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At least 19 records

Fused slurry silicide coatings for columbium alloys reentry heat shields. Volume 1: Evaluation analysis

The R-512E (Si-20Cr-20Fe) fused slurry silicide coating process was optimized to coat full size (20in x 20in) single face rib and corrugation stiffened panels fabricated from FS-85 columbium alloy for 100 mission space shuttle heat shield applications. Structural life under simulated space shuttle lift-off stresses and reentry conditions demonstrated reuse capability well beyond 100 flights for R-512E coated FS-85 columbium heat shield panels. Demonstrated coating damage tolerance showed no immediate structural failure on exposure. The FS-85 columbium alloy was selected from five candidate alloys (Cb-752, C-129Y, WC-3015, B-66 and FS-85) based on the evaluation tests which have designed to determine: (1) change in material properties due to coating and reuse; (2) alloy tolerance to coating damage; (3) coating emittance characteristics under reuse conditions; and (4) new coating chemistries for improved coating life.

Fitzgerald, B.

Large area Czochralski silicon for solar cells

A detailed model of a typical Czochralski silicon crystal puller is utilized to predict maximum crystal growth rate as a function of various furnace parameters. Results of this analysis, when combined with multiblade slurry sawing, indicate that the Czochralski process is highly attractive for achieving near-term cost reduction of solar cell silicon.

Rea, S. N.

Real Time, In-line Monitoring of Hanford Tank Wastes - Year 1 Report

The team comprised of students, postdocs, early, mid and senior career scientists from Los Alamos National Laboratory, Savanah River National Laboratory, Georgia Tech and Florida International University, with the guidance of H2C, is developing a suite of in-line instruments for the Hanford high level waste (HLW) and low active waste (LAW) processes to provide near-real-time analysis of waste form physical properties and composition. The work builds on results from the recent DOE-ORP, EM Technology Development and other projects that demonstrated promise for the use of real-time in-line monitoring (RTIM) to measure chemical compositions of slurries of up to 20 weight % solids. The goal is for this instrument suite is to substantially reduce the need for sampling for process control. Sample waste, exposure associated with sample analysis, and the demand for an external laboratory facility would be greatly reduced. The throughput of waste treatment systems would be improved by elimination of the downtime caused by waiting for sample results. This translates into reduced process storage as process knowledge will be continuously updated in near-real-time. These breakthrough technologies would significantly reduce the life cycle cost and accelerate the schedule for the Hanford tank waste mission.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W

Sensitivity analysis of add-on price estimate for select silicon wafering technologies

The cost of producing wafers from silicon ingots is a major component of the add-on price of silicon sheet. Economic analyses of the add-on price estimates and their sensitivity internal-diameter (ID) sawing, multiblade slurry (MBS) sawing and fixed-abrasive slicing technique (FAST) are presented. Interim price estimation guidelines (IPEG) are used for estimating a process add-on price. Sensitivity analysis of price is performed with respect to cost parameters such as equipment, space, direct labor, materials (blade life) and utilities, and the production parameters such as slicing rate, slices per centimeter and process yield, using a computer program specifically developed to do sensitivity analysis with IPEG. The results aid in identifying the important cost parameters and assist in deciding the direction of technology development efforts.

Mokashi, A. R.

Characterization of Precipitate Reactor Feed Tank (PRFT) Batches 15, 22, and 26 from the Defense Waste Processing Facility (DWPF)

The Savannah River Site (SRS) Defense Waste Processing Facility (DWPF) processes a Monosodium Titanate/Sludge Solids (MST/SS) waste stream received from the Salt Waste Processing Facility (SWPF) via the Precipitate Reactor Feed Tank (PRFT). During processing, DWPF is required to provide evidence of compliance with the Waste Acceptance Product Specifications (WAPS) to ensure acceptance of their vitrified high-level waste (HLW) into the Civilian Radioactive Waste Management System. Production Records must document the constituents of the MST/SS material in the PRFT from each salt batch (StB) processed at SWPF. Savannah River Mission Completion (SRMC) has requested Savannah River National Laboratory (SRNL) to analyze PRFT samples representing each SWPF salt batch for thirty-two radionuclides. Additionally, elemental analysis of PRFT slurry and MST/SS solids was performed to aid SRMC in further refinement of the inputs and assumptions used in future frit development and Material Tracking Program calculations. The analyses of PRFT Batches 15, 22, and 26, which corresponds to material from the processing of StB4, StB5, and StB7, respectively, are reported herein. The unwashed dried solids of the PRFT batches were found to be 86-87% MST. Additionally, the total sulfur values are well below the assumed 982 mg of sulfate/kg of PRFT slurry used in Material Tracking Program calculations.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W

