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NASA NTRS2001

Research on High Temperature Ceramic Insulation for Electrical Conductors

Three methods for applying ceramic coatings to wires were examined in depth and a fourth (chemical vapor deposition) was studied briefly. CVD coatings were not reported in the thesis because it was realized early in the study that the deposition rate of the coatings was too slow to be used in a commercial process. Of the methods reported in the thesis, slurry coating was the most promising. This method consists of slowly drawing a platinum wire through a thixotropic slurry of alumina in a vehicle composed of polyvinyl butyral, methyl ethyl ketone, and toluene. The coatings produced by this method were continuous and free of cracks after sintering. The sintered coatings crack when the wire is bent around sharp corners, but most of the coating remains in place and still provides electrical insulation between the wire and any metallic structure to which the wire may be attached. The coating thickness was 0.61 mm (16 micrometers). The electrical resistivity of the intact coating was 340 M-Ohm-cm at 800 C and 23 M-Ohm-cm at 1050 C. Therefore, these coatings more than meet the electrical requirements for use in turbine engines. Although adherence of the coating to the wire was generally excellent, a problem was noted in localized areas where the coating flaked off. Further work will be needed to obtain good coating adherence along the entire length of the wire. The next most promising coatings were made by electrophoretic deposition (EPD) of Al2O3 onto platinum wires, using mixtures of ethanol and acetone as the suspending liquid. These EPD coatings were made only on short lengths of wire because the coating is too fragile to allow spooling of the wire. The worst coatings were those made by electrophoretic deposition from aqueous suspensions. Continuous slurry coating of wire was achieved, but due to lack of suitable equipment, the wire had to be cut into short lengths for sintering.

Kreidler, Eric R.↗

NASA NTRS2000

Near-Net-Shape Processing of Sintered Fibrous Ceramics Achieved

A variety of sintered fibrous ceramic (SFC) materials have been developed over the last 50 years as thermal barrier materials for reentry applications. SFC materials typically exhibit very low thermal conductivities combined with low densities and good thermal stability up to 2500 F. These materials have flown successfully on the space shuttle orbiters since the 1960's. More recently, the McDonnell Douglas Corporation successfully used SFC tiles as a heat shield on the underside of its DC X test vehicle. For both of these applications, tiles are machined from blocks of a specific type of SFC called an alumina-enhanced thermal barrier (AETB). The sizes of these blocks have been limited by the manufacturing process. In addition, as much as 80 to 90 percent of the material can be lost during the machining of tiles with significant amounts of curvature. To address these problems, the NASA Glenn Research Center at Lewis Field entered a cooperative contract with the Boeing Company to develop a vacuum-assisted forming process that can produce large (approximately 4 square feet), severely contoured panels of AETB while saving costs in comparison to the conventional cast-and-machine billet process. For shuttle use, AETB is slurry cast, drained, and fired to form square billets conforming to the shape of the filtration box. The billets are then cut into tiles of the appropriate size for thermally protecting the space shuttle. Processing techniques have limited the maximum size of AETB billets to 21.5 square inches by 6.5-in. thick, but the space shuttles use discrete heat shield tiles no more than 8 to 12 square inches. However, in other applications, large, complex shapes are needed, and the tiling approach is undesirable. For such applications, vacuum-assisted forming can produce large parts with complex shapes while reducing machining waste and eliminating cemented joints between bonded billets. Because it allows contoured shapes to be formed, material utilization is inherently high. Initial estimates show that the amount of material lost during machining can be reduced by 50 percent or more. In addition, a fiber alignment favorable for minimum heat transfer is maintained for all panel shapes since the fibers are aligned parallel to the contoured surface of the forming tool or mold. The vacuum-assisted forming process can complete the entire forming operation in a matter of minutes and can produce multiple parts whose size is limited only by the size of the forming tool. To date, panels as large as 2 square feet have been demonstrated The vacuum-assisted forming process starts with the fabrication of a permeable forming tool, or mold, with the proper part contour. This reusable tool is mounted over an internal rib support structure, as depicted in the diagram, such that a vacuum can be pulled on the bottom portion of the tool. AETB slurry is then poured over and around the tool, liquid is drawn from the slurry, and the part forms over the tool surface. The part is then dried, fired, and finished machined. Future plans include an evaluation of the need for additional coatings and surface-toughness treatments to extend the durability and performance of this material.

