Development of an Effective Finite-rate Oxidation Model for NuSil-coated Charred Carbon Preform Ablators
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Krishnan Swaminathan Gopalan↗
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Characterizing Char Rate and Extent in Fiber-Reinforced Plastics Using X-ray Computed Tomography
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Benton Greene↗
Aerotherm Chemical Equilibrium (ACE) and Charring Material Thermal Response and Ablation Programs (CMA) Tutorial
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Michael O'Malley↗
Carbonization Under Confinement: Predicting Charring Behavior of Carbon Composite Resins
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polymer↗
Fracture of Charring Avcoat With Meshfree Material Response-Coupled Fracture Approach
Fracture of thermal protection systems (TPS) is typically unfavorable, but often unavoidable. TPS can fracture during entry, manufacturing or from impact. Many NASA missions use ablative materials for TPS, including the fore-body for Dragonfly (PICA) and Orion for Artemis-I (Avcoat). The material response to thermal and mechanical loads during entry is integral to TPS sizing, design and analysis. The fracture of TPS also depends, and can be caused by, the change of material properties during entry. Simulations that resolve fracture of TPS due to thermo-mechanical forces can identify TPS failure mechanisms and be applied to conditions inaccessible to ground testing. We present simulation work using a mesh-free/Lagrangian approach to solving continuum mechanics, coupled to material response. Two different materials are simulated under different model entry-like boundary conditions. The dynamic crack structure is analyzed and compared across simulations. Crack analyses inform the role of design features, such as entry trajectories and manufacturing-influenced material properties, play in TPS fracture.
Andrew P Santos↗
Effect of Microwave-Assisted Gasification on the Chemical and Physical Properties of Coal Chars
56th Annual Microwave Power Symposium (IMPI 56), Savannah, GA, June 14-16, 2022
Ellison, Candice↗
Real-Time X-ray Radiography Diagnostics of Components in Solid Rocket Motors
Solid rocket motors (SRMs) typically use nozzle materials which are required to maintain their shape as well as insulate the underlying support structure during the motor operation. In addition, SRMs need internal insulation materials to protect the motor case from the harsh environment resulting from the combustion of solid propellant. In the nozzle, typical materials consist of high density graphite, carbon-carbon composites and carbon phenolic composites. Internal insulation of the motor cases is typically a composite material with carbon, asbestos, Kevlar, or silica fibers in an ablative matrix such as EPDM or NBR. For both nozzle and internal insulation materials, the charring process occurs when the hot combustion products heat the material intensely. The pyrolysis of the matrix material takes away a portion of the thermal energy near the wall surface and leaves behind a char layer. The fiber reinforcement retains the porous char layer which provides continued thermal protection from the hot combustion products. It is of great interest to characterize both the total erosion rates of the material and the char layer thickness. By better understanding of the erosion process for a particular ablative material in a specific flow environment, the required insulation material thickness can be properly selected. The recession rates of internal insulation and nozzle materials of SRMs are typically determined by testing in some sort of simulated environment; either arc-jet testing, flame torch testing, or subscale SRMs of different size. Material recession rates are deduced by comparison of pre- and post-test measurements and then averaging over the duration of the test. However, these averaging techniques cannot be used to determine the instantaneous recession rates of the material. Knowledge of the variation in recession rates in response to the instantaneous flow conditions during the motor operation is of great importance. For example, in many SRM configurations the recession of the solid propellant grain can drastically alter the flow-field and effect the recession of internal insulation and nozzle materials. Simultaneous measurement of the overall erosion rate, the development of the char layer, and the recession of the char-virgin interface during the motor operation can be rather difficult. While invasive techniques have been used with limited success, they have serious drawbacks. Break wires or make wire sensors can be installed into a sufficient number of locations in the charring material from which a time history of the charring surface can be deduced. These sensors fundamentally alter the local structure of the material in which they are imbedded. Also, the location of these sensors within the material is not known precisely without the use of an X-ray. To determine instantaneous recession rates, real-time X-ray radiography (X-ray RTR) has been utilized in several SRM experiments at PSU. The X-ray RTR system discussed in this paper consists of an X-ray source, X-ray image intensifier, and CCD camera connected to a capture computer. The system has been used to examine the ablation process of internal insulation as well as nozzle material erosion in a subscale SRM. The X-ray source is rated to 320 kV at 10 mA and has both a large (5.5 mm) and small (3.0 mm) focal spot. The lead-lined cesium iodide X-ray image intensifier produces an image which is captured by a CCD camera with a 1,000 x 1,000 pixel resolution. To produce accurate imagery of the object of interest, the alignment of the X-ray source to the X-ray image intensifier is crucial. The image sequences captured during the operation of an SRM are then processed to enhance the quality of the images. This procedure allows for computer software to extract data on the total erosion rate and the char layer thickness. Figure 1 Error! Reference source not found.shows a sequence of images captured during the operation the subscale SRM with the X-ray RTR system. The X-rayTR system, alignment procedure, uncertainty determination, and image analysis process will be discussed in detail in the full manuscript.