Characterization of Precipitate Reactor Feed Tank (PRFT) Batches 44 and 49 from the Defense Waste Processing Facility (DWPF)

The Savannah River Site (SRS) Defense Waste Processing Facility (DWPF) processes a Monosodium Titanate/Sludge Solids (MST/SS) waste stream received from the Salt Waste Processing Facility (SWPF) via the Precipitate Reactor Feed Tank (PRFT). During processing, DWPF is required to provide evidence of compliance with the Waste Acceptance Product Specifications (WAPS). Savannah River Mission Completion (SRMC) has requested Savannah River National Laboratory (SRNL) to analyze PRFT samples representing each SWPF salt batch for thirty-two radionuclides. Additionally, elemental analysis of PRFT slurry and MST/SS solids was performed to aid SRMC in further refinement of the inputs and assumptions used in future frit development and Material Tracking Program calculations. The analyses of PRFT Batches 44 and 49, which correspond to material from the processing of Salt Batches (StB) 12 and 11, respectively, are reported herein. The unwashed dried solids of the PRFT Batches 44 and 49 are predominately MST, ~63-59% MST. The two batches have a much higher amount of Fe, Mn, and Ni compared to all previous batches. For Batch 44 this appears to be due to the use of a sludge simulant filter aid during processing of StB 12 and for Batch 49, it is possibly due to the larger amount of insoluble solids for StB 11 in comparison to all previous salt batches. Like previous PRFT batches, a significant amount of the unwashed dried solids are alkaline earth metals. The total sulfate, in mg/kg of slurry, for PRFT Batches 44 and 49 is 119 and 139, respectively, which is well below the current sulfate concentration used in Material Tracking Program calculations and is in agreement with DWPF laboratory sulfate measurements.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W

Alloyed coatings for dispersion strengthened alloys

Processing techniques were developed for applying several diffusion barriers to TD-Ni and TD-NiCr. Barrier coated specimens of both substrates were clad with Ni-Cr-Al and Fe-Cr-Al alloys and diffusion annealed in argon. Measurement of the aluminum distribution after annealing showed that, of the readily applicable diffusion barriers, a slurry applied tungsten barrier most effectively inhibited the diffusion of aluminum from the Ni-Cr-Al clad into the TD-alloy substrates. No barrier effectively limited interdiffusion of the Fe-Cr-Al clad with the substrates. A duplex process was then developed for applying Ni-Cr-Al coating compositions to the tungsten barrier coated substrates. A Ni-(16 to 32)Cr-3Si modifier was applied by slurry spraying and firing in vacuum, and was then aluminized by a fusion slurry process. Cyclic oxidation tests at 2300 F resulted in early coating failure due to inadequate edge coverage and areas of coating porosity. EMP analysis showed that oxidation had consumed 70 to 80 percent of the aluminum in the coating in less than 50 hours.

Wermuth, F. R.

Surfactant studies for bench-scale operation

A phase 2 study has been initiated to investigate surfactant-assisted coal liquefaction, with the objective of quantifying the enhancement in liquid yields and product quality. This report covers the second quarter of work. The major accomplishments were: completion of coal liquefaction autoclave reactor runs with Illinois number 6 coal at processing temperatures of 300, 325, and 350 C, and pressures of 1800 psig; analysis of the filter cake and the filtrate obtained from the treated slurry in each run; and correlation of the coal conversions and the liquid yield quality to the surfactant concentration. An increase in coal conversions and upgrading of the liquid product quality due to surfactant addition was observed for all runs.

Hickey, Gregory S.

Suspension of SiC Powders in Allyhydridopolycarbosilane (AHPCS): Control of Rheology

Inert particulate fillers can be blended with preceramic polymers prior to infiltration of composite preforms to increase pyrolysis yield and decrease shrinkage, thus reducing the number of infiltration/ pyrolysis cycles required for densification. However, particulate filler loadings and concentration of added dispersants necessary to maintain low viscosity (< 0.50 N.s/sq m) slurries vary with the characteristics of the particular AHPCS polymer batch. These batch to batch variations occur with alterations in the synthesis process and method of allyl substitution, which in turn alter polymer structure and molecular weight distribution. A number of different polymer batches were characterized by NMR, GPC and thermal analysis, and the influence of polymer structure on rheology of filled systems determined. When the high molecular weight fraction increased to too great a level, suitably fluid slurries could no longer be attained.

Hurwitz, Frances I.

