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At least 91 records · Page 5

Design of a Particle Shadow-graph Velocimetry and Size (PSVS) System to Determine Particle Size and Density Distributions in Hanford Nuclear Tank Wastes - 12280

Accurate particle size and density distributions for nuclear tank waste materials are essential information that helps determine the engineering requirements for a host of waste management unit operations (e.g., tank mixing, pipeline transport, and filtration). The most prevalent approach for determining particle size and density distribution is highly laborious and involves identifying individual particles using scanning electron microscope/x-ray diffraction and then acquiring the density of the materials from the technical literature. Other methods simply approximate individual particle densities by assuming chemical composition, rather than obtaining actual measurements of particle density. To overcome these limitations, a Particle Shadow-graph Velocimetry and Size (PSVS) system has been designed to simultaneously obtain particle size and density distributions for a broad range of Hanford tank waste materials existing as both individual particles and agglomerates. The PSVS system uses optical hardware, a temperature-controlled settling column, and particle introduction chamber to accurately and reproducibly obtain images of settling particles. Image analysis software provides a highly accurate determination of both particle terminal velocity and equivalent spherical particle diameter. The particle density is then calculated from Newton's terminal settling theory. The PSVS system was designed to accurately image particle/agglomerate sizes between 10 and 1000 μm and particle/agglomerate densities ranging from 1.4 to 11.5 g/cm{sup 3}, where the maximum terminal velocity does not exceed 10 cm/s. Preliminary testing was completed with standard materials and results were in good agreement with terminal settling theory. Recent results of this method development are presented, as well as experimental design. The primary goal of these PSVS system tests was to obtain accurate and reproducible particle size and velocity measurements to estimate particle densities within 20 percent of direct measured density values. The average percent error observed in particle densities was 4.8, 8.2, and 25.8 percent for S1D3 (high-density soda-lime glass), S3D4 (zirconia), and S1D2 (soda-lime glass) beads, respectively. The maximum measured particle density error observed was 14.5, 21.0, and 58.4, for S1D3, S3D4, and S1D2 beads, respectively. Multiple sources of error can exist that contribute to inaccurate estimates of particle density using the PSVS approach. Two significant influences observed were thermal convective currents in the settling column fluid and non-spherical (irregular) particle shapes in the standard test materials. Experimental results using buoyant beads suggest thermal convective currents can influence the movement of settling particles as much as 4 mm/s. These thermal convective currents are clearly a significant concern for smaller and less-dense particles/agglomerates which have terminal velocities of the same magnitude. Significant effort went into the design and fabrication of a thermal control system for the PSVS settling column. However, small temperature variations (<0.3 deg. C) are difficult to prevent and measure accurately. Therefore, although designing the thermal control system was necessary, it is not considered the only solution to minimize error due to thermal convective currents. The use of small diameter (10 to 27 μm) polyethylene buoyant beads (in low concentrations) during actual settling experiments may be necessary to provide insight into particle-particle interactions and fluid velocity correction factors to account for potential influences from thermal convective currents. Future testing will incorporate the buoyant beads into the analysis technique when the suspension fluid is chemically compatible. The use of the Newton's law to calculate particle/agglomerate densities assumes spherical particle shapes. As the actual particle/agglomerates diverge from spherical, the margin of error increases. The selection of high quality (in density and shape) monodispersed particle standards was a direct attempt to reduce the uncertainties associated with non-spherical or irregular particles and to only observe the PSVS method and analysis error. While investigating the source of data scatter for the S1D3 bead (nominal 700 μm) standard, significant irregular particles where discovered. Yet, a subsequent investigation into the S3D4 bead standard was also conducted and it was determined that 60 percent of the particles had a 0.9 to 0.8 centricity, 32 percent were between 0.8 and 0.7, only 7 percent were between 1.0 and 0.9, and the remaining 1 percent of the particles had centricities between 0.7 and 0.6. Contrast this with the S1D3 bead standard, where 100 percent of particles had centricities between 0.95 and 0.98, upon applying the centricity filter. The influence of the non-spherical shape of the S3D4 bead standard is evident when comparing a 3.9 percent average density error for S1D3 glass bead standard with an 8.3 percent average density error for the S3D4 bead standard. Model corrections for non-spherical shape must be implemented to account for these measurement errors during future method validation and system performance assessments. In addition, further work is needed to resolve the higher than expected velocities for the smaller S1D2 particles. Initial measurements conducted with buoyant beads as fluid velocity tracers indicate that fluid velocities can be subtracted from the increased particle velocities to determine the particle terminal velocity, regardless of the surrounding fluid velocity. However, this approach is in its infancy and will need to be carefully and methodically validated. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