Cortopassi, A. C.↗
Environmental Influence of Gravity and Pressure on Arc Tracking of Insulated Wires Investigated
Momentary short-circuit arcs between a defective polyimide-insulated wire and another conductor may thermally char (pyrolize) the insulating material. The charred polyimide, being conductive, can sustain the short-circuit arc, which may propagate along the wire through continuous pyrolization of the polyimide insulation (arc tracking). If the arcing wire is part of a multiple-wire bundle, the polyimide insulation of other wires within the bundle may become thermally charred and start arc tracking also (flash over). Such arc tracking can lead to complete failure of an entire wire bundle, causing other critical spacecraft or aircraft failures. Unfortunately, all tested candidate wire insulations for aerospace vehicles were susceptible to arc tracking. Therefore, a test procedure was designed at the NASA Lewis Research Center to select the insulation type least susceptible to arc tracking. This test procedure addresses the following three areas of concern: (1) probability of initiation, (2) probability of reinitiation (restrike), and (3) extent of arc tracking damage (propagation rate). Item 2 (restrike probability) is an issue if power can be terminated from and reapplied to the arcing wire (by a switch, fuse, or resettable circuit breaker). The degree of damage from an arcing event (item 3) refers to how easily the arc chars nearby insulation and propagates along the wire pair. Ease of nearby insulation charring can be determined by measuring the rate of arc propagation. Insulation that chars easily will propagate the arc faster than insulation that does not char very easily. A popular polyimide insulated wire for aerospace vehicles, MIL-W-81381, was tested to determine a degree of damage from an arcing event (item 3) in the following three environments: (1) microgravity with air at 1-atm pressure, (2) 1g with air at 1 atm, and (3) 1g within a 10^-6 Torr vacuum. The microgravity 1-atm air was the harshest environment, with respect to the rate of damage of arc tracking, for the 20 AWG (American Wiring Gauge) MIL-W-81381 wire insulation type . The vacuum environment resulted in the least damage. Further testing is planned to determine if the environmental results are consistent between insulation types and to evaluate the other two parameters associated with arc tracking susceptibility.
Source record↗
A Comprehensive Greenhouse Gas Assessment of Biomass-Based Carbon Dioxide Removal and Storage
Biomass-based Carbon Removal and Storage (BiCRS) is a suite of technological pathways that provide a relatively affordable and high-potential way to remove carbon dioxide from the atmosphere and simultaneously re-purpose residual biomass. BiCRS technologies are individually optimized to different biomass feedstocks, temperatures and oxygen, with the primary goal of capturing a high percentage of biomass-derived carbon dioxide and storing it in permanent below-ground storage (i.e. geologic storage), and a secondary goal of producing renewable energy. The current standard for BiCRS life cycle assessments does not account for greenhouse gas (carbon dioxide, methane and nitrous oxide) fluxes from surface soil amendment of BiCRS byproducts (e.g. char, ash) and their alternate fates. This is partly due to a paucity of empirical data due to the novelty of BiCRS conversion technologies, the range in feedstocks, and the heterogeneity of soils to which they might be amended. To fill this gap in in the life-cycle assessment and provide a realistic range of parameters for a soil amendment component of the BiCRS life cycle assessment, we conducted an incubation experiment to measure soil carbon changes, microbial respiration, methane fluxes, and nitrous oxide fluxes from two different soils amended with char- and ash- byproducts from biomass after gasification to hydrogen, fast pyrolysis to bio-oil, and torrefaction. Our results suggest that nitrous oxide and methane emission or consumption from BiCRS char amendments to soil are context dependent. Nitrous oxide emissions from amendments are higher in soils with higher pH, whereas some char amendments to low pH soil can reduce N 2 O emissions relative to control. In contrast, methane is emitted from BiCRS char amended to low pH soil, but consumed or neutral relative to control when amended to high pH soil. We present carbon and nitrogen mass balance throughout the experiment to help understand short-term durability of BiCRS chars and their counterfactuals, and preliminary suggestions for revisions to the broader BiCRS Measurement, Reporting, and Verification framework.
