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All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Reactive flash sintering of TiZrN and TiAlN ternary metal nitrides

Here, this study demonstrated the reactive flash sintering (RFS) for two powder mixtures: TiN-ZrN (both conducting) and AlN-TiN (TiN conducting but AlN insulating), targeting ternary metal nitrides (TMN) of Ti 0.5 Zr 0.5 N and Ti 0.5 Al 0.5 N, respectively. A constant volage and pressure (e.g., 8 V DC, ∼15 MPa) at room temperature triggered the flash (current density up to 27 A/mm 2 ) without pre-heating, and the entire RFS process finished in a few minutes. For TiZrN, the flash was instantaneous whereas for TiAlN, there was a long incubation before the flash followed by a quick and dramatic flash. Both conventional ex situ XRD and in situ synchrotron study had been carried out. They showed a uniform Ti 0.57 Zr 0.43 N solution formed in RFS and persisted upon cooling, while (Ti, Al) N solid solution formed at high temperature was not stable and likely went through a very quick phase separation in the cooling process. The final products from RFS had been characterized using SEM/EDS for microstructure. Both TiZrN and TiAlN were dense. Distribution of Ti, Zr, and N was uniform for TiZrN; for TiAlN, Ti and N distribution was uniform, while association of Al with oxygen was observed. TGA-DSC revealed the onset oxidation temperature for TiZrN was comparable to TiN and ZrN, while it was higher by ∼200 °C for TiAlN, likely due to the formation of Al 2 O 3 . In terms of mechanical properties such as hardness or fracture toughness, forming a single-phase solid solution (like TiZrN) does not offer obvious benefits. while large grain size from RFS seemed to be unfavorable. Future optimization of RFS condition and in-depth study by both experiments and simulation are needed to fully understand the composition-processing-structure-property relationships for such TMN from the reactive flash sintering process.

Flash Sintering↗
DOE OSTI2024

Computer vision models and advanced TEM imaging for microstructures of irradiated AM316 stainless steels

Advancements were made in automating microscopy-based material characterization, particularly in studying irradiation effects on additively manufactured (AM) materials using machine learning (ML) and computer vision (CV). These automation efforts address the challenges of analyzing complex microstructures, accelerating the detection of irradiation-induced defects. Two CV models were developed at Argonne National Laboratory (ANL) to enhance transmission electron microscopy (TEM) analysis of irradiated AM 316 stainless steel. The first model focused on the detection of irradiation-induced dislocation loops, which contribute to material hardening and embrittlement. These loops, categorized as faulted or perfect, were automatically detected and classified using a Mask R-CNN model trained on TEM images from both in-situ and ex-situ ion irradiation experiments. The model achieved high accuracy, with precision, recall, and F1 scores of 0.839, 0.734, and 0.776, respectively, demonstrating its effectiveness in analyzing dislocation loops in irradiated AM materials. The second CV model was developed to analyze the size and wall thickness of dislocation cells in laser powder bed fusion (LPBF) 316 stainless steel. Using a U-Net++ architecture with EfficientNet as the encoder, the model was trained on TEM images to segment and measure cell size and wall thickness.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Nanocrystalline ZrN thin film development via atomic layer deposition for U-Mo powder

Zirconium nitride (ZrN) thin film deposited via thermal atomic layer deposition (ALD) has been recently chosen as a candidate technology for application of a diffusion barrier coating on the low enriched uranium alloy powder considered in the NNSA research reactor conversion program. Reported here is the first instance of using ALD for coating actinide materials. For this study, a modified ALD system was constructed to produce one micron thick zirconium nitride (ZrN) coating over spherical particulate of natural uranium-molybdenum (U-Mo) based fuel. The ALD system was designed to have a rotating drum system, with provisions for facilitating sequential exposures of chemicals such as tetrakis dimethyl amido zirconium (TDMAZr) and ammonia (NH 3 ) in order to deposit ZrN. The ALD system was successful in developing a highly conformal ZrN coating covering every individual U-7Mo particle. This article describes the ZrN film synthesis details and reports the produced microstructure and composition of the ALD ZrN as deposited on fuel particulates. The as-fabricated coating was determined to have a nanocrystalline structure in the cubic-ZrN (cF8) phase. It exhibited a dense microstructure with adequate interfacial bonding. TEM-EELS characterization demonstrated that the coating contains a very low amount of oxygen impurity. To understand the potential microstructural evolution for ALD ZrN during reactor operation, an in-situ heavy ion (Kr) irradiation experiment was performed at the IVEM-Tandem facility. A total fluence of 7.5 x 10 15 ions/cm 2 (similar to 10 dpa) was achieved, and apart from minor grain coarsening in the ALD ZrN coating, no significant radiation effects were observed.