On the measurement of austenite in supermartensitic stainless steel by X-ray diffraction

Sections of a 13Cr supermartensitic stainless steel were investigated to determine the optimum sample preparation for measurement of the austenite content by X-ray diffraction. The surface of several samples was mechanically ground or polished using media of grit sizes in the range 1–120 μm. The strained surface layer was afterwards removed stepwise by electropolishing, and the austenite content measured at each step. It was found that any level of mechanical grinding or polishing results in a reduction of the measured austenite fraction relative to the true bulk value, and that coarser grinding media impart greater damage and greater reduction in the measured austenite content. The results thus highlight the importance of the electropolishing step in preparation of such samples, but suggest that the American Society for Testing and Materials standard E975-03 substantially overestimates the amount of material which needs to be removed to recover the true “bulk” content. - Highlights: • Quantitative Rietveld analysis of austenite/martensite ratio in supermartensitic stainless steels • Critical evaluation of sample preparation for residual austenite measurements by X-ray diffraction • Highlighting of the importance of electropolishing as a final preparation step.

36 MATERIALS SCIENCE↗

Tensile and Microstructure Characterization of SNS Target Swirl Bubblers Fabricated by Additive Manufacturing

During operation the mercury facing surfaces of the Spallation Neutron Source target vessel are damaged by cavitation-induced erosion. One option to decrease the erosion damage to the SNS target vessel surfaces is to decrease the intensity of the pressure waves using small bubble mitigation. Injection of small diameter helium bubbles into mercury has been shown in decrease the intensity of proton-induced pressure waves and mitigate erosion damage to mercury/container interface surfaces. Several bubbler designs have been evaluated for implementation in the SNS target. One promising bubbler design is called a swirl bubbler, which is capable of producing a high density of very small diameter helium bubbles in flowing mercury. Due to the complexity of the swirl bubbler design and the geometric restrictions of conventional machining processes, additive manufacturing was considered for fabrication. But there was uncertainty with the mechanical properties of bubblers fabricated with additive manufacturing. A series of experiments were designed to characterize the tensile properties and microstructure of swirl bubblers fabricated using selective laser melting (SLM), both before and after consolidation via hot isostatic pressing (HIPing). This report summarizes the tensile and microstructural characterization of HIPed and non-HIPed swirl bubblers produced via the SLM process. The results show that the as-fabricated material contained appreciable porosity, lack-of-fusion defects, and inconsistent tensile properties with essentially zero ductility. But after a HIPing treatment the microstructure became fully consolidated, and the tensile properties surpassed the requirements specified in the material standard for steel-mill produced 316L plate material used to fabricate the SNS target vessel. While further testing is recommended to evaluate the material’s susceptibility to fatigue fracture, these results indicate 316L bubbler assemblies produced SLM and HIPed are promising candidates for implementation in a future SNS target module.

36 MATERIALS SCIENCE↗

Fabrication of Lightweight Radiation Shielding Composite Materials by Field Assisted Sintering Technique (FAST)

Advances in radiation shielding technologies are needed to protect humans and electronic components from all threats of space radiation over long durations. In this paper, we report on the use of the innovative and novel fabrication technology known as Field Assisted Sintering Technology (FAST) to fabricate lightweight material with enhanced radiation shielding strength to safeguard humans and electronics suitable for next generation space exploration missions. The base materials we investigated were aluminum (Al), the current standard material for space hardware, and Ultra-High Molecular Weight Polyethylene (UHMWPE), which has high hydrogen content and resistance to nuclear reaction from neutrons, making it a good shielding material for both gamma radiation and particles. UHMWPE also has high resistance to corrosive chemicals, extremely low moisture sensitivity, very low coefficient of friction, and high resistance to abrasion. We reinforced the base materials by adding high density (ie, high atomic weight) metallic material into the composite. These filler materials included: boron carbide (B4C), tungsten (W), tungsten carbide (WC) and gadolinium (Gd).

