SEARCH · Engineering Papers

Results for “Powder Removal”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

SourceResearch connectionFrom yearThrough year

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 235 records · Page 13

All sources NASA NTRS DOE OSTI

DOE OSTI2025

Size and Structural Control of Mechanoluminescent ZnS:Mn 2+ Nanocrystals for Optogenetic Neuromodulation

Mechanoluminescent materials hold immense potential for various transformative applications, from medical imaging and diagnostics to health monitoring and wearable displays. Conventionally produced as bulk powders or microparticles, they face significant size limitations for advanced applications, particularly in biological systems and microscale devices. Here, this work presents an approach to ZnS:Mn 2+ nanocrystal synthesis that involves self-assembly and subsequent calcination. In addition to effective size control within the nanoscale, this approach promotes the formation of abundant stacking faults, significantly enhancing piezoelectric and mechanoluminescent properties by increasing trap density and reducing trap depth. Unlike mechanoluminescent materials produced using conventional methods, these nanocrystals demonstrate strong mechanoluminescence without requiring UV pre-excitation, and the light emission persists even after mechanical stress is removed. These advantageous properties make them promising candidates for optogenetic neuromodulation, as they can effectively trigger electrical signals in neurons upon ultrasound stimulation both with and without UV pre-excitation. The persistent mechanoluminescence prolongs the duration of neuronal electrical activity, providing an extended temporal window for neuromodulation compared to conventional mechanoluminescent materials. This study provides a scalable method for producing efficient mechanoluminescent nanoparticles and reveals the crucial role of particle size and defect structures in determining their mechanoluminescent behavior.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

Testing of Helium Cooled Metal Molybdenum Disk Target System

NorthStar Medical Radioisotopes LLC is planning to produce the important medical radioisotope molybdenum-99 (Mo-99) through a photonuclear reaction on molybdenum-100 (Mo-100). In this approach, multiple thin disks of enriched molybdenum metal will be bombarded with a 40-MeV electron beam. Because enriched Mo-100 is expensive, we intend to use as much beam power as possible to achieve maximum production yield and minimize the size of the target. This requirement leads to very high beam power density (heat deposition in the target), which sets challenging requirements for cooling. Together with scientists at Los Alamos National Laboratory, a team at Argonne National Laboratory has developed and demonstrated a cooling approach using pressurized helium, which allows for efficient heat removal. One of the challenges in this approach is the management of the heat load on the target window. The target window separates the high-pressure helium atmosphere inside the target from the vacuum in the beamline, so it is constantly under stress from differential pressure. Also, the window is cooled only by the helium gas flow from one side, making the window design challenging. High heat deposition in the target disks also imposes a strict requirement on performance of the helium cooling system and thickness of the target disks. The target disks are produced from metal powder via a press-and-sinter process. The resulting disks do not possess as high a tensile strength as solid molybdenum and might not survive the vibration from the high-velocity helium coolant and the high thermal stress from beam heating.

42 ENGINEERING↗

NASA NTRS1995

Cratering and penetration experiments in Teflon targets at velocities from 1 to 7 km/s

Approximately 20 sq m of protective thermal blankets, largely composed of Teflon, were retrieved from the Long Duration Exposure Facility (LDEF) after the spacecraft had spent approximately 5.7 years in space. Examination of these blankets revealed that they contained thousands of hypervelocity impact features ranging from micron-sized craters to penetration holes several millimeters in diameter. We conducted impact experiments in an effort to reproduce such features and to -- hopefully -- understand the relationships between projectile size and the resulting crater or penetration-hole diameter over a wide range of impact velocity. Such relationships are needed to derive the size- and mass-frequency distribution and flux of natural and man-made particles in low-Earth orbit. Powder propellant and light-gas guns were used to launch soda-lime glass spheres of 3.175 mm (1/8 inch) nominal diameter (Dp) into pure Teflon FEP targets at velocities ranging from 1 to 7 km/s. Target thickness (T) was varied over more than three orders of magnitude from infinite halfspace targets (Dp/T less than 0.1) to very thin films (Dp/T greater than 100). Cratering and penetration of massive Teflon targets is dominated by brittle failure and the development of extensive spall zones at the target's front and, if penetrated, the target's rear side. Mass removal by spallation at the back side of Teflon targets may be so severe that the absolute penetration-hole diameter (Dh) can become larger than that of a standard crater (Dc) at relative target thicknesses of Dp/T = 0.6-0.9. The crater diameter is infinite halfspace Teflon targets increases -- at otherwise constant impact conditions -- with encounter velocity by a factor of V0.44. In contrast, the penetration-hole size is very thin foils (Dp/T greater than 50) is essentially unaffected by impact velocity. Penetrations at target thicknesses intermediate to these extremes will scale with variable exponents of V. Our experimental matrix is sufficiently systematic and complete, up to 7 km/s, to make reasonable recommendations for the velocity-scaling of Teflon craters and penetrations. We specifically suggest that cratering behavior and associated equations dominate all impacts in which the shock-pulse duration of the projectile (tp) is shorter than that of the target (tt). We also demonstrate that each penetration hole from space-retrieved surfaces may be assigned a unique projectile size, provided an impact velocity is known or assumed. This calibration seems superior to the traditional ballistic-limit approach.