36 MATERIALS SCIENCE↗
DOE OSTI2024

The Role of Alkalis in Orchestrating Uranyl-Peroxide Reactivity Leading to Direct Air Capture of Carbon Dioxide

Spectator ions have known and emerging roles in aqueous metal-cation chemistry, respectively directing solubility, speciation, and reactivity. Here, in this work, we isolate and structurally characterize the last two metastable members of the alkali uranyl triperoxide series, the Rb + and Cs + salts (Cs-U 1 and Rb-U 1 ). We document their rapid solution polymerization via small-angle X-ray scattering, which is compared to the more stable Li + , Na + and K + analogues. To understand the role of the alkalis, we also quantify alkali-hydroxide promoted peroxide deprotonation and decomposition, which generally exhibits increasing reactivity with increasing alkali size. Cs-U 1 , the most unstable of the uranyl triperoxide monomers, undergoes ambient direct air capture of CO 2 in the solid-state, converting to Cs 4 [U VI O 2 (CO 3 ) 3 ], evidenced by single-crystal X-ray diffraction, transmission electron microscopy, and Raman spectroscopy. We have attempted to benchmark the evolution of Cs-U 1 to uranyl tricarbonate, which involves a transient, unstable hygroscopic solid that contains predominantly pentavalent uranium, quantified by X-ray photoelectron spectroscopy. Powder X-ray diffraction suggests this intermediate state contains a hydrous derivative of CsU V O 3 , where the parent phase has been computationally predicted, but not yet synthesized.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Assessment of Impurities in Neptunium Metal Using Double-Focusing SF-ICP-MS

In the transmutation process, minor actinides such as neptunium, americium and curium obtained from spent nuclear fuel are incorporated into new fuel that can be placed into a fast reactor, where these elements fission into products with shorter half-lives which reduces the health and safety hazards. In order to better understand the all the involved processes, fundamental physical properties of actinides should be investigated, and for that reason, high-purity materials need to be produced. One of the main challenges in characterizing these materials is the lack of pure metal available for study, and lack of analytical methods to determine the purity. Trans-uranic elements are challenging to study because of the need to be handled in specialized facilities, safeguards concerns and they are not easily purchased and/or produced. High-purity Np metal is being produced at the Materials and Fuels Complex (MFC) of Idaho National Laboratory (INL), in a process of direct oxide reduction developed by Squires and Lessing, with a target purity of 99.999%. The goal of this research is to develop methods to determine the impurities in the Np metal, with detection limits low enough to achieve this purity level. In this work, we have used several ICP-MS and ICP OES techniques, but the focus was the method development using a recently acquired Double-Focusing Sector Field Inductively Coupled Plasma Mass Spectrometer (SF-ICP-MS). To produce the Np metal, approximately 20 g of the neptunium oxide powder was calcined at 800 oC for 6 h in a magnesium oxide crucible, which is placed inside a stainless steel crucible, that goes into the Hot Uniaxial Press (HUP) furnace insert. After the calcining step, the Np oxide was mixed with approximately 9 g of calcium metal and 100 g of ultra-dry calcium chloride. The HUP furnace was heated in a ramp rate of 50 oC min -1 up to 1000 oC. When the reaction mixture reached 850 oC, a tantalum stirrer was activated at 100 rpm. After the tantalum stirrer was removed and the mixture cooled overnight, the MgO crucible was opened with a hammer and chisel to retrieve the Np metal button at the bottom of the reaction mixture. Prior to the dissolution process, the surface contaminants of the sample were removed. The Np button was washed in 10 mL of ultra-pure water for 1 min, with a faint reaction observed on the surface, indicating the presence of Ca metal. The water-washed sample was placed in a tube with 2 M HCl for only 3 s, as a vigorous reaction in the button surface was observed. The leachates were saved for further analysis. The sample was then rinsed with ultra-pure water and air-dried prior to dissolution. The cleaned sample was placed in a PTFE beaker and 25 mL of 6 M HCl and 150 µL of 24 M HF were added. After 10 minutes of reaction, the beaker was placed on a hot plate for 1 h and 30 min, followed by the addition of 1 mL of 16 M HNO3 and allowed to react for a further 1 h and 20 min. The sample was removed from heat and 10 mL of HNO3 16 M was added to react with the HCl. The beaker was covered and left for overnight reaction, producing a solution with approximately 20 mL of final volume. A Quadrupole Inductively Coupled Plasma Mass Spectrometer (Q-ICP-MS, Perkin Elmer ELAN DRC II Q-ICP-MS) was used to obtain qualitative mass spectra for the dissolution blank, each of the leachates and the dissolved sample. In the water leachate spectrum mainly Ca and Mg were observed, while the acid wash had a similar peak pattern to the one observed for the Np metal sample, indicating that the process not only removed surface contamination, but also reacted with the sample itself. In the Np material spectrum, Ta and actinides were identified as candidates for major contaminants, as the most intense peaks corresponded to the mass-to-charge ratios of these elements. Minor contaminants included Al, Au, Ca, Cr, Fe, I, Na, Nb, Pb, Sn, Ti, Tl, V, Y. The presence of impurities in the material could have originated from several sources, such as the materials used for the casting process, the use of impure NpO2 or contamination of reagents and materials used for the analysis. Some of the isotopes listed as potential contaminants are susceptible to spectral interferences, so Double-Focusing SF-ICP-MS (Nu Instruments Attom ES HR-ICP-MS) was used for the quantitative analysis. For each isotope determined, several items were evaluated: raw signal of a blank solution, sensitivity and determination coefficient of calibration curves, possibility of interferences and comparison of results obtained for at least two resolving powers (RP): 300 and 4000. The evaluation of the signal in a blank solution can indicate if a spectral interference from the plasma gas and/or the solvent was successfully resolved (commonly observed for 52Cr+/40Ar12C+, for example). It is important to highlight that a signal reduction is expected when a higher RP is used, as the ion beam transmission is decreased by the use of narrower slits