54 ENVIRONMENTAL SCIENCES↗
The thermal and mechanical properties of a low density elastomeric ablation material
Thermal and mechanical properties data were obtained for a low density elastomeric resin based ablation material with phenolic-glass honeycomb reinforcement. Data were obtained for the material in the charred and uncharred state. Ablation material specimens were charred in a laboratory furnace at temperatures in the range from 600 K to 1700 K to obtain char specimens representative of the ablation char layer formed during reentry. These specimens were then used to obtain effective thermal conductivity, heat capacity, porosity, and permeability data at the char formation temperature. This provided a boxing of the data which enables the prediction of the transient response of the material during ablation. Limited comparisons were made between the furnace charred specimens and specimens which had been exposed to simulated reentry conditions.
Engelke, W. T.↗
Burn severity and vegetation type control phosphorus concentration, molecular composition, and mobilization
Shifting phosphorus (P) dynamics after wildfires can have cascading impacts from terrestrial to aquatic environments. However, it is unclear whether shifts in P composition or P concentration are responsible for changes in P dynamics post-fire. We used laboratory leaching experiments of Douglas fir forest and sagebrush shrubland chars to examine how the potential mobility of P compounds is influenced by different burn severities. Burning produced a 6.9- and 29-fold increase in particulate P mobilization but a 3.8- and 30.5-fold decrease in aqueous P released for Douglas fir forest and sagebrush shrubland, respectively. The mechanisms driving particulate- and dissolved-phase P compound mobilization were contrasting. Phosphorus compound mobilization in the particulate phase was controlled by solid char total P concentrations, while the aqueous phase was driven by solubility changes of molecular species. Nuclear magnetic resonance (NMR) and X-ray absorption near-edge structure (XANES) on the solid chars indicated that organic orthophosphate monoester and diester species were thermally mineralized to inorganic P moieties with burning in both vegetation types, which decreases P solubility. This coincided with the production of calcium- and magnesium-bound inorganic P compounds. With increasing burn severity there were systematic shifts in P concentration and composition – higher-severity chars mobilized P compounds in the particulate phase, although the magnitude of change was vegetation-specific. Our results indicate a post-fire transformation to both the composition of the solid charred material and how P compounds are mobilized, which may influence its environmental cycling and fate.
31P solution-state NMR↗
Graphite and ablative material response to CO2 laser, carbon-arc, and xenon-arc radiation
The behavior was investigated of graphite and several charring ablators in a variety of high-radiative heat-flux environments. A commercial-grade graphite and nine state-of-the-art charring ablators were subjected to various radiative environments produced by a CO2 laser and a carbon arc. Graphite was also tested in xenon-arc radiation. Heat-flux levels ranged from 10 to 47 MW/sq m. Tests were conducted in air, nitrogen, helium, and a CO2-N2 mixture which simulated the Venus atmosphere. The experimental results were compared with theoretical results obtained with a one-dimensional charring-ablator analysis and a two-dimensional subliming-ablator analysis. Neither the graphite nor the charring ablators showed significant differences in appearance or microstructure after testing in the different radiative environments. The performance of phenolic nylon and graphite was predicted satisfactorily with existing analyses and published material property data. Good agreement between experimental and analytical results was obtained by using sublimation parameters from a chemical nonequilibrium analysis of graphite sublimation. Some charring ablators performed reasonably well and could withstand radiative fluxes of the level encountered in certain planetary entries. Other materials showed excessive surface recession and/or large amounts of cracking and spalling, and appear to be unsuitable for severe radiative environments.
Brewer, W. D.↗
Experimental performance of an ablative material as an external insulator for a hypersonic research aircraft
An ablative material composed of silica-filled elastomeric silicone was tested to evaluate its thermal and structural performance as an external insulator, or heat shield, for a hypersonic research aircraft. The material was also tested to determine whether it would form a durable char layer when initially heated and thereafter function primarily as an insulator with little further pyrolysis or char removal. Aerothermal tests were representative of nominal Mach 6 cruise conditions of the aircraft, and additional tests were representative of Mach 8 cruise and interference heating conditions. Radiant heating tests were used to simulate the complete nominal Mach 6 surface-temperature history. The silica char that formed during aerothermal tests was not durable. The char experienced a general and preferential surface recession, with the primary mechanism for char removal being erosion. Tests revealed that radiant heating is not a valid technique for simulating aerodynamic heating of the material.