Angel, Paul W.↗

NASA NTRS2006

Making Plant-Support Structures From Waste Plant Fiber

Environmentally benign, biodegradable structures for supporting growing plants can be made in a process based on recycling of such waste plant fiber materials as wheat straw or of such derivative materials as paper and cardboard. Examples of structures that can be made in this way include plant plugs, pots, planter-lining mats, plant fences, and root and shoot barriers. No chemical binders are used in the process. First, the plant material is chopped into smaller particles. The particles are leached with water or steam to remove material that can inhibit plant growth, yielding a fibrous slurry. If the desired structures are plugs or sheets, then the slurry is formed into the desired shapes in a pulp molding subprocess. If the desired structures are root and shoot barriers, pots, or fences, then the slurry is compression-molded to the desired shapes in a heated press. The processed materials in these structures have properties similar to those of commercial pressboard, but unlike pressboard, these materials contain no additives. These structures have been found to withstand one growth cycle, even when wet

Morrow, Robert C.↗

NASA NTRS2003

Software Computes Tape-Casting Parameters

Tcast2 is a FORTRAN computer program that accelerates the setup of a process in which a slurry containing metal particles and a polymeric binder is cast, to a thickness regulated by a doctor blade, onto fibers wound on a rotating drum to make a green precursor of a metal-matrix/fiber composite tape. Before Tcast2, setup parameters were determined by trial and error in time-consuming multiple iterations of the process. In Tcast2, the fiber architecture in the final composite is expressed in terms of the lateral distance between fibers and the thickness-wise distance between fibers in adjacent plies. The lateral distance is controlled via the manner of winding. The interply spacing is controlled via the characteristics of the slurry and the doctor-blade height. When a new combination of fibers and slurry is first cast and dried to a green tape, the shrinkage from the wet to the green condition and a few other key parameters of the green tape are measured. These parameters are provided as input to Tcast2, which uses them to compute the doctor-blade height and fiber spacings needed to obtain the desired fiber architecture and fiber volume fraction in the final composite.

deGroh, Henry C., III↗

NASA NTRS2013

Enabling Microliquid Chromatography by Microbead Packing of Microchannels

The microbead packing is the critical element required in the success of on-chip microfabrication of critical microfluidic components for in-situ analysis and detection of chiral amino acids. In order for microliquid chromatography to occur, there must be a stationary phase medium within the microchannel that interacts with the analytes present within flowing fluid. The stationary phase media are the microbeads packed by the process discussed in this work. The purpose of the microliquid chromatography is to provide a lightweight, low-volume, and low-power element to separate amino acids and their chiral partners efficiently to understand better the origin of life. In order to densely pack microbeads into the microchannels, a liquid slurry of microbeads was created. Microbeads were extracted from a commercially available high-performance liquid chromatography column. The silica beads extracted were 5 microns in diameter, and had surface coating of phenyl-hexyl. These microbeads were mixed with a 200- proof ethanol solution to create a microbead slurry with the right viscosity for packing. A microfilter is placed at the outlet via of the microchannel and the slurry is injected, then withdrawn across a filter using modified syringes. After each injection, the channel is flushed with ethanol to enhance packing. This cycle is repeated numerous times to allow for a tightly packed channel of microbeads. Typical microbead packing occurs in the macroscale into tubes or channels by using highly pressurized systems. Moreover, these channels are typically long and straight without any turns or curves. On the other hand, this method of microbead packing is completed within a microchannel 75 micrometers in diameter. Moreover, the microbead packing is completed into a serpentine type microchannel, such that it maximizes microchannel length within a microchip. Doing so enhances the interactions of the analytes with the microbeads to separate efficiently amino acids and amino acid enantiomers.

Balvin, Manuel↗

NASA NTRS2014

Enabling Microliquid Chromatography by Microbead Packing of Microchannels

Balvin, Manuel↗

NASA NTRS2023

Satellite-Derived Estimates of Suspended CaCO3 Mud Con-Centrations from the West Florida Shelf Induced by Hurricane Ian

In the days following the passage of Hurricane Ian over the West Florida Shelf, a large plume of calcium carbonate (CaCO3) mud slurry was observed extending from west of the Dry Tortugas and curving to the east into the Straits of Florida. This discreet target offered a unique opportunity to quantify the suspended mass of CaCO3 in the slurry. Estimating the concentration of sediment in a plume of suspended CaCO3 by satellite sensor observations has been stymied up to now owing to a lack of in situ suspended sediment measurements during storm events, as “sea truth” data for such events is difficult to acquire. However, the Particulate Inorganic Carbon (PIC) standard product provided by the NASA Ocean Biology Distributed Active Archive Center (OBDAAC) is based on Moderate Resolution Imaging Spectroradiometer (MODIS) observations of a plume of coccolith chalk released from a ship in the “Chalk-Ex” experiment. Due to the similarities (particle size, mineralogy, and reflectance properties) of the suspended chalk features and the Ian-induced slurry, we utilized this data product to make initial estimates of the concentration of suspended sediment in the plume.