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2019

ASSESMENT OF IMPURITIES IN NP METAL USING DOUBLE-FOCUSING SF-ICP-MS

In the transmutation process, minor actinides such as neptunium, americium and curium obtained from spent nuclear fuel are incorporated into new fuel that can be placed into a fast reactor, where these elements fission into products with shorter half-lives which reduces the health and safety hazards [1]. In order to better understand the all the involved processes, fundamental physical properties of actinides should be investigated, and for that reason, high-purity materials need to be produced. One of the main challenges in characterizing these materials is the lack of pure metal available for study, and lack of analytical methods to determine the purity. Trans-uranic elements are challenging to study because of the need to be handled in specialized facilities, safeguards concerns and they are not easily purchased and/or produced. High-purity Np metal is being produced at the Materials and Fuels Complex (MFC) of Idaho National Laboratory (INL), in a process of direct oxide reduction developed by Squires and Lessing [2], with a target purity of 99.999%. The goal of this research is to develop methods to determine the impurities in the Np metal, with detection limits low enough to achieve this purity level. In this work, we have used several ICP-MS and ICP OES techniques, but the focus was the method development using a recently acquired Double-Focusing Sector Field Inductively Coupled Plasma Mass Spectrometer (SF-ICP-MS). To produce the Np metal, approximately 20 g of the neptunium oxide powder was calcined at 800 oC for 6 h in a magnesium oxide crucible, which is placed inside a stainless steel crucible, that goes into the Hot Uniaxial Press (HUP) furnace insert. After the calcining step, the Np oxide was mixed with approximately 9 g of calcium metal and 100 g of ultra-dry calcium chloride. The HUP furnace was heated in a ramp rate of 50 oC min -1 up to 1000 oC. When the reaction mixture reached 850 oC, a tantalum stirrer was activated at 100 rpm. After the tantalum stirrer was removed and the mixture cooled overnight, the MgO crucible was opened with a hammer and chisel to retrieve the Np metal button at the bottom of the reaction mixture [2]. Prior to the dissolution process, the surface contaminants of the sample were removed. The Np button was washed in 10 mL of ultra-pure water for 1 min, with a faint reaction observed on the surface, indicating the presence of Ca metal. The water-washed sample was placed in a tube with 2 M HCl for only 3 s, as a vigorous reaction in the button surface was observed. The leachates were saved for further analysis. The sample was then rinsed with ultra-pure water and air-dried prior to dissolution. The cleaned sample was placed in a PTFE beaker and 25 mL of 6 M HCl and 150 µL of 24 M HF were added. After 10 minutes of reaction, the beaker was placed on a hot plate for 1 h and 30 min, followed by the addition of 1 mL of 16 M HNO3 and allowed to react for a further 1 h and 20 min. The sample was removed from heat and 10 mL of HNO3 16 M was added to react with the HCl. The beaker was covered and left for overnight reaction, producing a solution with approximately 20 mL of final volume. A Quadrupole Inductively Coupled Plasma Mass Spectrometer (Q-ICP-MS, Perkin Elmer ELAN DRC II Q-ICP-MS) was used to obtain qualitative mass spectra for the dissolution blank, each of the leachates and the dissolved sample. In the water leachate spectrum mainly Ca and Mg were observed, while the acid wash had a similar peak pattern to the one observed for the Np metal sample, indicating that the process not only removed surface contamination, but also reacted with the sample itself. In the Np material spectrum, Ta and actinides were identified as candidates for major contaminants, as the most intense peaks corresponded to the mass-to-charge ratios of these elements. Minor contaminants included Al, Au, Ca, Cr, Fe, I, Na, Nb, Pb, Sn, Ti, Tl, V, Y. The presence of impurities in the material could have originated from several sources, such as the materials used for the casting process, the use of impure NpO2 or contamination of reagents and materials used for the analysis. Some of the isotopes listed as potential contaminants are susceptible to spectral interferences, so Double-Focusing SF-ICP-MS (Nu Instruments Attom ES HR-ICP-MS) was used for the quantitative analysis. For each isotope determined, several items were evaluated: raw signal of a blank solution, sensitivity and determination coefficient of calibration curves, possibility of interferences and comparison of results obtained for at least two resolving powers (RP): 300 and 4000. The evaluation of the signal in a blank solution can indicate if a spectral interference from the plasma gas and/or the solvent was successfully resolved (commonly observed for 52Cr+/40Ar12C+, for example). It is important to highlight that a signal reduction is expected when a higher RP is used, as the ion beam transmission is decreased by the use of na