Prasad, Narasimha↗

Challenges and Vision for Standardization of Biopolymer Data Sets for Machine Learning

Machine learning (ML) is transforming materials research, yet potential for biopolymer discovery remains constrained by fragmented data and nonstandardized reporting. Biopolymers differ significantly from synthetic polymers, requiring specialized approaches to represent their biosynthetic origins, hierarchical structures, and application-specific metrics. In this Perspective, we identify three core challenges limiting biopolymer representation: information encoding, data quality, and data sharing. We describe the most pressing issues and propose commensurate approaches to address each key challenge. Recommendations include the design and adoption of biopolymer-specific fingerprinting and representation frameworks, development of hybrid human-large language model (LLM) data extraction strategies, and expanding Findable, Accessible, Interoperable, Reusable (FAIR)-compliant repositories. We propose a robust foundation to define interoperable, high-quality data sets that capture the full context of biopolymer materials. Standardized metadata, shared ontologies, and community-driven infrastructure would enable scalable, reproducible workflows and accelerate the ML-driven development of biopolymers.

36 MATERIALS SCIENCE↗

Electron and Light Microscopy Techniques Suitable for Studying Fatigue Damage in a Crystallized Glass Ceramic

The crystals of Pyroceram are randomly oriented and highly reflective so that standard microscopy techniques are not satisfactory for studying this material. Standard replicating procedures proved difficult to use. New microscopy techniques and procedures have therefore been developed. A method for locating, orienting, and identifying specific areas to be viewed with an electron microscope is described. This method not require any special equipment. Plastic replicas were found to be unsatisfactory because of their tendency to adhere to Pryoceram. This caused them to tear when released or resulted in artifacts. Preshadowed silicon monoxide replicas were satisfactory but required a releasing agent. A method of depositing the releasing agent is described. To polish specimens without evidence of fire-polishing, it was found necessary to use a vibratory polishing technique. Chrome oxide was used as the abrasive and either water or kerosene as the lubricant. Vibratory polishing is extremely slow, but surfaces so polished show no evidence of fire polishing, even when examined by electron microscopy. The most satisfactory etching process used for Pyroceram 9608 consisted of a primary etch of 5 milliliters of hydrochloric acid (concentrated), 5 milliliters of hydrogen fluoride (45 percent), and 45 milliliters of water, and a secondary etch with methyl alcohol replacing the water. Best results were obtained with total etching times from 25 to 30 seconds. Staining of the Pyroceram surface with a Sanford's marker was found to be an expedient way to reduce the glare of reflected light.

Harrell, Shelley↗

Insitu Calibration of Quartz Crystal Microbalances

Computer models that predict the rate at which molecular contamination will deposit on optical surfaces typically use outgassing source terms, measured with quartz crystal microbalances, as a basis for the prediction. The American Society of Testing and Materials, Standard Test Method for Contamination Outgassing Characteristics of Spacecraft Materials (Method E-1559), is probably the best know technique used by the aerospace community to measure the outgassing rates or source terms of materials. A simple method for the insitu calibration of quartz crystal microbalances, based on the heat of enthalphy of Adipic Acid, has been developed and demonstrated by the Marshall Space Flight Center, Environmental Effects Group. The calibration has been demonstrated over a sample temperature range of 25 to 66 degrees Celsius and deposition rates of 7 x 10 (exp -11) grams/cm(sup 2)-s and greater, for several measurement system configurations. This calibration technique is fully compatible with the American Society for Testing and Materials, Method E-1559, as well as other methodology. The calibration requires no modification of outgassing facilities employing an effusion cell and does not degrade the performance or function of typical vacuum systems.

Albyn, Keith↗

Developing quartz and molybdenum as impedance-matching standards in the 100-Mbar regime

We present quartz and molybdenum single-shock Hugoniot data to 62 Mbar and 120 Mbar, respectively. Quartz and molybdenum are attractive standard materials for Hugoniot equation-of-state impedance-matching studies. Quartz is advantageous because a reflecting shock front is supported above ~1 Mbar whose velocity can be tracked in situ to very high accuracy. Molybdenum's relatively high impedance makes it a more appropriate standard for other high-impedance material studies to avoid large departures from the standard principal Hugoniot upon release or reshock into the sample. Extensive measurements already exist for both materials up to about 10 Mbar and 10 eV, but new high-energy-density facilities and techniques have extended the experimentally accessible pressure range to >100 Mbar. The data presented here indicate which modern equation-of-state models can be reliably extended into newly-accessible experimental regimes.