Hoerz, Friedrich↗

DOE OSTI2024

Testing of Helium-Cooled Metal Molybdenum Disk Target

NorthStar Medical Radioisotopes LLC is planning to produce an important medical radioisotope, molybdenum-99 (Mo-99), through photonuclear reaction on molybdenum-100 (Mo-100). In this approach, molybdenum metal will be bombarded with a 40-MeV electron beam. Because enriched Mo-100 is expensive, it is desired to use as much beam power as possible to achieve maximum production yield and minimize target mass. This objective leads to very high beam power density (heat deposition in the target), which sets challenging requirements for cooling. Together with scientists at Los Alamos National Laboratory, a team at Argonne National Laboratory has developed and demonstrated a cooling approach using pressurized helium, which allows for efficient heat removal. One of the main challenges in this approach is the management of the heat load on the target window. The target window separates the high-pressure helium inside the target from the vacuum in the beamline, so it is constantly under stress from differential pressure. Also, the window is cooled only by the helium gas flowing on one side, making the window cooling even more challenging. High heat deposition in the target disks also imposes a strict requirement on performance of the helium cooling system and thickness of the target disks. The target disks are produced from metal powder via a press-and-sinter process. The resulting disks do not possess tensile strength as high as solid molybdenum and might not survive the vibration from the high-velocity helium coolant and high thermal stress from beam heating. An Argonne team of scientists performed a series of tests at Argonne’s Low Energy Accelerator Facility (LEAF) [3-7]. This report describes two series of tests for scale down production target designs that utilize full-scale 29 millimeters diameter, 0.75 mm thick press-and-sintered disks. We performed two thermal tests with different beam parameters and configurations of the disk laminations. We compared the results of the window temperature measurements and cooling system parameters obtained in the experiments with those predicted by analytical calculations and Computation Flow Dynamic (CFD) simulations. Results of the experiments and calculations are presented below.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Effect of stress and temperature on zero group velocity Lamb modes

Zero group velocity (ZGV) Lamb wave resonances are highly localized and sensitive to changes in material properties, making them a viable option for probing residual stresses and elastic nonlinearity through acoustoelastic effects. Temperature changes also influence ZGV modes and need to be accounted for, particularly when measuring the small frequency shifts associated with acoustoelastic effects. We use a laser-based ultrasonic system to measure the third-order elastic constants of several materials. A temperature compensation scheme is devised to remove the effects of temperature fluctuations from the measurements. Furthermore, the measured third-order elastic constants are used to predict the temperature dependence of the ZGV resonances using thermo-acoustoelasticity theory, and these predictions are compared to experimental measurements. We find that thermo-acoustoelasticity theory was unable to reliably predict the shift in ZGV resonances with temperature. These results could have important implications in understanding the limitations of thermo-acoustoelasticity theory and in developing precision ZGV resonance-based systems to detect and quantify residual stress in parts, a particularly relevant problem in additive manufacturing techniques including powder bed fusion and directed energy deposition.