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Additive manufacturing of metal matrix composites

Although Metal matrix composites (MMCs) are superior to most sought-after metallic alloys, their challenging fabricability has limited their widespread use in bulk-form applications. Among the many advanced fabrication techniques, Additive Manufacturing (AM), owing to its unique capabilities to produce near-net shapes, has drawn significant traction in the past two decades, especially for materials that are difficult to process using traditional methods. However, unlike pure metal/alloy systems, MMCs are highly sensitive to the processing conditions prevailing in AM techniques due to factors such as the high melting point of reinforcement particles and the potential for in-situ reactions. Therefore, it may be a while before metal matrix composites are commercially produced via AM. This review will discuss the current state-of-the-art design, fabricability, and performance of various additively manufactured MMCs. A particular focus will be on microstructural evolution and microstructure-property relationships. The most employed AM techniques, such as directed energy deposition, powder bed fusion, binder jetting, sheet lamination, and solid-state friction stir processing, are fundamentally different in terms of thermo-kinetics, forming the perspective for this review. A detailed comparison of microstructural evolution and process parameter optimization, including feedstock preparation methods and the role of machine learning and modeling among the different AM processes, is also presented. Finally, a critical evaluation of emerging AM technologies for MMCs is also provided, highlighting their potential advantages and challenges.

36 - MATERIALS SCIENCE↗
DOE OSTI2020

Nucleation of Dislocations in 3.9 nm Nanocrystals at High Pressure

As circuitry approaches single nanometer length scales, it has become important to predict the stability of single nanometer-sized metals. The behavior of metals at larger scales can be predicted based on the behavior of dislocations, but it is unclear if dislocations can form and be sustained at single nanometer dimensions. Here, we report the formation of dislocations within individual 3.9 nm Au nanocrystals under nonhydrostatic pressure in a diamond anvil cell. We used a combination of x-ray diffraction, optical absorbance spectroscopy, and molecular dynamics simulation to characterize the defects that are formed, which were found to be surface-nucleated partial dislocations. These results indicate that dislocations are still active at single nanometer length scales and can lead to permanent plasticity.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2022

Solvent-Driven Transformation of Zn/Cd 2+ -Deoxycholate Assemblies

Deoxycholic acid (DOC) is a unique, biologically derived surfactant with facial amphiphilicity that has been exploited, albeit minimally, in supramolecular assembly of materials. Here, we present the synthesis and structural characterization of three hybrid metal (Zn 2+ and Cd 2+ )-DOC compounds. Analysis by single-crystal Xray diffraction reveals the many interactions that are possible between these facial surfactants and the influence of solvent molecules that drive the assembly of materials. These structures are the first metal- DOC complexes besides those obtained from alkali and alkaline earth metals. We isolated polymeric chains of both Cd and Zn (Zn poly -DOC and Cd poly -DOC) from water. Major interactions between DOC molecules in these phases are hydrophobic in nature. Cd poly -DOC exhibits unique P1 symmetry, with complete interdigitation of the amphiphiles between neighboring polymeric chains. Zn 4 -DOC, obtained from methanol dissolution of Zn poly -DOC, features the OZn 4 tetrahedron, widely known in basic zinc acetate and MOF-5 (metal organic framework). We document a solvent-driven, roomtemperature transition between Zn poly -DOC and Zn 4 -DOC (in both directions) by scanning and transmission electron microscopies in addition to small-angle X-ray scattering, powder X-ray diffraction, and infrared spectroscopy. These studies show the methanoldriven transition of Zn poly -DOC to Zn 4 -DOC occurs via an intermediate with no long-range order of the Zn 4 clusters, indicating the strongest interactions driving assembly are intramolecular. On the contrary, water-driven solid-to-solid transformation from Zn 4 -DOC to Zn poly -DOC exhibits crystal-to-crystal transformation. Zn poly -DOC is robust, easy to synthesize, and comprised of biologically benign components, so we demonstrate dye absorption as a proxy for water treatment applications. It favors absorption of positively charged dyes. These studies advance molecular level knowledge of the supramolecular assembly of facial surfactants that can be exploited in the design of organic-inorganic hybrid materials. This research also highlights the potential of solvent for tuning supramolecular assembly processes, leading to new hybrid materials featuring facial surfactants.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

A process optimization framework for laser direct energy deposition: Densification, microstructure, and mechanical properties of an Fe-Cr alloy