remote sensing↗

DOE OSTI2021

BETO 2021 Peer Review - Bench Scale Integration WBS 2.4.1.100

Bench Scale Integration develops and optimizes fermentation processes to produce bio-based fuels and chemicals from biomass sugars. The project uses fermentation science to achieve high titers and production rates by, for example, manipulating how the microorganisms are fed biomass sugars and nutrients, modifying fermentation conditions (pH, temperature, aeration) or developing online control strategies that increase production rates. For this period of performance, we conducted small scale fermentation research using strategies mentioned to produce 2,3-butanediol (BDO) from biomass utilizing NREL's proprietary Zymomonas mobilis microorganism. BDO is a versatile chemical which can be catalytically upgraded to a variety of hydrocarbon fuels and chemicals. The 3-yr project goal was to increase BDO titers from 50 g/L (FY17 level) to 125 g/L on biomass sugars by 2020. This is a 150% increase in titer showing the commercial potential of Z. mobilis while reducing the cost to downstream processing. We successfully achieved this target. The project also showed yearly progress improvements to the process design case by using a whole biomass slurry. Future work will focus on procedures for scaling to produce large quantities of BDO broth for separations and upgrading R&D and improve the titer and rates from biomass whole slurry. Our goal is to produce 100 g/L BDO titer from whole slurry at >1000L by 2023 which will meet the technical targets set by our techno-economic analysis.

29 ENERGY PLANNING, POLICY, AND ECONOMY↗

DOE OSTI2021

Apparatus and method for three-dimensional metal printing

An apparatus and device for building an article by additive manufacturing or 3-D printing. The method includes feeding a supply of particulate slurry to and through a nozzle, such as including an integrated pump, to form a plurality of beads and layers of the slurry on a deposition surface, and ultimately forming a desirable article from the layers of deposited material. The liquid phase of the slurry is desirably removed by heat, and the deposited layers can be sintered or otherwise fused as needed.

Klett, James W.↗

DOE OSTI2022

Multiphysics Simulation of Supercritical CO2 Gasification for Hydrogen Production

A bench-scale supercritical CO2 gasifier is being considered by the U.S. Department of Energy’s National Energy Technology Laboratory (NETL). A reacting computational fluid dynamics (CFD) model was developed using ANSYS/Fluent in order to investigate the impact of various operating parameters on syngas composition. The model was validated using available data in the literature. Simulations were conducted over a range of coal-slurry loadings, reaction temperatures, system pressures, and oxygen mass flowrates with the goal of optimizing hydrogen production for the considered reactor. The results from the simulations identified a positive correlation between slurry loading and hydrogen production, while reactor temperature and pressure had a limited impact on H2 production at the conditions of interest. Additionally, the simulations indicated that oxygen mass flowrate has less of an impact on hydrogen production at higher slurry loadings.

Prlina, Alexander↗

DOE OSTI2023

Methods and systems for liquid separations

Methods and systems for separating liquid components are disclosed. A vessel is provided containing a solids conveyance device. At least a first portion of the vessel acts as an indirect-contact heat exchanger and a second portion of the vessel contains a filter. A process liquid stream, containing a first component and a second component, is passed into the first portion of the vessel. A portion of the second component is frozen and entrained in the first portion of the vessel into the process liquid stream, resulting in a process slurry stream. The process slurry stream is passed into a second portion of the vessel by the solids conveyance device. The process slurry stream is separated into a solid product stream and a primary liquid product stream by passing the primary liquid product stream through the filter and out of the vessel while separately removing the solid product stream out of the vessel.

Baxter, Larry↗

DOE OSTI2023

Method and integrated process for the carboxylation of furan derived carboxylic acids to 2,5-furandicarboxylic acid

A process for carboxylation of a furoate slurry to produce FDCA, especially 2,5-FDCA, includes the steps of: feeding a slurry containing a suspension fluid, furoate, a surfactant and an alkali metal carbonate to a carboxylation reactor; and feeding a flow of CO 2 to the carboxylation reactor at flow conditions sufficient to suspend the slurry in the reactor and react the furoate with CO 2 to form 2,5-FDCA. A fully integrated process is also disclosed.