Engineering↗

DOE OSTI2024

Characterization Techniques Investigated for Characterization of Anomalous Materials in Plutonium Oxide – 25666

The DOE has adopted a Dilute and Dispose approach for processing surplus plutonium which consists of blending plutonium oxide with adulterants and packaging it in a form which is acceptable for disposal at the Waste Isolation Pilot Plant. The feed material for the downblend process is intended to be pure plutonium oxide powder, however other objects are occasionally encountered within the oxide, particularly with legacy material. Potential technologies which could assist in the resolution of incidents where such anomalies are encountered have been investigated. Resolution of these incidents requires characterization of the anomalous object so that plutonium oxide processing can resume and so that a disposition pathway can be determined for the anomalous material. Technologies including gamma ray spectroscopy, alpha-gamma coincidence, LiDAR volumetric measurements, and surface conductivity measurements were investigated for this purpose, with a focus on systems which can be easily introduced into the processing environment when an anomaly is encountered, then removed from the environment after resolution to avoid impeding normal processing activities. This places an emphasis on small and portable measurement systems and systems that can operate in a high-background, oxide-processing environment. Gamma ray systems investigated include the GR1™a CZT detector and the MicroGe™a germanium detector, with a focus on detecting characteristic gamma rays from Pu-239 and other actinides. A gamma ray and alpha particle coincidence method was investigated with the goal of identifying actinides in the presence of a gamma ray background produced by adjacent plutonium oxide material. Leica™b BLK360 G1 and Keyence™c LJ-X8300 LiDAR systems were investigated for use in conjunction with mass measurements to gain accurate material density values, and a Foerster Sigmatest™d 2.070 was tested to determine surface conductivity. The combination of these properties would allow improved identification and characterization of a wide variety of potential anomalous material.

Munson, Justin M.↗

NASA NTRS1977

Low-temperature thermionic emitter

An improved photodelineatable cathode material is disclosed comprising a combination of triple carbonate (TC) and a hydrocarbon polymeric photoresist PR. A mixture of TC powder and PR is applied to a cathode by spraying, spinning or dipping and is then subjected to activation at a temperature from about 800.degree. C up to the melting temperature. The cathodes can be activated at a temperature as low as 800.degree. C and still deliver a 0-field, temperature-limited current density of 750 milliamperes per sq. centimeter at 600.degree. C. If a pattern is desired, the coating is exposed through a suitable mask to actinic light to harden the photoresist in the desired areas. Following exposure, the exposed image areas are developed and the unexposed portions of the coating are removed with solvent. When dry, the cathode is ready for activation.

Remington, Richard W.↗

DOE OSTI2021

Cs absorption capacity and selectivity of crystalline and amorphous Hf and Zr phosphates

Removal of radioactive Cs from sodium-rich solutions is a technical challenge that goes back to post World War II nuclear waste storage and treatment; and interest in this topic was reinvigorated by the Fukushima-Daiichi nuclear power plant disaster, 10 years ago. Since the 1960's there has been considerable focus on layered Zr phosphates as robust inorganic sorbents for separation of radionuclides such as Cs. Here we present synthesis and characterization, and direct comparison of Cs sorption capacity and selectivity of four related materials: 1) crystalline α-Zr phosphate and α-Hf phosphate, and 2) amorphous analogues of these. Powder X-ray diffraction, thermogravimetry, solid-state 31P magic angle spinning nuclear magnetic resonance (MAS-NMR) spectroscopy, and compositional analysis (inductively coupled plasma optical emission spectroscopy and mass spectroscopy, ICP OES and ICP MS) provided formulae; respectively M(HPO4)2∙1H2O and M(HPO4)2∙4H2O (M = Hf, Zr) for crystalline and amorphous analogues. Maximum Cs loading, competitive Cs-Na selectivity and maximum Cs-Na loading followed by the above characterizations plus 133Cs MAS-NMR spectroscopy revealed that amorphous analogues are considerably better Cs-sorbents (based on maximum Cs-loading and selectivity over Na) than the well-studied crystalline Zr-analogue. Additionally, crystalline α-Hf phosphate is better Cs-sorbent than crystalline α-Zr phosphate. All these studies consistently show that Hf phosphate is less crystallize than Zr phosphate, when obtained under similar or identical synthesis conditions. We attribute this to lower solubility of Hf phosphate compared to Zr phosphate, preventing ‘defect healing’ during the synthesis process.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1997