Laser Direct Energy Deposition (DED) is a metal additive manufacturing technique with the ability to fabricate large and complex parts through deposition of metal powders. However, achieving high-density parts and targeted build heights using DED can be challenging due to the large number of highly sensitive process variables. This work proposes a robust fabrication parameter optimization framework to generate process maps for primary parameters in DED, including laser power, scan speed, mass flow rate, hatch spacing, and layer height. Simple single-track experiments were utilized to map out the parameter space, and a combination of geometric criteria for hatch spacing and layer height were proposed to determine parameter sets that achieve both targeted build heights and mitigate porosity formation. Using this framework, specimens with >99 % density and consistent mechanical properties were successfully fabricated over a wide range of process parameters for an Fe-9wt.%Cr (Fe9Cr) alloy, a surrogate for radiation damage-resistant reduced activation ferritic/martensitic (RAFM) steels. Processing these materials using DED is of particular interest in the development of plasma facing components for nuclear fusion applications. The microstructure and mechanical properties of as-printed Fe9Cr were characterized using optical and electron microscopy, X-ray diffraction, and uniaxial tensile tests. As-printed Fe9Cr displayed ~25 % elongation and ultimate tensile strengths of up to 475 MPa which is comparable to similar wrought alloys. Finally, the proposed framework will allow for accelerated DED parameter optimization for novel alloy systems, as well as open the possibility for local microstructure control while simultaneously mitigating defect formation.

42 ENGINEERING↗
DOE OSTI2024

Elemental profiling and genomewide association studies reveal genomic variants modulating ionomic composition in Populus trichocarpa leaves

Samples were collected from a population of 1,089 black cottonwood genotypes (P. trichocarpa) assembled from native stands to encompass the central portion of the natural range of the species, stretching from 38.8° to 54.3° N Q13 latitude from California, USA, to British Columbia, Canada. Establishment of the common garden, growth conditions, and site maintenance have been described by Muchero et al (2015). In this study, leaf samples for ionomic profiling were collected from 4-year-old trees, during the growing season, in July 2012, from a field located in Clatskanie, Oregon, USA (46°6′11″N 123°12′13″W). The field site was located in a protected alluvial floodplain containing a uniform Wauna-Locoda silt loam soil area characterized by an acidic pH, in Columbia County, Oregon. A subset of 584 out of the 1,089 P. trichocarpa genotypes were represented in this sampling. These genotypes were randomly selected to represent the geographical distribution of the population. A single fully mature (LPI 7-9) leaf on the south side of the tree exposed to full sunlight conditions was removed from the tree within a 6-hour window centering on solar noon and immediately frozen under dry ice before processing. Leaf samples of 584 P. trichocarpa genotypes were finely ground to 40 mm particle size using a mortar and pestle, and ionomic composition was analyzed using ICP-MS. In total, 20 elements were profiled, including aluminum (Al27), arsenic (As75), boron (B11), cadmium (Cd111), calcium (Ca43), cobalt (Co), copper (Cu), iron (Fe57), magnesium (Mg25), manganese (Mn55), molybdenum (Mo), nickel (Ni60), phosphorus (P31), potassium (K39), rubidium (Rb85), selenium (Se82), sodium (Na23), strontium (Sr88), sulfur (S34), and zinc (Zn66), following a protocol established by Ziegler et al. (2013). For each sample, 75mg of powder was digested overnight in 2.5 mL HNO3 containing 20 parts per billion (ppb) indium as an internal standard, following the protocol described in Ziegler et al. (2013). Following a dilution, concentration of the 20 elements was measured using an Elan 6000 DRC-e mass spectrometer (Perkin-Elmer SCIEX) connected to a PFA microflow nebulizer (Elemental Scientific) and Apex HF desolvator (Elemental Scientific). One measurement per sample per genotype was done. For subsequent analyses, the quantifications were converted to total element concentration.

CBI ionomics, GWAS, plasma-mass spectrometry, neut↗
NASA NTRS2005

Effects of High-Temperature Exposures on the Fatigue Life of Disk Superalloys Examined

Tests used to characterize the low-cycle-fatigue resistance of disk superalloys are usually performed at cyclic frequencies of 0.33 Hz or faster. However, service conditions for disks in some aerospace and land-based gas turbine engines can produce major cycle periods extending from minutes to hours and days. Over a service life, this can produce total service times near the maximum temperature that exceed 100 hr for aerospace applications and 100,000 hr for land-based applications. Such time-dependent effects of realistic mission cycles on fatigue resistance can be significant in superalloy disks, and need to be considered for accurate disk life prediction. The purpose of this study at the NASA Glenn Research Center was to examine the effects of extended exposures and extended cycle periods on the fatigue resistance of two disk superalloys. Current alloy Udimet 720 (Special Metals Corporation, Huntington, WV) disk material was provided by Solar Turbines/Caterpillar Co., and advanced alloy ME3 was provided by the NASA Ultra-Efficient Engine Technologies (UEET) Project, in powder-metallurgy-processed, supersolvus heat-treated form. Fatigue specimens were fully machined and exposed in air at temperatures of 650 to 704 C for extended times. Then, they were tested using conventional fatigue tests with a total strain range of 0.70 percent and a minimum-to-maximum strain ratio of zero to determine the effects of prior exposure on fatigue resistance. Subsequent tests with extended dwells at minimum strain in each fatigue cycle were performed to determine cyclic exposure effects.