36 MATERIALS SCIENCE↗

Dispersive interactions between standard and Dirac materials and the role of dimensionality

The van der Waals (vdW) interaction plays a prominent role between neutral objects at separations where short ranged chemical forces are negligible. This type of dispersive coupling is determined by the interplay between geometry and response properties of the materials making up the objects. Here, we investigate the vdW interaction between 1D, 2D, and 3D standard and Dirac materials within the Random Phase Approximation, which takes into account collective excitations originating from the electronic Coulomb potential. A comprehensive understanding of characteristic functionalities and scaling laws are obtained for systems with parabolic energy dispersion (standard materials) and crossing linear bands (Dirac materials). By comparing the quantum mechanical and thermal limits the onset of thermal fluctuations in the vdW interaction is discussed showing that thermal effects are significantly pronounced at smaller scales in reduced dimensions.

36 MATERIALS SCIENCE↗

Quantum Chemistry Calculations for Metabolomics

A primary goal of metabolomics and exposomics studies is to fully characterize the small molecule composition of complex biological and environmental samples. However, despite advances in analytical technologies over the past two decades, the majority of small molecules in complex samples are not readily identifiable due to the immense structural and chemical diversi-ty present within the metabolome and exposome. Current gold-standard identification methods rely on reference libraries built using authentic chemical materials (“standards”), which are not available for most molecules. Computational quantum chemis-try methods, which can be used to calculate chemical properties that are then measured by analytical platforms, offer an alter-native route for building reference libraries, i.e., in silico libraries for “standards-free” identification. In this review, we cover the major roadblocks currently facing metabolomics and discuss applications where quantum chemistry calculations offer a solu-tion. Several successful examples for nuclear magnetic resonance spectroscopy, ion mobility spectrometry, infrared spectros-copy, and mass spectrometry methods are reviewed. Finally, we consider current best practices, sources of error, and provide an outlook for quantum chemistry calculations in metabolomics and exposomics studies. We expect this review will inspire researchers in the field of small molecule identification to accelerate adoption of in silico methods for generation of reference libraries and to add quantum chemistry calculations as another tool at their disposal to characterize complex samples.

Metabolism↗

Radiometry of water turbidity measurements

An examination of a number of measurements of turbidity reported in the literature reveals considerable variability in the definitions, units, and measurement techniques used. Many of these measurements differ radically in the optical quantity measured. The radiometric basis of each of the most common definitions of turbidity is examined. Several commercially available turbidimeters are described and their principles of operation are evaluated radiometrically. It is recommended that the term turbidity be restricted to measurements based upon the light scattered by the sample with that scattered by standard suspensions of known turbidity. It is also recommended that the measurement procedure be standardized by requiring the use of Formazin as the turbidity standardizing material and that the Formazin Turbidity Unit (FTU) be adopted as the standard unit of turbidity.

Mccluney, W. R.↗

Molecular Substrate Alteration by Solar Wind Radiation Documented on Flown Genesis Mission Array Materials

The Genesis spacecraft sampling arrays were exposed to various regimes of solar wind during flight that included: 313.01 days of high-speed wind from coronal holes, 335.19 days of low-speed inter-stream wind, 191.79 days of coronal mass ejections, and 852.83 days of bulk solar wind at Lagrange 1 orbit. Ellipsometry measurements taken at NASA s Johnson Space Center show that all nine flown array materials from the four Genesis regimes have been altered by solar wind exposure during flight. These measurements show significant changes in the optical constant for all nine ultra-pure materials that flew on Genesis when compared with their non-flight material standard. This change in the optical constant (n and k) of the material suggests that the molecular structure of the all nine ultra-pure materials have been altered by solar radiation. In addition, 50 samples of float-zone and czochralski silicon bulk array ellipsometry results were modeled with an effective medium approximation layer (EMA substrate layer) revealing a solar radiation molecular damage zone depth below the SiO2 native oxide layer ranging from 392 to 613 . This bulk solar wind radiation penetration depth is comparable to the depth of solar wind implantation depth of Mg measured by SIMS and SARISA.