Transpiring Cooling of a Scram-Jet Engine Combustion Chamber

The peak cold-wall heating rate generated in a combustion chamber of a scram-jet engine can exceed 2000 Btu/sq ft sec (approx. 2344 W/sq cm). Therefore, a very effective heat dissipation mechanism is required to sustain such a high heating load. This research focused on the transpiration cooling mechanism that appears to be a promising approach to remove a large amount of heat from the engine wall. The transpiration cooling mechanism has two aspects. First, initial computations suggest that there is a reduction, as much as 75%, in the heat flux incident on the combustion chamber wall due to the transpirant modifying the combustor boundary layer. Secondly, the heat reaching the combustor wall is removed from the structure in a very effective manner by the transpirant. It is the second of these two mechanisms that is investigated experimentally in the subject paper. A transpiration cooling experiment using a radiant heating method, that provided a heat flux as high as 200 Btu/sq ft sec ( approx. 234 W/sq cm) on the surface of a specimen, was performed. The experiment utilized an arc-lamp facility (60-kW radiant power output) to provide a uniform heat flux to a test specimen. For safety reasons, helium gas was used as the transpirant in the experiments. The specimens were 1.9-cm diameter sintered, powdered-stainless-steel tubes of various porosities and a 2.54cm square tube with perforated multi-layered walls. A 15-cm portion of each specimen was heated. The cooling effectivenes and efficiencies by transpiration for each specimen were obtained using the experimental results. During the testing, various test specimens displayed a choking phenomenon in which the transpirant flow was limited as the heat flux was increased. The paper includes a preliminary analysis of the transpiration cooling mechanism and a scaling conversion study that translates the results from helium tests into the case when a hydrogen medium is used.

Choi, Sang H.↗

NASA NTRS2008

Photocatalytic Coatings for Exploration and Spaceport Design

This project developed self-cleaning photocatalytic coatings that remove contamination without human intervention. The coatings chemically remove organic contaminants and leave no residue. The photocatalyst will not negatively affect other coating properties, especially corrosion resistance. Titanium dioxide, TiO2, is an extremely popular photocatalyst because of its chemical stability, nontoxicity, and low cost. TiO2 is commonly used in the photocatalytic oxidation of organic matter or pollutants in the gas and liquid phases. However, TiO2 does have some drawbacks. It has limited light absorption because of its large band-gap and suffers from a photonic efficiency of less than 10 percent for organic degradation. Dopants can lower the band-gap and improve efficiency. Since the photocatalytically active form of TiO2 is a nanocrystalline powder, it can be difficult to make a robust coating with enough catalyst loading to be effective. Photocatalysts become active when certain light energy is absorbed. When photons with an energy greater than the band-gap, Eg, (wavelengths shorter than 400 nm) impinge upon the surface of the TiO2, an electron-hole pair is formed. The electron-hole pair oxidizes adsorbed substances either directly or via reactive intermediates that form on the surface, such as hydroxyl radicals (OH) or superoxide ions (O2-). Several factors can influence the band-gap energy of TiO2, two of which are crystal structure and impurities. TiO2 exists as three crystal structures brookite, anatase, and rutile that can be controlled via heat treatment. Anatase is the most photocatalytically active crystal form of TiO2. Doping TiO2 with impurities can alter its band-gap energy, as well as its effectiveness as a catalyst. Depending on their size, dopant atoms can occupy either the substitutional or interstitial lattice positions. Atoms that are relatively large will assume the interstitial positions and create a much greater energy disturbance in the crystal than will smaller atoms that take on the substitutional positions. This energy disturbance narrows the band-gap and thus allows photons with longer wavelengths and smaller energies (such as those in the visible-light spectrum) to create electron-hole pairs. Raman spectroscopy was performed for the purpose of determining the crystal structure and the degree of crystallinity of the TiO2 particles. Reflectance measurements indicated the wavelengths of light absorbed by the different catalysts.

Source record↗

DOE OSTI2022

Models to Incorporate Reaction Mechanisms into DG-OSPREY: Fixed-Bed Simulations for Organic Iodides Capture Using Ag 0 Z