Gabb, Timothy P.↗
DOE OSTI2019

Criticality Accident Alarm System Shielding Benchmark: Integral Experiment Request 498, Critical Engineering Decision 1 Report

This report supports Critical/Subcritical Experiment Decision 1 (CED-1) for Integral Experiment Request (IER) 498, a shielding benchmark produced using the Godiva IV critical assembly at the National Critical Experiments Research Center (NCERC). Shielding benchmarks are datasets collected to provide a comparison for computer models that simulate the effect of shielding on radiation transmission from a source to a detector. The purpose of a CED-1 report is to produce a conceptual design for an integral experiment and to identify the long lead-time items. The design presented in this report favors certain detailed design options such as material selections. However, alternative options can be selected as the project evolves. Dimensions are specified only as needed to evaluate feasibility and performance. Development of Criticality Accident Alarm System (CAAS) shielding benchmarks supports two main programmatic needs. The first need is to improve confidence in models of facilities that house nuclear material handling operations. Better models can support effective CAAS detector placement when criticality may result in dose, and it enables more accurate analysis of criticality accident impacts at various locations in a facility. A key quantity that can be verified is the secondary gamma production caused by neutron interactions with various materials. The second programmatic need supported by shielding benchmarks is the ongoing development of methods being integrated into nuclear simulation codes such as the Monte Carlo N-Particle (MCNP) transport code and the SCALE code system used in efforts funded by the Nuclear Criticality Safety Program (NCSP). Previous work performed under the International Criticality Safety Benchmark Experimental Program (ICSBEP) to produce shielding benchmark data is primarily limited to a set of measurements at the SILENE critical assembly at the Valduc facility in France. The experiment used an open configuration and a burst mode operation, which limited detector options to thermoluminescent dosimeters (TLDs) and activation foils. Because TLDs do not record gamma spectra, it was difficult to verify the gamma energy spectrum from the experiment. In this work, the Godiva IV assembly will be used because it is a fast system capable of producing a wide range of source strengths, including super-prompt critical bursts. The room return for the facility is expected to be substantial and challenging to characterize, so a more closed, shielded experimental configuration is considered. Furthermore, because the physics of radiation transport outside the assembly does not change between the burst mode and the delayed critical mode, it is anticipated that most measurements will be made with the Godiva IV assembly in delayed critical mode, operating within a range that will allow electronic counters to collect accurate data. Scoping calculations concluded that a workable room return shield is comprised of 40 cm of 5% borated polyethylene backed by 7 cm of lead. This configuration was shown to produce a ratio of signal–to–room return of over 100 for up to 2 mean free paths of shield sample material, and over 10 for up to 4 mean free paths of shield sample material, ensuring that useful results can be obtained. With no shielding sample in the room return shield, it was shown that the neutron and gamma spectra do not appreciably change with a change in room size. This scoping calculation does not preclude the use of tungsten powder in a binder, some other effective gamma shielding material, or a hybrid design. Dose rates for various source intensities at an unshielded detector are listed herein to inform detector selection during CED-2, and calibration chains are identified. Preliminary estimates of costs and schedules are outlined but remain to be verified. Values could double or triple as estimates become more accurate and are principally included here to demonstrate feasibility. Preliminary estimates indicate that the apparatus can be installed within a feasible schedule and budget. Two measurements per day are assumed. Producing a shielding benchmark at NCERC using the Godiva IV assembly has been shown to be feasible, with manageable uncertainties and risks. A clear, continuing need for shielding benchmark data remains present, and this report identifies and evaluates a method for creating integrated shielding benchmark datasets.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
NASA NTRS2019

New Perspectives of Ancient Mars: Mineral Diversity and Crystal Chemistry at Gale Crater, Mars from the CheMin X-Ray Diffractometer