Kittrell, James R.↗

DOE OSTI2021

Developing a Novel Ultrafine Coal Dewatering Process

Dewatering fine coal is needed in many applications but has remained a great challenge. The hydrophobic-hydrophilic separation (HHS) method is a powerful technology to address this problem. However, organic solvents in solvent-coal slurries produced during HHS must be recovered for the method to be economically viable. Here, the experimental studies of recovering solvents from pentane-coal and hexane-coal slurries by combining liquid-solid filtration and in-situ vaporization and removing the solvent by a carrier gas (i.e., drying) are reported. The filtration behaviors are studied under different solid mass loading and filtration pressure. It is shown that using pressure filtration driven by 20 psig nitrogen, over 95% of solvents by mass in the slurries can be recovered, and filtration cakes can be formed in 60 s. The drying behavior was studied using nitrogen and steam at different temperatures and pressures. It is shown that residual solvents in filtration cakes can be reduced below 1400 ppm within 10 s by 15 psig steam superheated to 150 degree C, while other parameter combinations are far less effective in removing solvents. Physical processes involved in drying and the structure of solvent-laden filtration cakes are analyzed in light of these results.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2024

Vessel and method for solid-liquid separation

Devices, systems, and methods for separating solids from liquids are disclosed. A vessel includes an inlet, a carrier liquid outlet, a product outlet, a purifying section, and a heater. The inlet directs a slurry into the purifying section. The slurry comprises particles of a solid and a carrier liquid. The purifying section preferentially drives the particles of the solid towards a heating zone of the purifying section versus the carrier liquid. This displaces a first portion of the carrier liquid away from the heating zone of the purifying section. The heater heats the slurry. The carrier liquid outlet drives a majority of the carrier liquid out of the vessel. The product outlet is adjacent to the heating zone of the purifying section.

Baxter, Larry↗

DOE OSTI2022

Industrial scale mesofluidic particle separation

Here we explore the potential of a mesofluidic separator that fits within industrial piping and is designed to remove large aspherical particles out of an abrasive slurry at fast flow rates. Mesofluidic separators have recently demonstrated separation of spherical particles at flow rates of ~1 gallon/min (gpm) (6.3.10 -5 m 3 /s). Yet, the performance of these separators at flow rates achievable within industrial piping have not been explored. Here we evaluate the permeate flowrate fraction, large particle mass fraction, and pressure drop from approximately 35-100 gpm (2.2.10-3-6.3.10-3 m 3 /s) in a three inch tube using an abrasive and modestly non-spherical slurry. Faster flow rates may be achieved with larger pumps and larger diameters. We find the permeate fraction and pressure drop both increase with flow rate, though the pressure drop remains modest. Only two feet of inserts removed 97.6±2.1% of large particles for conditions tested. Separation was demonstrated in both vertical and horizontal orientations with the horizontal orientation benefiting marginally from gravitational settling.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Stirring and peristaltic pumping alter flow electrode particle size and morphology

Flowable carbon-based electrodes are widely studied in electrochemical systems for energy storage and water treatment. Most laboratory- and pilot-scale studies employ active mixing for slurry preparation and handling and use peristaltic pumps for slurry circulation. Magnetic stirring is the most prevalent mixing method at the laboratory scale, and the combination of magnetic mixing and peristaltic pumping is favored for convenience and compatibility with particulate suspensions. However, these methods can strongly affect particle size and morphology (and therefore cell performance). In this study, we evaluate how mixing and pumping influence particle degradation in two commonly used carbon materials: spherical carbon black (CB) beads and powdered activated carbon (AC). We performed 24 h stirring-only experiments using magnetic, orbital, and overhead stirring. Separately, we conducted 32 h circulation experiments using a commercial peristaltic pump. Particle morphology and size were analyzed using optical microscopy and laser diffraction. The initially spherical CB beads (~580 μm, 1.5 wt%) exhibit rapid and extensive breakdown under both peristaltic pumping and magnetic stirring. By comparison, AC particles (initially ~31 μm) tested at 1.5 and 15 wt% showed measurable size reductions of up to ~25 % under either stirring or pumping. In conclusion, these findings highlight the need to account for and quantify morphological changes caused by both stirring and pumping in the design and associated evaluation of flowable electrode systems.