PERFORMANCE ANALYSIS OF AN ENGINEERING SCALE HYDROTHERMAL LIQUEFACTION SYSTEM

This work evaluates the Modular Hydrothermal Liquefaction System (MHTLS), an engineering-scale, integrated continuous HTL plant operated at the Pacific Northwest National Laboratory (PNNL), for converting realistic wet wastes into energy-dense biocrudes. The production campaigns discussed here processed algae, sewage sludges, lignocellulosic blends, Industrial food waste, and engineered food-waste slurries at 350?°C and around 200?bar, with nominal feed rates of ~12?L?h?¹. We report biocrude yields and composition, establish mass and elemental (C, N) balances, and quantify energy performance via heater duties, heat-exchanger behavior, and system-level efficiencies. Biocrudes contained 76–80?wt?% C (dry, ash-free) with HHVs of 38-41?MJ?kg?¹, substantially higher than feed materials HHVs of 16.6–26.1?MJ?kg?¹ and approaching petroleum fuels. Dry, ash-free biocrude yields of 32–53?wt?% corresponded to 43–71?wt?% carbon yields, with 18–40?wt?% of feed carbon routed to the aqueous phase. Thermal efficiencies were 50-65%, and total energy efficiencies, including reactor heat input, were 35-55%. A counter-current tube-in-tube heat exchanger delivered U values of 200–450?W?m?²?K?¹, with fouling-induced declines impacting heat recovery and heater duty. The analysis highlights three priorities for the process intensification of HTL: robust, fouling-resistant heat recovery, hydrodynamically suitable reactor and heat-exchanger designs, simplified and predictable solids management, and biocrude-water separation.

Biocrude production

Analysis and Evaluation of Processes and Equipment in Tasks 2 and 4 of the Low-cost Solar Array Project

The significant economic data for the current production multiblade wafering and inner diameter slicing processes were tabulated and compared to data on the experimental and projected multiblade slurry, STC ID diamond coated blade, multiwire slurry and crystal systems fixed abrasive multiwire slicing methods. Cost calculations were performed for current production processes and for 1982 and 1986 projected wafering techniques.

Goldman, H.

Advanced thermoplastic resins, phase 1

Eight thermoplastic polyimide resin systems were evaluated as composite matrix materials. Two resins were selected for more extensive mechanical testing and both were versions of LaRC-TPI (Langley Research Center - Thermoplastic Polyimide). One resin was made with LaRC-TPI and contained 2 weight percent of a di(amic acid) dopant as a melt flow aid. The second system was a 1:1 slurry of semicrystalline LaRC-TPI powder in a polyimidesulfone resin diglyme solution. The LaRC-TPI powder melts during processing and increases the melt flow of the resin. Testing included dynamic mechanical analysis, tension and compression testing, and compression-after-impact testing. The test results demonstrated that the LaRC-TPI resins have very good properties compared to other thermoplastics, and that they are promising matrix materials for advanced composite structures.

Hendricks, C. L.

Cold-Sprayed NMC622 Composite as a Cathode for Lithium-Ion Batteries

The growing demand for high-energy, low-cost lithium-ion batteries (LIBs) to power electric vehicles (EVs) necessitates advances in both materials and manufacturing processes. Conventional cathode fabrication methods, such as slurry casting and drying, are energy-intensive and pose challenges for scalability and environmental compliance. In this study, we propose cold-spray (CS) deposition as a solvent-free approach for fabricating LiNi 0.6 Mn 0.2 Co 0.2 O 2 (NMC622) composite cathodes. Powder blends of NMC622, poly(vinylidene fluoride) (PVDF), and carbon black (CB) are directly deposited onto stainless steel and Inconel substrates under varied gas temperatures, pressures (and thus velocities), and standoff distances. The effects of temperature on the deposit morphology, coating density, and volume are systematically investigated. Computational fluid dynamics simulations reveal that increasing the gas temperature enhances the particle velocity, narrows the spray angle, and reduces the mass concentration radially at the nozzle outlet. CS deposition results in a dense cathode microstructure, accompanied by fracture in polycrystalline NMC622 particles. X-ray diffraction analysis further verifies that there are no phase changes during the deposition process. The electrochemical performance of the cold-sprayed cathodes reveals an initial capacity of approximately 96 mAh g –1 for single-crystal NMC622 and 167 mAh g –1 for polycrystalline NMC622. While these values are modest compared to state-of-the-art slurry-cast cathodes, which typically exhibit 180–200 mAh g –1 under optimized conditions. The results demonstrate a competitive performance given the solvent-free nature of the CS process and compare favorably with tape-cast samples made from identical feedstock. In conclusion, he CS process enables the formation of dense, binder-integrated cathode coatings without the need for solvent processing, offering a promising pathway for scalable, energy-efficient dry electrode manufacturing of next-generation LIBs.

