contact optical surface profiling technique for materials characterization that offers excellent lateral and vertical resolution. A depleted uranium sample was used to assess the ability of white-light interferometry to provide quantitative corrosion reaction rates at metal surfaces for by hydriding and oxidation and compare this technique to existing characterization tools for capturing early-stage hydride and oxide growth kinetics.

36 MATERIALS SCIENCE↗

Jitter-induced Max-of-N fluence distribution at the National Ignition Facility

Max-of-N fluence is the maximum peak fluence at a given location over N number of shots and is important for calculating fluence dependence for intrinsic laser-induced optic damage. Previously, we observed the Max-of-N effect on the National Ignition Facility and developed an ad-hoc model to calculate its effect. In this work, we attempt to understand the fundamental mechanism that causes this Max-of-N effect. We conclude that the primary fundamental mechanism responsible for this effect is dominated by the combination of fluence variations and pointing jitter of the laser. This discovery both strengthens our model for predicting optics longevity and gives us insight into how to mitigate this effect.

42 ENGINEERING↗

Learnings from the Marcellus Shale Energy and Environmental Lab (MSEEL) Using Fiber Optic Tools and Geomechanical Modeling

The study focuses on the MIP and Boggess pads of the MSEEL (Marcellus Shale Energy and Environmental Laboratory), a public-private partnership with a mandate to publicly release data for scientists and engineers to engage with. Multiple diagnostic tools are used to characterize the formation and monitor fracture treatment and propagation. Geomechanical modeling is used to understand the insitu stresses, microseismic to describe half-lengths and heights, and fiber optics to characterize offset well. Fracture Driven Interactions (FDI’s) and interstage communication. Recent publications covering the MSEEL MIP-3H and MIP-5H wells are reviewed and discussed. A preview of the findings from the Boggess pad (first production in November 2019) is also shared here

03 NATURAL GAS↗

6 nm super-resolution optical transmission and scattering spectroscopic imaging of carbon nanotubes using a nanometer-scale white light source

Abstract Optical transmission and scattering spectroscopic microscopy at the visible and adjacent wavelengths denote one of the most informative and inclusive characterization methods in material research. Unfortunately, restricted by the diffraction limit of light, it cannot resolve the nanoscale variation in light absorption and scattering, diagnostics of the local inhomogeneity in material structure and properties. Moreover, a large quantity of nanomaterials has anisotropic optical properties that are appealing yet hard to characterize through conventional optical methods. There is an increasing demand to extend the optical hyperspectral imaging into the nanometer length scale. In this work, we report a super-resolution hyperspectral imaging technique that uses a nanoscale white light source generated by superfocusing the light from a tungsten-halogen lamp to simultaneously obtain optical transmission and scattering spectroscopic images. A 6-nm spatial resolution in the visible to near-infrared wavelength regime (415–980 nm) is demonstrated on an individual single-walled carbon nanotube (SW-CNT). Both the longitudinal and transverse optical electronic transitions are measured, and the SW-CNT chiral indices can be identified. The band structure modulation in a SW-CNT through strain engineering is mapped.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