As one of the most potent radioisotopes released during spent nuclear fuel reprocessing, 129 I is strictly regulated and must be removed before discharge. Organic iodides (primarily alkyl iodides with different chain lengths, i.e., CH 3 I, C 4 H 9 I, and C 12 H 25 I) comprise ~2% of the total iodine in the reprocessing off-gases and are primarily present in vessel off-gas (VOG). Reduced silver mordenite (Ag 0 Z) is predominantly considered for the removal of radioiodine; however, its capture performance and underlying interaction processes with long-chain organic iodides are not fully understood. Two major tasks were accomplished in this study. First, to improve upon the previous experimental studies where Ag 0 Z was used to capture CH 3 I, C 4 H 9 I, and C 12 H 25 I at different concentrations, we comprehensively investigated the corresponding capture mechanisms by characterizing fully loaded Ag 0 Z samples. Second, computational codes were implemented to perform fixed-bed simulations that account for transport and reaction mechanisms. Scanning electron microscopy with energy dispersive X-ray analysis (SEM-EDX), powder X-ray diffraction (PXRD), UV-visible diffuse reflectance spectroscopy (UV-vis DRS), and thermogravimetric analysis (TGA) were conducted on Ag 0 Z samples that are saturated with I 2 , CH 3 I, C 4 H 9 I, and C 12 H 25 I), respectively. Results indicate that AgI is the predominant adsorption product regardless of the adsorbed iodine species, yet alkyl iodides with different carbon chain lengths may have different compositions of α- and γ-AgI. Synchrotron pair distribution function (PDF) measurements and TGA coupled with a Fourier transformed infrared detector (TGA FTIR) have been performed, and experimental data are currently analyzed. Results are expected to provide further insights into the adsorption mechanisms. The fixed-bed capture performance for CH 3 I was successfully simulated by solving mathematical equations that describe the underlying transport processes and adsorption reactions. The computational framework, Catalytic After Treatment System (CATS), that was originated in our research group, was used to solve the governing equations. Kinetic parameters, including the pore diffusivity and reaction rate constant were obtained by optimization techniques using data from thin-bed experiments performed at Oak Ridge National Laboratory. The performance of a deep bed predicted using the optimized parameters showed promising agreement with the experimental data.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

NASA NTRSDate not supplied

Additive Manufacturing and Experimental Characterization of Nickel-Titanium Shape-Memory Alloy Wick Structures and Heat Pipes for Spacecraft Thermal Control

Shape memory alloys (SMA), such as those based on nickel-titanium (NiTi), are increasingly being applied as multifunctional spacecraft components. For thermal management applications, NiTi flow tubing hinges and self-deploying loop heat pipes have been demonstrated. Emerging additive manufacturing (AM) processes are enabling more complex SMA devices than can be formed from conventional plain wire, tubing, and sheet stock materials. This paper presents our progress toward applying powder bed fusion AM to producing porous NiTi wicks and NiTi-H2O heat pipes, which could be embedded in thermally deploying radiators for spacecraft thermal management. AM near-equiatomic NiTi (55.1 wt% Ni) porous wick specimens were produced with a range of deposition parameters. Transient acetone rate-of-rise experiments were performed to estimate wick permeability (K) and average pore radius (r_pore) values and identify parameter sets with high capillary performance. Surface treatments were evaluated to achieve hydrophilic wick structures. Evaluated treatments included chemical oxide growth with H2O2, oxide and sodium titanate growth with NaOH solution, and ultrasonic cleaning with specialty detergents that can remove hydrocarbon contaminants. The most durable hydrophilic surface conditions were obtained with the NaOH treatment. High performing wick deposition parameters were used to produce a full AM NiTi heat pipe, which was treated with NaOH solution to activate the wick. This heat pipe was operated on a test stand in the inverted configuration (upper evaporator and lower condenser), and demonstrated stable nearly isothermal operation for 150 hrs.

Thermal management↗

NASA NTRSDate not supplied

Additive Manufacturing and Experimental Characterization of Nickel-Titanium Shape-Memory Alloy Wick Structures and Heat Pipes for Spacecraft Thermal Control

Thermal management↗

NASA NTRS1981

Photoproduction of I2, Br2, and Cl2 on n-semiconducting powder

The photosynthetic production of Br2 and Cl2 and the photocatalytic production of I2 from aqueous solutions of the respective halide ions in the presence of platinized semiconducting n-TiO2 powder are reported. Reactions were produced in 2-3 M oxygen-saturated aqueous solutions of KI, KBr or NaCl containing Pt-TiO2 powder which were irradiated by a high-pressure mercury lamp at a power of 400 mW/sq cm. Halogens are found to be produced in greater quantities when platinized TiO2 powders are used rather than pure TiO2, and rates of halogen production are observed to increase from Cl2 to Br2 to I2. The presence of the synthetic reactions producing Br2 and Cl2 with a net influx of energy indicates that an effective separation of the photoproduced electron-hole pair occurs in the semiconductor. Quantum efficiencies of the reaction, which increase with decreasing solution pH, are found to be as high as 30%, implying a solar-to-chemical energy conversion efficiency between 0.03% and 3% for the case of chlorine production. It is concluded that the photoproduction of halogens may be of practical value if product halogens are efficiently removed from the reaction cell.