Batteries

Feedstock/Pretreatment Screening for Bioconversion of Sugars and Lignin Residues

This project will conduct biomass deconstruction (pretreatment and enzymatic saccharification) on two representative biomass feedstocks and four different pretreatment processes, including three high temperature steam/chemical pretreatments and one low temperature chemical/mechanical pretreatment. A third biomass feedstock will undergo biomass deconstruction with three different pretreatment processes, including two high temperature chemical pretreatments and one low temperature chemical/mechanical pretreatment. Several pretreatment conditions will be performed in a screening study using NLR pilot-scale pretreatment equipment to generate a range of pretreated biomass substrates. A selected number of these substrates will be chosen for enzymatic saccharification evaluation, based on standard compositional analysis of the pretreated substrates as a primary indicator of pretreatment efficacy. Resulting enzymatic hydrolysis slurries will be analyzed to determine overall biomass sugar yields. Additional compositional analysis will be performed to determine oligomeric sugar composition and structure, to analyze structural characteristics of solids fractions on native, pretreated, and enzymatically saccharified biomass residues for one of the biomass feedstocks, corn stover. The enzymatically saccharified materials will undergo 2,3-butanediol fermentation in a shaker flask as bench scale. Using relevant process performance data collected in these various conversion steps, technoeconomic analysis activities will be performed to compare the economic potential of the various biomass feedstock and pretreatment processes and to identify key economic drivers and sustainability metrics.

09 BIOMASS FUELS

Carbon–Mineral Slurry Electrodes for Energy-Efficient Lithium Leaching from Low-Grade Clay Feedstocks

Lithium extraction from clay deposits is typically hampered by low lithium grades and the high capital and energy demands of conventional processing. We report an ambient temperature electrochemical leaching method that bypasses high-temperature roasting and concentrated-acid leaching, directly liberating 93% of lithium from low-grade hectorite in 24 h at 1 V, with 77% Faradaic efficiency, an energy intensity of 3.91 MWh/t lithium carbonate equivalent (LCE). Utilizing a carbon-mineral composite slurry electrode strategy we achieve electron-driven lattice deconstruction through iron oxidation coupled with proton uptake to drive lithium deintercalation, offering a new strategy for low-temperature critical-metal recovery. A preliminary cost analysis highlights pathways to achieving cost intensities below $3000/t LCE. Challenges remain in improving current density, extraction kinetics, and demonstrating process scalability, however, this work establishes a foundation for effective electrochemical lithium extraction from abundant but previously uneconomical clay deposits.

Haddad, Andrew Z

A Preliminary Study of the Preparation of Slurry Fuels from Vaporized Magnesium

Slurry fuels containing extremely small particles of magnesium were prepared by concentrating the dilute slurry product resulting from the shock-cooling of magnesium metal vapors with a liquid hydrocarbon spray. A complete description of the equipment and procedure used in preparing the fuel is given. Ninety-five percent by weight of the solid particles formed by this process passed through a 100-mesh screen. The particle-size distribution of the screened fraction of one run, as determined by sedimentation analysis, indicated that 73 percent by weight of the metal particles were finer than 2 microns in equivalent spherical diameter. The purity of the solid particles ranged as high as 98.9 percent by weight of free magnesium. The screened product was concentrated by means of a bowl-type centrifuge from 0.5 to more than 50 percent by weight solids content to form an extremely viscous, clay-like mass. By addition of a surface active agent, this viscous material was converted into a pumpable slurry fuel.

FUELS, PREPARATION

Low gravity synthesis of polymers with controlled molecular configuration

Heterogeneous chemical systems have been studied for the synthesis of isotactic polypropylene in order to establish baseline parameters for the reaction process and to develop sensitive and accurate methods of analysis. These parameters and analytical methods may be used to make a comparison between the polypropylene obtained at one g with that of zero g (gravity). Baseline reaction parameters have been established for the slurry (liquid monomer in heptane/solid catalyst) polymerization of propylene to yield high purity, 98% isotactic polypropylene. Kinetic data for the slurry reaction showed that a sufficient quantity of polymer for complete characterization can be produced in a reaction time of 5 min; this time is compatible with that available on a sounding rocket for a zero-g simulation experiment. The preformed (activated) catalyst was found to be more reproducible in its activity than the in situ formed catalyst.

Heimbuch, A. H.