High temperature stable carborane adhesives First quarterly progress report, 21 Dec. 1965 - 20 Mar. 1966
Synthesis of carborane-expoxy adhesives for use in high temperature aerospace environments
BORON COMPOUND↗
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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.
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Current Issues with Environmental Barrier Coatings for Ceramics and Ceramic Composites
The environmental barrier coating (EBC) for SiC/SiC ceramic matrix composites and Si3N4 ceramics is an emerging field as the application of silicon-based ceramics in the gas turbine engine hot section is on the horizon, both for aero and industrial gas turbines. EBC is an enabling technology for silicon-based ceramics because these materials without an EBC cannot be used in combustion environments due to rapid surface recession. Significant progress in EBC development has been made during the last decade through various government-sponsored programs. Current EBCs are based on silicon, mullite (3Al2O3-2SiO2) and BSAS (barium strontium aluminum silicate with celsian structure). Volatility of BSAS, BSAS-silica chemical reaction, and low melting point of silicon limit temperature capability of current EBCs to about 1350 C for long-term applications. There is a need for higher temperature EBCs as the temperature capability of silicon-based ceramics continue to increase. Therefore, research is underway to develop EBCs with improved temperature capability compared to current EBCs. The current status and issues with the advanced EBC development efforts will be discussed.
Lee, Kang N.↗
Implementation of the Glycolate Destruction Process with Sodium Permanganate in the Defense Waste Processing Facility (DWPF) - 20141
The Savannah River Site (SRS) seeks to replace formic acid with glycolic acid as a chemical reductant in the Defense Waste Processing Facility (DWPF), where borosilicate glass is mixed with high-level radioactive waste, melted at high temperatures, then poured into stainless steel canisters for safe storage. Prior research and development have demonstrated the feasibility and advantages of the new nitric-glycolic acid flowsheet over the current nitric-formic acid flowsheet to chemically adjust the radioactive sludge slurry waste in the Sludge Receipt and Adjustment Tank (SRAT) prior to vitrification. Use of glycolic acid reduces hydrogen and ammonia generation during the reduction process, thus reducing flammability hazards and purge requirements in the DWPF processing vessels. In addition, glycolic acid will support the new Salt Waste Processing Facility (SWPF) by allowing for receipt of higher volumes of waste due to reduction of flammable gases, increased boil-up rates in the vessels, and easing the processing of future sludge batches containing high levels of mercury. However, during DWPF operations, trace amounts of glycolate are anticipated to be entrained in the recycle stream and sent to the Concentration, Storage, and Transfer Facilities (CSTF) via the Recycle Collection Tank (RCT). The RCT receives condensate from the Slurry Mix Evaporator Condensate Tank (SMECT) and Off-gas Condensate Tank (OGCT) that may contain unreacted glycolate. A literature review found the potential for hydrogen generation due to thermolysis of glycolate in caustic CSTF conditions. Savannah River National Laboratory (SRNL) conducted several tests on simulant and radioactive waste from various tanks at SRS and confirmed that glycolate added to waste at concentrations of approximately 1000 mg/L and higher generates hydrogen through thermolysis. There are potential operating scenarios in the future where glycolate concentration could exceed 1000 mg/L in the 2H Evaporator Drop Tank, the highest accumulation point for DWPF organics received via recycle. These findings presented a need to develop another process to mitigate the impact of glycolic acid to the CSTF. Several DWPF compatible options were evaluated for their ability to destroy glycolate in the DWPF recycle stream under various processing conditions, thereby mitigating its introduction to the CSTF. Downselection testing identified sodium permanganate as the most promising and simplest option to oxidize glycolate. It has been demonstrated to be effective in various RCT simulant compositions, operating temperatures, oxidant addition rates, solution pH, and initial glycolate concentrations. A feasibility study identified existing tanks within the facility that could be used for receiving and storing the commercially available sodium permanganate, as well as feeding it to the RCT for processing. The use of existing equipment as well as the ability to purchase the pre-mixed chemical reduces implementation and operational complexity. The downstream impacts of the sodium permanganate reaction were also evaluated and demonstrated to have minimal impact on other chemical species present in the RCT and CSTF, as well as on the materials of construction of the RCT and CSTF vessels and associated piping and instrumentation. Future work is in progress to validate the glycolate destruction process with testing in actual radioactive RCT waste before implementation in DWPF. (authors)
12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
Theoretical estimates of flammability bounds for thin condensed fuel diffusion flames in microgravity using detailed models of chemistry and radiation
Recently, U-shape flammability maps have been constructed showing minimal oxygen vs. flame strain for opposed flame spread in micro-gravity by Olson and Ferkul. The U-shape defines the limiting flammability bounds from radiative extinction and flame blow-off. Here, the minimum of the U corresponds to the minimum possible oxidizer concentration where burning can occur, and is an important quantity of interest for fire safety. While high strain extinction bounds have been well analyzed, low strain radiative extinction has not. To estimate low strain extinction, in this study an analytical theory is developed based on thin flame theory coupled with a heat and mass transfer model for solid fuels. A reaction progress variable based on the Damköhler number is adapted in the theory to account for incomplete combustion at high strain rates and enable the capturing of the full flammability map. The analytical model is compared to a one dimensional numerical model w/ detailed chemical kinetics and coupled radiation heat transfer in planar and spherical geometries. The flammability maps are then qualitatively compared to experimental extinguishment data compiled by Olson and Ferkul for cylindrical rods of PMMA showing similar trends. The results show the newly developed analytics capture the radiative extinction bound compared to the numerical model and qualitatively agrees with microgravity data.