Reichman, B.↗

DOE OSTI2024

High-pressure synthesis and neutron scattering study of tantalum hydride TaH 1.23(5) and a tantalum polymorph with A15-type structure

A unique type of tantalum hydride was synthesized by exposing tantalum dihydride to the high hydrogen pressure of 9 GPa and a temperature of using toroid-type high-pressure chambers. The samples of this hydride were cooled down to 100 K, recovered to ambient pressure, and studied in a metastable state by hot extraction, powder x-ray and neutron diffraction, and inelastic neutron scattering. X-ray diffraction demonstrated that this hydride had an A15-type crystal structure of metal lattice (space group , Ta atoms at the 2a and 6c Wyckoff positions) and a lattice parameter of a = 5.150(5) Å at T = 85 K. The hydrogen content determined by hot extraction was H/Ta - 1.23(5). Hydrogen desorption during heating the sample in vacuum proceeded in two steps—first, Δ⁢H⁡/Ta=0.2 was desorbed at around -70 °⁢C, and then the rest of the hydrogen was desorbed between 100 ⁢°C and 390 ⁢°⁢C. The A⁢15-type metal lattice was preserved upon hydrogen removal, leaving a unique polymorph of tantalum. Neutron diffraction of A⁢15-TaH 1.23⁢(5) demonstrated that hydrogen atoms occupy the 24⁢k and 16⁢i Wyckoff sites in the crystal structure, and annealing at 250 K resulted in a decrease of the 24⁢k and an increase of the 16⁢i site occupancies. Inelastic neutron scattering revealed four vibrational modes in the fundamental band of A⁢15-TaH 1.23⁢(5) at 72, 135, 145, and 166 meV, the first three and the last one of which were tentatively assigned to the vibrations of H atoms at the 24⁢k and 16⁢i sites, respectively. No superconductivity was found in A⁢15-TaH 1.1 and hydrogen-free A15-Ta at temperatures down to 1.5 K.

36 MATERIALS SCIENCE↗

NASA NTRS2004

Composite-Material Tanks with Chemically Resistant Liners

Lightweight composite-material tanks with chemically resistant liners have been developed for storage of chemically reactive and/or unstable fluids . especially hydrogen peroxide. These tanks are similar, in some respects, to the ones described in gLightweight Composite-Material Tanks for Cryogenic Liquids h (MFS-31379), NASA Tech Briefs, Vol. 25, No. 1 (January, 2001), page 58; however, the present tanks are fabricated by a different procedure and they do not incorporate insulation that would be needed to prevent boil-off of cryogenic fluids. The manufacture of a tank of this type begins with the fabrication of a reusable multisegmented aluminum mandrel in the shape and size of the desired interior volume. One or more segments of the mandrel can be aluminum bosses that will be incorporated into the tank as end fittings. The mandrel is coated with a mold-release material. The mandrel is then heated to a temperature of about 400 F (approximately equal to 200 C) and coated with a thermoplastic liner material to the desired thickness [typically approxiamtely equal to 15 mils (approximately equal to 0.38 mm)] by thermal spraying. In the thermal-spraying process, the liner material in powder form is sprayed and heated to the melting temperature by a propane torch and the molten particles land on the mandrel. The sprayed liner and mandrel are allowed to cool, then the outer surface of the liner is chemically and/or mechanically etched to enhance bonding of a composite overwrap. The etched liner is wrapped with multiple layers of an epoxy resin reinforced with graphite fibers; the wrapping can be done either by manual application of epoxy-impregnated graphite cloth or by winding of epoxy-impregnated filaments. The entire assembly is heated in an autoclave to cure the epoxy. After the curing process, the multisegmented mandrel is disassembled and removed from inside, leaving the finished tank. If the tank is to be used for storing hydrogen peroxide, then the liner material should be fluorinated ethylene/propylene (FEP), and one or more FEP O ring(s) should be used in the aluminum end fitting(s). This choice of materials is dictated by experimental observations that pure aluminum and FEP are the only materials suitable for long-term storage of hydrogen peroxide and that other materials tend to catalyze the decomposition of hydrogen peroxide to oxygen and water. Other thermoplastic liner materials that are suitable for some applications include nylon 6 and polyethylene. The processing temperatures for nylon 6 are lower than those for FEP. Nylon 6 is compatible with propane, natural gas, and other petroleum-based fuels. Polyethylene is compatible with petroleum- based products and can be used for short-term storage of hydrogen peroxide.