The Mars Science Laboratory Curiosity rover arrived at Mars in August 2012 with a primary goal of characterizing the habitability of ancient and modern environments. Curiosity landed in Gale crater to study a sequence of ~3.5 Ga old sedimentary rocks that, based on orbital visible/near-infrared reflectance spectra, contain secondary minerals that suggest deposition and/or alteration in liquid water. The sedimentary sequence that comprises the lower slopes of Mount Sharp within Gale crater may preserve a dramatic shift on early Mars from a relatively warm and wet climate to a cold and dry climate based on a transition from smectite-bearing strata to sulfate-bearing strata. The rover is equipped with cameras and geochemical and mineralogical instruments to examine the sedimentology and identify compositional changes within the stratigraphy. These observations provide information about variations in depositional and diagenetic environments over time. The Chemistry and Mineralogy (CheMin) instrument is one of two internal laboratories on Curiosity and includes a transmission X-ray diffractometer (XRD) and X-ray fluorescence (XRF) spectrometer with a Co-K source. CheMin measures loose sediment samples scooped from the surface and drilled rock powders. The XRD provides quantitative mineralogy of scooped and drilled samples to a detection limit of ~1 wt.%. Curiosity has traversed >20 km since landing and has primarily been exploring the site of a predominantly ancient lake environment fed by groundwater and streams emanating from the crater rim. Results from CheMin demonstrate an incredible diversity in the mineralogy of fluvio-lacustrine rocks that signify variations in source rock composition, sediment transport mechanisms, and depositional and diagenetic fluid chemistry. Abundant trioctahedral smectite and magnetite at the base of the section may have formed from low-salinity pore waters with a circumneutral pH within lake sediments. A transition to dioctahedral smectite, hematite, and Ca-sulfate going up section suggests a change to more saline and oxidative aqueous conditions within the lake waters themselves and/or within diagenetic fluids. The primary minerals detected in fluvio-lacustrine samples by CheMin also suggest diversity in the igneous source regions for the sediments, where abundant pyroxene and plagioclase in most samples suggest a basaltic protolith, but sanidine and pyroxene in one sample may have been sourced from a potassic trachyte, and tridymite and sanidine in another sample may have been transported from a rhyolitic source. Crystal chemistry of major phases in each sample have been calculated from refined unit-cell parameters, providing further constraints on aqueous alteration processes and igneous protoliths for the sediments. Perhaps one of the biggest mysteries revealed by the CheMin instrument is the high abundance of X-ray amorphous materials (15 to 73 wt.%) in all samples measured to date. X-ray amorphous materials were detected by CheMin based on the observation of broad humps in XRD patterns. How these materials formed, their composition, and why they persist near the martian surface remain a topic of debate. The sedimentology and composition of the rocks analyzed by Curiosity demonstrate that habitable environments persisted intermittently on the surface or in the subsurface of Gale crater for perhaps more than a billion years.

Rampe, E. B.↗
DOE OSTI2021

Microscopic ejecta measurements from hypervelocity impacts on aluminum and powdered regolith targets

Meteoroids and space debris pose a two-fold threat to spacecraft due to the risk of both mechanical damage from the impact and electrical damage from the impact-generated plasma, which produces electromagnetic emissions. Analysis of impact products, however, has the potential to provide useful information about planetary rings and small solar system bodies, such as asteroids and comets. Understanding the plasma dynamics and radiation mechanism is essential to addressing the impact threat and extracting science data from impacts. Charge attachment to condensed-phase debris may lead to a dusty plasma under certain conditions, so interpreting hypervelocity impacts requires knowledge of both the nature of the plasma and of the ejecta. We address the latter with measurements of the microscopic ejecta distribution produced by light gas gun impacts on solid aluminum and powdered regolith simulant targets. We examine both the size and shape of the ejecta using thin-film witness plates and find that the size distributions of microscopic ejecta follow power laws. Observations from the powdered regolith simulant match well with disruption experiments of solid basalt, while measurements from the aluminum impacts diverge from extrapolations based on studies of macroscopic debris. Analysis of the ejecta shape shows a transition from smooth to irregularly shaped ejecta at the material grain size, and the shape of debris may provide insight on the phase of the ejected material. Finally, based on our results, we predict a significant number of secondary impacts on plasma sensors due to ejecta, even at considerable distance from the target, supporting the hypothesis that charged dust affects plasma measurements in the ejecta curtain.

42 ENGINEERING↗
DOE OSTI2022

Unexpected features in the optical vibrational spectra of δ-UO 3

Uranium trioxide displays a complex chemical phase space, with at least six structurally distinct polymorphs accessible via different synthetic routes. Remarkably, despite its technological importance, full structural and electronic characterization of these polymorphs remains an open area of study. δ-UO 3 in particular has attracted significant theoretical attention due to its high point group and space group symmetries, having U (VI) in octahedral coordination with polyhedra interconnected through corner-sharing to build a 3-D cubic lattice with space group symmetry Pm-3m and Z = 1. Critical experimental information, such as its optical vibrational spectra, are not known. Here, we study the Raman and infrared (IR) spectra of δ-UO 3 together with the support of density functional theory (DFT) calculations for spectral interpretation. A symmetry analysis of the DFT-predicted phonon eigenmodes indicates that δ-UO 3 should have two IR active modes and no Raman active modes. Experimental results, however, indicate significant Raman scattering from δ-UO 3 . We therefore propose four potential explanations for this apparent contradiction: a possible tetragonal distortion to the cubic cell, the existence of a surface impurity layer, vacancy scattering, and structural activation of Raman signal. We use powder X-ray diffraction and confocal Raman spectroscopy with depth profiling to investigate these possibilities and suggest future experiments to explore this phenomenon in more detail. Understanding the lattice dynamics of δ-UO 3 is important for identification of technogenic U phases via Raman and infrared spectroscopy and our results indicate that the simple understanding of δ-UO 3 as a high-symmetry cubic structure should be reconsidered.