38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
Ionospheric chemistry
This report deals primarily with progress in the chemistry of minor neutrals and ionized constituents of the thermosphere. Significant progress was made over the last few years in quantitative studies of many chemical processes. This success was primarily due to the advent of multiparameter multisatellite programs which permitted accurate simultaneous measurements to be made of many important parameters. In many cases studies of chemical reactions were made with laboratory-like precision. Rate coefficients have been derived as functions of temperature for a number of important reactions. New information has been acquired on nearly every major process which occurs in the thermosphere, including the recombination rates of all major molecular ions, charge transfer reactions, ion atom interchange reactions, and reactions of neutral and ionized metastable atoms and molecules.
Torr, D. G.↗
Study of recirculating gas flow fields in the base region of Saturn-class vehicles quarterly progress report, 1 May - 31 Jul. 1965
Chemical and chemical radiative effects on base flow field of multiple nozzled launch vehicles of Saturn launch vehicle type
NOZZLE FLOW↗
Toward efficient single-atom catalysts for renewable fuels and chemicals production from biomass and CO 2
Transformation of biomass and CO 2 into renewable value-added chemicals and fuels has been identified as a promising strategy to fulfill high energy demands, lower greenhouse gas emissions, and exploit under-utilized resources. Cost-effective and performance-efficient catalysts are of great importance to lowering the conversion cost of biomass and CO 2 . Significant progress has been made to advance the catalyst design for these processes, with metal catalysts playing a critical role in many involved catalytic reactions. Traditional nanoparticle-based metal catalysts still require improvement in metal utilization rates, stability, and selectivity tunability. Single-atom catalysts, which have maximum atomic efficiency and a uniform and tunable metal center, as well as an adjustable metal-support interaction, provide potential opportunities to boost catalyst efficiency and thermal stability. Their well-defined and uniform structure also provides advantages to fundamental studies for understanding of the intrinsic reaction mechanism and site requirement in biomass and CO 2 conversion. In this article, we summarize and highlight the recent advances in converting biomass and CO 2 to renewable fuels and chemicals using single-atom catalysts. We discuss the design principles of single-atom catalysts and their potential applications to biomass and CO 2 upgrading as well as the origins of catalytic activity. Moreover, we compare the catalytic efficiency of various catalysts reported thus to provide a fair assessment of these catalysts. Finally, perspectives are given on the interesting fields that may guide future studies.