Puster, R. L.↗
Radiative Ignition and Transition to Spread Investigation (RITSI)
A total of 25 experiments was conducted in the Glovebox Facility on the Third United States Microgravity payload (USMP3) mission to study the behavior of both flaming and smoldering ignition events, the transition from ignition to the flame/smoldering spread, and the flame/smoldering growth pattern in air. Twenty one of the 25 experiments were flaming experiments and the remainder were smoldering experiments. Ignition was initiated by a heated wire across a thermally thin filter paper in the middle of the sample for the two-dimensional configuration and by a focused beam from a halogen/tungsten lamp at the center of the sample for the three-dimensional configuration. The external air flow velocity was varied from 0 cm/s to 6.5 cm/s. The ignition and subsequent flame spread events were recorded by a video camera, a 35 mm camera, and 6 thermocouples (2 in the gas phase and 4 in the sample). The results indicate that non-piloted radiative ignition of the paper by external thermal radiation tends to occur more easily than in normal gravity. In the two-dimensional configuration, the transition from ignition to downstream flame spread never occurred; only the transition to upstream spread took place. In the three-dimensional configuration, a char growth pattern emerged in the shape of a fan, with the ignited area as the center of the fan and the fan spreading in the upstream direction. The internal angle of the fan increased with an increase in external flow velocity (higher flow velocity gave a more opened fan pattern). At an external flow velocity of 5 cm/s, the flame was horseshoe-shaped and the char pattern became an elongated semicircle toward upstream. It appears that the peak upstream flame spread rate was reached at a higher external velocity than for the two-dimensional flame front. Flame spread much faster along open edges of the sample paper than along the sample face, presumably due to there being larger supply of oxygen and energy feedback at the open edges than at the surface. These results indicate the possible importance of the effect of the flame front shape such as the curvature of the flame front on spread rate and flame strength. A complex, unexpected finger-shaped char growth pattern was observed during the smoldering experiment. Higher external flow velocity increased the number of localized smoldering fronts, of the char fingers they left behind, and frequency of bifurcations from the fingers. At present, it is not clear what caused such a complex char growth pattern.
Kashiwagi, Takashi↗
Light Weight Ceramic Ablators for Mars Follow-on Mission Vehicle Thermal Protection System
New Light Weight Ceramic Ablators (LCA) were produced by using ceramic and carbon fibrous substrates, impregnated with silicone and phenolic resins. The special infiltration techniques (patent pending) were developed to control the amount of organic resins in the highly porous fiber matrices so that the final densities of LCA's range from 0.22 to 0.24 g/cc. This paper presents the thermal and ablative performance of the Silicone Impregnated Reusable Ceramic Ablators (SIRCA) in simulated entry conditions for Mars-Pathfinder in the Ames 60 MW Interaction Heating Facility (I HF). Arc jet test results yielded no evidence of char erosion and mass loss at high stagnation pressures to 0.25 atm. Minimal silica melt was detected on surface char at a stagnation pressure of 0.31 atm. Four ceramic substrates were used in the production of SIRCA's to obtain the effective of boron oxide present in substrate so the thermal performance of SIRCA's. A sample of SIRCA was also exposed to the same heating condition for five cycles and no significant mass loss or recession was observed. Tensile testing established that the SIRCA tensile strength is about a factor of two higher than that of the virgin substrates. Thermogravimetric Analysis (TGA) of the char in nitrogen and air showed no evidence of free carbon in the char. Scanning Electron Microscopy of the post test sample showed that the char surface consists of a fibrous structure that was sealed with a thin layer of silicon oxide melt.