98 NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL P↗
NASA NTRS2000

SEM Characterization of Extinguished Grains from Plasma-Ignited M30 Charges

M30 propellant grains that had been ignited in interrupted closed bomb experiments were characterize by scanning electron microscopy (SEM). Previous chemical analysis of extinguished grains had given no indications of plasma-propellant chemical interactions that could explain the increased burning rates that had been previously observed in full-pressure closed bomb experiments. (This does not mean that there is no unique chemistry occurring with plasma ignition. It may occur very early in the ignition event and then become obscured by the burning chemistry.) In this work, SEM was used to look at grain morphologies to determine if there were increases in the surface areas of the plasma-ignited grains which would contribute to the apparent increase in the burning rate. Charges were made using 30 propellant grains (approximately 32 grams) stacked in two tiers and in two concentric circles around a plastic straw. Each grain was notched so that, when the grains were expelled from the bomb during extinguishment, it could be determined in which tier and which circle each grain was originally packed. Charges were ignited in a closed bomb by either a nickel wire/Mylar-capillary plasma or black powder. The bomb contained a blowout disk that ruptured when the pressure reached 35 MPa, and the propellant was vented into a collection chamber packed with polyurethane foam. SEM analysis of the grains fired with a conventional black powder igniter showed no signs of unusual burning characteristics. The surfaces seemed to be evenly burned on the exteriors of the grains and in the perforations. Grains that had been subjected to plasma ignition, however, had pits, gouges, chasms, and cracks in the surfaces. The sides of the grains closest to the plasma had the greatest amount of damage, but even surfaces facing the outer wall of the bomb had small pits. The perforations contained gouges and abnormally burned regions (wormholes) that extended into the web. The SEM photos indicated that a grain from the top tier, which was farther away from the plasma ignition source, sustained more plasma-induced damage to the perforations and the web than did the grains on the bottom tier.

Kinkennon, A.↗
NASA NTRSDate not supplied

Additional Trials & Tribulations in Synthesizing a Sulfide Standard

Well-characterized sulfide reference materials that can serve as matrix-matched calibrants for in-situ trace element analyses via laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) remain elusive. Here, we describe the creation an in-house sulfide standard at NASA JSC that will be used to measure siderophile and chalcophile trace elements in low pressure experimental products, specifically pentlandite ([FeNi]9S8) and pyrrhotite ([FeNi]1-xS), as well as natural sulfides in terrestrial and meteoritic mineral assemblages. Recent methods in creating a homogenous sulfide standard include pressed pellets, synthesized chips, or fused glass [e.g. 1-3]. Other studies, however, have had success in forming homogenous FeS standards via synthesization methods [e.g. 4-6]. We present a variation of the method described in [4], in which we create a pyrrhotite standard doped with a variety of trace elements (Zn, As, Se, Mo, Ru, Rh, Pd, Sn, Sb, Te, W, Os, Ir, Pt, Au) at ~10-40 ppm and Cu at ~200 ppm. Sulfide compositions were constructed using Fe and Ni metal and elemental sulfur powders. Trace elements were added to elemental sulfur from Atomic Absorption Spectroscopy (AAS) elemental standards as either nitrate or chloride solutions to prevent oxidation of the metal powders. The dried sulfur mixture was mixed with Fe and Ni powders and mechanically mixed before two aliquots were placed in separate SiO2 tubes. Each tube was held under vacuum for ~30 minutes, sealed under vacuum, and then heated at 800C for 48 hours. Like [4], the synthesis products were composed of pourous sulfide crystals. Major element analyses of both experimental aliquots, collected using an Electron Probe Microanalyser (EPMA), yield indistinguishable major element compositions (uncertainties in 2SE & 2RSE[%]), with an average of 57.90  0.09 (0.16 %), 4.95  0.03 (0.55 %), and 39.70  0.14 (0.34 %), for Fe, Ni, and S, respectively. Trace element data were measured using a Photon Machines 193nm laser ablation system coupled to a Thermo-Scientific Element-XR ICP-MS. Spot sizes were limited to 50 μm due to the porous nature of the sulfide target material. Trace element abundances, normalized to Fe as an internal standard, were also found to be homogenous between the two aliquots, with weighted mean 2RSE (%) values of <3.0 for all trace elements. Synthesized products were re-powdered and absolute concentrations measured via solution ICP-MS. Although the sulfide appears to be homogenous, sintering experiments will be performed to more closely match the standard density to natural sulfides and minimize differences in ablation behavior. Improved density also allows for higher sensitivity (i.e. more compact target material) and larger spot sizes or traverses, as void space is eliminated. Additional major and trace element analyses on the products of the sintering experiments will be undertaken.

Jacob B Setera↗