09 BIOMASS FUELS↗
Analytical study of catalytic reactors for hydrazine decomposition Quarterly progress report, 15 Jul. - 14 Oct. 1966
Computer programs used for formulating and solving integral and differential equations in study of catalytic reactors for hydrazine decomposition
COMPUTER PROGRAM↗
Recent Progress on Cerium Oxide‐Based Nanostructures for Energy and Environmental Applications
Cerium oxide (CeO 2 ) photo/electrocatalysts for energy storage and environmental applications have attracted considerable interest because of stable crystal structure, low toxicity/cost, superior chemical stability, stable redox (Ce 3+ /Ce 4+ ) pairs, abundant oxygen defects, and capablility for intense interaction with other materials. However, the wide bandgap and poor conductivity lower the CeO 2 photo/electrocatalytic and energy storage performances. To overcome these limitations, various modification strategies (tuning morphology, doping or loading of metal nanoparticles, and heterostructures) have been applied for the improvement of photocatalytic (removal of organic contaminants from water/wastewater and H 2 production and CO 2 reduction reactions) efficiency, electrocatalytic (hydrogen/oxygen evolution reactions and CO 2 reduction reactions), and energy storage performances (supercapacitor) of CeO 2 ‐based materials. Herein, the recent progress of CeO 2 ‐based materials for electro(photo)catalysis and energy storage applications has been discussed. The challenges and possible direction of CeO 2 ‐based materials for electro(photo)catalysis and energy storage applications have been emphasized. Furthermore, this comprehensive review is expected to advance the design of CeO 2 ‐based materials and their applications in electro(photo)catalysis and energy.
Ray, Schindra Kumar [Department of Chemistry North↗
Combustion of bulk titanium in oxygen
The combustion of bulk titanium in one atmosphere oxygen is studied using laser ignition and several analytical techniques. These were high-speed color cinematography, time and space resolved spectra in the visible region, metallography (including SEM) of specimens quenched in argon gas, X-ray and chemical product analyses, and a new optical technique, the Hilbert transform method. The cinematographic application of this technique for visualizing phase objects in the combustion zone is described. The results indicate an initial vapor phase reaction immediately adjacent to the molten surface but as the oxygen uptake progresses the evaporation approaches the point of congruency and a much reduced evaporation rate. This and the accumulation of the various soluble oxides soon drive the reaction zone below the surface where gas formation causes boiling and ejection of particles. The buildup of rutile cuts off the oxygen supply and the reaction ceases.
Clark, A. F.↗
Center for Modeling of Turbulence and Transition (CMOTT): Research Briefs, 1992
The progress is reported of the Center for Modeling of Turbulence and Transition (CMOTT). The main objective of the CMOTT is to develop, validate and implement the turbulence and transition models for practical engineering flows. The flows of interest are three-dimensional, incompressible and compressible flows with chemical reaction. The research covers two-equation (e.g., k-e) and algebraic Reynolds-stress models, second moment closure models, probability density function (pdf) models, Renormalization Group Theory (RNG), Large Eddy Simulation (LES) and Direct Numerical Simulation (DNS).
Liou, William W.↗
Fungal degradation of fiber-reinforced composite materials
As described in a previous report, a fungal consortium isolated from degraded polymeric materials was capable of growth on presterilized coupons of five composites, resulting in deep penetration into the interior of all materials within five weeks. Data describing the utilization of composite constituents as nutrients for the microflora are described in this article. Increased microbial growth was observed when composite extract was incubated with the fungal inoculum at ambient temperatures. Scanning electron microscopic observation of carbon fibers incubated with a naturally developed population of microorganisms showed the formation of bacterial biofilms on the fiber surfaces, suggesting possible utilization of the fiber chemical sizing as carbon and energy sources. Electrochemical impedance spectroscopy was used to monitor the phenomena occurring at the fiber-matrix interfaces. Significant differences were observed between inoculated and sterile panels of the composite materials. A progressive decline in impedance was detected in the inoculated panels. Several reaction steps may be involved in the degradation process. Initial ingress of water into the resin matrix appeared to be followed by degradation of fiber surfaces, and separation of fibers from the resin matrix. This investigation suggested that composite materials are susceptible to microbial attack by providing nutrients for growth.
Environmental Microbiology↗
Progressive growth of the solid–electrolyte interphase towards the Si anode interior causes capacity fading
The solid–electrolyte interphase (SEI), a layer formed on the electrode surface, is essential for electrochemical reactions in batteries and critically governs the battery stability. Active materials, especially those with extremely high energy density, such as silicon (Si), often inevitably undergo a large volume swing upon ion insertion and extraction, raising a critical question as to how the SEI interactively responds to and evolves with the material and consequently controls the cycling stability of the battery. Here, by integrating sensitive elemental tomography, an advanced algorithm and cryogenic scanning transmission electron microscopy, we unveil, in three dimensions, a correlated structural and chemical evolution of Si and SEI. Furthermore, corroborated with a chemomechanical model, we demonstrate progressive electrolyte permeation and SEI growth along the percolation channel of the nanovoids due to vacancy injection and condensation during the delithiation process. Consequently, the Si–SEI spatial configuration evolves from the classic ‘core–shell’ structure in the first few cycles to a ‘plum-pudding’ structure following extended cycling, featuring the engulfing of Si domains by the SEI, which leads to the disruption of electron conduction pathways and formation of dead Si, contributing to capacity loss. The spatially coupled interactive evolution model of SEI and active materials, in principle, applies to a broad class of high-capacity electrode materials, leading to a critical insight for remedying the fading of high-capacity electrodes.