Calaway, Michael J.↗

Estimation of Performance of an Active Well Coincidence Counter Equipped with Boron-Coated Straw Neutron Detectors - 13401

He-3, a very rare isotope of natural helium gas, has ideal properties for the detection of thermal neutrons. As such it has become the standard material for neutron detectors and sees ubiquitous use within many radiometric applications that require neutron sensitivity. Until recently, there has been a fairly abundant supply of He-3. However, with the reduction in nuclear weapons, production of tritium ceased decades ago and the stockpile has largely decayed away, reducing the available He-3 supply to a small fraction of that needed for neutron detection. A suitable and rapidly-deployable replacement technology for neutron detectors must be found. Many potential replacement technologies are under active investigation and development. One broad class of technologies utilizes B-10 as a neutron capture medium in coatings on the internal surfaces of proportional detectors. A particular implementation of this sort of technology is the boron-coated 'straw' (BCS) detectors under development by Proportional Technologies, Inc. (PTi). This technology employs a coating of B-10 enriched boron carbide (B{sub 4}C) on the inside of narrow tubes, roughly 4 mm in diameter. A neutron counter (e.g. a slab, a well counter, or a large assay counter designed to accommodate 200 liter drums) could be constructed by distributing these narrow tubes throughout the polyethylene body of the counter. One type of neutron counter that is of particular importance to safeguards applications is the Active Well Coincidence Counter (AWCC), which is a Los Alamos design that traditionally employs 42 He-3 detectors. This is a very flexible design which can accurately assay small samples of uranium- and plutonium-bearing materials. Utilizing the MCNPX code and benchmarking against measurements where possible, the standard AWCC has been redesigned to utilize the BCS technology. Particular aspects of the counter performance include the single-neutron ('singles') detection efficiency and the time constant for the decrease in neutron population in the counter following a fission event (a.k.a. the die-away time). Results of the modeling and optimization are presented. (authors)

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Meta-Study of Particulate Detection Losses on Radioactive Air Sample Filters

Several mathematical relationships between air sample filter mass loading and the correlated analytical self-absorption factor were developed using data from other published research in this meta-study. Gross-alpha and -beta applications are addressed for this research. As filter media becomes loaded with particulate matter, there is potential for measurement losses due to self-absorption by mass loading. Components contributing to absorption include particulate dust, radioactive particulates, and filter material. Standards indicate a correction factor should be used when the penetration of radioactive material into the collection media or self-absorption of radiation by the material collected would reduce the detection rate by more than 5%. Previously, losses due to self-absorption have been reported up to 100% over a range up to ~10 mg∙cm -2 mass loading. These absorption losses then can be used to determine a correction factor for sample results. For low mass loadings (e.g., ≤0.1 mg∙cm -2 ) corrections factors in the 0.85 - 1 range have been recommended and used, while at higher mass loadings nearer to 10 mg∙cm -2 correction factors closer to 0 (representing near 100% losses) are used. Based on data from published studies, the different methods for relating percent loss due to self-absorption to mass loading include linear, exponential, quadratic, and trinomial derived functions. Where applicable, both forced zero and non-forced zero results were evaluated. From the derived functions evaluated, the trinomial function provided the best fit. Once the sample filter mass loading is known, the trinomial function can be applied to estimate losses and the corresponding self-absorption factor. When applied to routine operating conditions for radiological facility stacks monitored at the Pacific Northwest National Laboratory for an average sample filter mass loading of 0.09 ± 0.12 (2σ) mg∙cm -2 (excluding negative values and outliers) and a range from 0 - 0.24 mg∙cm -2 , the estimated trinomial function nominal self-absorption losses are less than 5% at 0.09 mg∙cm -2 and less than 10% at 0.24 mg∙cm -2 . The trinomial function is one method that may be used to adjust the activity results of an air sample when the sample-specific mass loading is determined. The application of no correction factor when the ANSI/HPS N13.1-2021 guidance of a 5% threshold for loss is not reached with typical stack sample mass loadings may be reasonable in high-efficiency particulate air filtered systems. For simplicity, it would be conservative in assigning the self-absorption correction factor at the 5% threshold (i.e., 0.95) for general uses but in cases of heavy mass loading to calculate the factor.

air sampling↗