DeLay, Thomas K.↗

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↗

DOE OSTI2020

Characterization and CST Batch Contact Equilibrium Testing of Modified Tank 9H Process Supernate Samples in Support of TCCR

The Tank Closure Cesium Removal (TCCR) system uses ion exchange columns filled with crystalline silicotitanate (CST) media to process radioactive waste solutions for the removal of ¹³⁷Cs. TCCR currently focuses on dissolving Savannah River Site (SRS) radioactive tank waste (primarily sodium saltcake solids) within Tank 10H followed by at-tank ion exchange column treatment. Two supernate batches from Tank 10H have been processed through the TCCR unit and processing of a third batch is expected soon. After processing of this supernate batch, plans are to replace the CST columns and process dissolved salt solution from Tank 9H through Tank 10H and then through the new CST columns installed in the TCCR unit. The new columns are expected to contain either a media similar to an archived CST batch (IE-911) or the R9120-B CST media used in the current TCCR columns (the two materials are fundamentally the same; just different specifications, product names, and preconditioning steps). Samples of Tank 9H dissolved saltcake were received at the Savannah River National Laboratory (SRNL) and characterized. The Tank 9H supernate contained a high sodium concentration (~9.6 M Na⁺) and will require dilution to near 6 M [Na⁺] prior to processing through the TCCR unit. The cesium concentration in Tank 9H is currently significantly higher than was observed with Tank 10H. Three dilutions of the Tank 9H supernate were conducted to mimic possible dilutions that could be conducted in the tank farm prior to TCCR processing using inhibited water, sodium hydroxide, and sodium nitrate solutions. Dilution #1 was prepared by diluting the Tank 9H supernate by a factor of 1.6 with inhibited water, Dilution #2 was prepared by diluting the Tank 9H supernate by a factor of 3.7 with a mixed sodium hydroxide/sodium nitrate diluent, and Dilution #3 was prepared by also diluting by a factor of 3.7 but with sodium hydroxide only. All three dilutions have similar Na⁺ concentrations (~6 M), but Dilutions #2 and #3 contain significantly less cesium. Major and key minor components of the diluted Tank 9H supernate samples are provided in Table ES-1. Batch contact equilibrium tests were conducted with the Tank 9H dilutions and the two different CST media batches being considered for use in the new TCCR columns. Results are summarized in Table ES-2 and compared to ZAM model predictions. The highest cesium distribution coefficient and percent removal were observed with Dilution #3. IE-911 CST (an archived CST media batch) was more effective at removing cesium than the more recently prepared R9120-B CST media, though both media samples removed >88% of the cesium and the differences may not be statistically different considering the overall uncertainty. Based on the results, maximum cesium loadings were calculated for each CST media type and Tank 9H dilution. In general, maximum cesium loadings from dilutions of this supernate batch are quite high (approaching 0.1 mmol total Cs⁺/g CST for Dilution #1). The highest calculated maximum ¹³⁷Cs loading for the Tank 9H dilutions using the ZAM model with input of the tank compositions and batch contact results was 207 Ci/kg CST (Dilution #1 with IE-911 CST). In all cases, higher maximum cesium loading values were predicted for IE-911 CST versus R9120-B, although the differences varied considerably between the dilutions. The maximum loading value for IE-911 CST with Tank 9H Dilution #1 was only 7% higher than the maximum loading for R9120-B. The maximum loading value for IE-911 CST with Dilution #3 was 24% higher than the maximum loading for R9120-B. Dilution #2 was intermediate between these values. Note that these maximum loading values are the theoretical calculated values, and actual operating conditions will cause differences. A CST binder dilution (correction) factor near 0.7 (relative to pure powder CST) was required for each batch contact test with IE-911 engineered CST using the three Tank 9H dilutions. Correction factors calculated for R9120-B CST ranged from 0.56 to 0.66 for the three dilutions. Following the batch contact tests, the CST samples were isolated from the Tank 9H solution, washed, dried, and digested in acid following established procedures. The analysis results are provided in Table ES-3. Total cesium loading values determined by CST digestion were similar to the calculated loading values based on solution analysis (Table ES-2) for all samples. In addition, the CST was observed to load calcium (R9120-B sample only), iron, strontium, lead, uranium, and plutonium after contact with the waste supernate, as has been observed previously.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