36 MATERIALS SCIENCE↗
Role of H 2 O in Catalytic Conversion of C 1 Molecules
Due to their role in controlling global climate change, the selective conversion of C 1 molecules such as CH 4 , CO, and CO 2 has attracted widespread attention. Typically, H 2 O competes with the reactant molecules to adsorb on the active sites and therefore inhibits the reaction or causes catalyst deactivation. However, H 2 O can also participate in the catalytic conversion of C 1 molecules as a reactant or a promoter. Herein, we provide a perspective on recent progress in the mechanistic studies of H 2 O-mediated conversion of C 1 molecules. We aim to provide an in-depth and systematic understanding of H 2 O as a promoter, a proton-transfer agent, an oxidant, a direct source of hydrogen or oxygen, and its influence on the catalytic activity, selectivity, and stability. We also summarize strategies for modifying catalysts or catalytic microenvironments by chemical or physical means to optimize the positive effects and minimize the negative effects of H 2 O on the reactions of C 1 molecules. Finally, we discuss challenges and opportunities in catalyst design, characterization techniques, and theoretical modeling of the H 2 O-mediated catalytic conversion of C 1 molecules.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Multifunctional Chiral Chemically‐Powered Micropropellers for Cargo Transport and Manipulation
Practical applications of synthetic self-propelled nano and microparticles for microrobotics, targeted drug delivery, and manipulation at the nanoscale are rapidly expanding. However, fabrication limitations often hinder progress, resulting in relatively simple shapes and limited functionality. Here, taking advantage of 3D nanoscale printing, chiral micropropellers powered by the hydrogen peroxide reduction reaction are fabricated. Due to their chirality, the propellers exhibit multifunctional behavior controlled by an applied magnetic field: spinning in place (loitering), directed migration in the prescribed direction, capture, and transport of polymer cargo particles. Design parameters of the propellers are optimized by computation modeling based on mesoscale molecular dynamics. It is predicted by computer simulations, and confirmed experimentally, that clockwise rotating propellers attract each other and counterclockwise repel. These results shed light on how chirality and shape optimization enhance the functionality of synthetic autonomous micromachines.
36 MATERIALS SCIENCE↗
Silicon production process evaluations
Chemical engineering analysis was continued for the HSC process (Hemlock Semiconductor Corporation) in which solar cell silicon is produced in a 1,000 MT/yr plant. Progress and status are reported for the primary engineering activities involved in the preliminary process engineering design of the plant base case conditions (96%), reaction chemistry (96%), process flow diagram (85%), material balance (85%), energy balance (60%), property data (60%), equipment design (40%), major equipment list (30%) and labor requirements (10%). Engineering design of the second distillation column (D-02, TCS column) in the process was completed. The design is based on a 97% recovery of the light key (TCS, trichlorosilane) in the distillate and a 97% recovery of the heavy key (TET, silicon tetrachloride) in the bottoms. At a reflux ratio of 2, the specified recovery of TCS and TET is achieved with 20 trays (equilibrium stages, N=20). Respective feed tray locations are 9, 12 and 15 (NF sub 1 = 9, NF sub 2 = 12,, and NF sub 3 = 15). A total condenser is used for the distillation which is conducted at a pressure of 90 psia.
Source record↗
Silicon production process evaluations
The chemical engineering analysis of the preliminary process design of a process for producing solar cell grade silicon from dichlorosilane is presented. A plant to produce 1,000 MT/yr of silicon is analyzed. Progress and status for the plant design are reported for the primary activities of base case conditions (60 percent), reaction chemistry (50 percent), process flow diagram (35 percent), energy balance (10 percent), property data (10 percent) and equipment design (5 percent).
Source record↗
Study of recirculating gas flow fields in the base region of Saturn-class vehicles Quarterly progress report, 1 Aug. - 31 Oct. 1965
Transformation of chemically reacting high speed turbulent boundary layer to equivalent low speed flow in study of recirculating gas flow fields in base region of Saturn vehicles
GAS FLOW↗