Chemistry↗

DOE OSTI2024

Recovery of Oxpure 612C-50 Coconut Carbon Particles Using Bump Arrays

Cyanide is used to leach gold from crushed ore (solid matrix) into a gold cyanide solution. The gold is extracted from the cyanide solution by adsorption onto activated carbon. The gold extraction process occurs when the activated coconut carbon is placed into tanks that contain the gold cyanide solution either in a batch process or into a continuous flow circuit. The coconut carbon is then removed from the solution for gold recovery. The use of the mesofluidic separation system (a deterministic lateral displacement system) can significantly reduce costs and waste generated from the process of removing the coconut carbon from the solution. In the coconut carbon recovery process used at many gold mines in Nevada, the gold is attached to carbon particles that are still in the cyanide liquor. The mesofluidic system can rapidly remove the gold bearing carbon particles from the cyanide liquor quickly and with no operating costs. The benefits include: • Reduce operational costs related to filtration and hydro-cyclones • Reduced acid usage for the elution gold stripping phase as only 25% of the fluids will follow the carbon particles to the final express lane when two mesofluidic systems are used in series This alternative particle removal techniques would be advantageous. A promising technique for removing larger particles from slurries is mesofluidic separation, similar to deterministic lateral displacement arrays or “bump” arrays [1] but operates at much larger flow rates. As described by Pease, et al. [2], “Bump arrays in deterministic lateral displacement devices separate large particles from small particles using arrays of staggered posts. Large particles, defined as those with radii larger than the distance between the edge of a post and the stagnation streamline from the next downstream post, must bump toward one side of the device, whereas particles smaller than this distance slalom from entrance to exit without net lateral displacement.” Unlike filters or sieves, the posts in the arrays that cause separation do not block or occlude particle flow but work because particles go around the posts. Unlike hydrocyclones separation, separation is not driven by particle density, because gravitational forces are unimportant to mesofluidic separation. Burns, et al., and Pease, et al., have shown that particles may be separated from complex suspensions, under turbulent flow conditions, and at industrially important flow rates [3-5]. They have also recently shown that mesofluidic devices may be arranged in series to increase separation performance [6]. In this paper, we evaluate the mesofluidic system for the separation of commercial OxPure GR 612 Charred Coconut shell particles as a proof of principle test for the rapid separation using the 1500 micron cut mesofluidic separator. We first describe the experimental system and conditions. We then present the experimental results. [1] Huang, L.R., E.C. Cox, R.H. Austin, J.C. Sturm. 2004. Continuous particle separation through deterministic lateral displacement. Science, 304, 987–990. https://doi.org/10.1126/science.1094567. [2] Pease L.F., J.A. Bamberger, C.A. Burns, and M.J. Minette. 2021. Large Particle Separation from Non-Newtonian Slurries using Bump Arrays. In Proceedings of the ASME 2021 Fluids Engineering Division Summer Meeting FEDSM2021-65904, V003T08A023. New York, New York: ASME. doi:10.1115/FEDSM2021-65904 [3] Burns C.A., T.G. Veldman, J. Serkowski, R.C. Daniel, X.-Y. Yu, M.J. Minette, L.F. Pease. 2021. Mesofluidic separation versus dead-end filtration. Separation and Purification Technology, 254, 117256. https://doi.org/10.1016/j.seppur.2020.117256. [4] Pease L.F., J.E. Serkowski, T.G. Veldman, J. Williams, X.-Y. Yu, M.J. Minette, J.A. Bamberger, C.A. Burns. 2021. Can Bump Arrays Separate Particles from Turbulent Flows?. In Proceedings of the ASME 2021 Fluids Engineering Division Summer Meeting FEDSM2021-67696, V003T08A024. New York, New York: ASME. doi:10.11

mesofluidic separation, slurry, bump array↗

DOE OSTI2021

A Process Intensification Approach for CO 2 Absorption Using Amino Acid Solutions and a Guanidine Compound

Environmentally friendly amino-acid salt solutions are used for the absorption of carbon dioxide from concentrated flue-gas streams via chemical absorption. Process intensification reduces operating and capital costs by combining chemical reactions and separation operations. Here, we present a new process-intensification approach that combines the CO 2 capture and the amino-acid regeneration steps into a single process carried out in a slurry three-phase reactor. The absorbed CO 2 precipitates as a solid carbonated guanidine compound. The cycle is completed by separation of the solid precipitate to strip the CO 2 and regenerate the guanidine compound, while the liquid solution is recycled to the slurry reactor. The process was studied by modifying a model developed by the authors for a gas-liquid bubble column without the presence of the guanidine compound. The guanidine precipitation reaction was accounted for using kinetic parameters calculated by the authors in another study. The proposed model was implemented by modifying an existing computer code used for the simulation of gas-liquid bubble columns. The calculated results showed that the proposed cycle can significantly reduce energy, equipment, and operating costs and can make an important contribution to developing a competitive cost-effective large-scale process for CO 2 capture.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