Tran, Huy K.↗
Novel Low-Density Ablators Containing Hyperbranched Poly(azomethine)s
An ablative composite is low-density (0.25 to 0.40 g/cu cm), easy to fabricate, and superior to the current state-of-the-art ablator (phenolic impregnated carbon ablator, PICA) in terms of decomposition temperature, char yield, and mechanical strength. Initial ablative testing with a CO2 laser under high-heat-flux (1,100 W/sq cm) conditions showed these new ablators are over twice as effective as PICA in terms of weight loss, as well as transfer of heat through the specimen. The carbon fiber/poly(azomethine) composites have the same density as PICA, but are 8 to 11 times stronger to irreversible breaking by tensile compression. In addition, polyazomethine char yields by thermogravimetric analysis are 70 to 80 percent at 1,000 C. This char yield is 10 to 20 percent higher than phenolic resins, as well as one of the highest char yields known for any polymer. A high char yield holds the composite together better toward shearing forces on reentry, as well as reradiates high heat fluxes. This innovative composite is stronger than PICA, so multiple pieces can be sealed together without fracture. Researchers have also studied polyazomethines before as linear polymers. Due to poor solubility, these polymers precipitate from the polymerization solvent as a low-molecular-weight (2 to 4 repeat units) powder. The only way found to date to keep linear polyazomethines in solution is by adding solubilizing side groups. However, these groups sacrifice certain polymer properties. These hyperbranched polyazomethines are high molecular weight and fully aromatic.
Tigelaar, Dean↗
Intumescent Coatings as Fire Retardants
The development of fire-retardant coatings to protect surfaces which may be exposed to fire or extreme heat is a subject of intense interest to many industries. A fire-retardant paint has been developed which represents a new chemical approach for preparing intumescent coatings, and potentially, is very important to fire-prevention authorities. The requirements for a superior coating include ease of application, suitability to a wide variety of surfaces and finishes, and stability over an extended period of time within a broad range of ambient temperature and humidity conditions. These innovative coatings, when activated by the heat of a fire, react to form a thick, low-density, polymeric coating or char layer. Water vapor and sulphur dioxide are released during the intumescent reaction. Two fire-protection mechanisms thus become available: (1) the char layer retards the flow of heat, due to the extremely low thermal conductivity; and (2) water vapor and sulfur dioxide are released, providing fire quenching properties. Still another mechanism functions in cases where the char, by virtue of its high oxidation resistance and low thermal conductivity, reaches a sufficiently high temperature to re-radiate much of the incident heat load. The coatings consist of dispersions of selective salts of a nitro-amino-arornatic compound. Specifically, para-nitroaniline bisulfate and the ammonium salt of para-nitroaniline-ortho sulphuric acid (2-amino-5-nitrobenzenesulphuric acid) are used. Suitable vehicles are cellulose nitrate of lacquer grade, a nitrite-phenolic modified rubber, or epoxy-polysulfide copolymer. Three separate formulations have been developed. A solvent is usually employed, such as methylethyl ketone, butyl acetate, or toluene, which renders the coatings suitably thin and which evaporates after the coatings are applied. Generally, the intumescent material is treated as insoluble in the vehicle, and is ground and dispersed in the vehicle and solvent like an ordinary coating pigment. The char found on intumescence is better in terms of yield and physical properties than chars obtained from many previously known intumescent materials. Prior to intumescence, the coating has a density of 85 pounds per cubic foot. After intumescence, the density is approximately 0.3 pounds per cubic loot. The linear expansion of the coatings ranges from 70 to 200 times the applied coating thickness.
Parker, J. A.↗
Temperature and Frequency Dependent Electrical Properties of AVCOAT and Shuttle Tile Material
This technical memorandum presents the data and results from a series of tests performed on AVCOAT, charred AVCOAT, and different Shuttle Thermal Protection System (TPS) tile coatings to determine their electrical properties as a function of temperature and frequency. Initially, the samples were assumed to be insulators and the complex permittivities were measured from data collected by sandwiching each sample between two conductors to form a sandwich. However, the AVCOAT sample data showed that the material becomes conductive as it begins to char. To get an accurate conductivity reading on these charred samples, a four-point resistance probe was used to collect data. Overall, this testing showed that the virgin AVCOAT starts out as a material that is a good insulator but transitions to one with a conductivity on the order of 1860 S/m as it chars. The deeper layers of AVCOAT (un-charred) all exhibited a temperature and frequency dependence that is possibly indicative of a dielectric relaxation in the material. As the sample temperatures were increased, a knee appears in the real permittivity data sets below 1 kHz. Both the real permittivity and resistivity drop up to several orders of magnitude yet show that the material remains an insulator. The Shuttle High Temperature Reusable Surface Insulation (HRSI) tile coatings studied included Reac- tion Cured Glass (RCG), Aluminum Enhanced Thermal Barrier (AETB), and Toughened Unipiece Fibrous Insulation (TUFI). The purely glass fiber parts of the tile were removed leaving only the outer layers con- taining just the coating. The data collected shows that the RCG, AETB, and outermost layer of the TUFI have similar electrical properties. The real permittivity plots show that there appears to be a relaxation that shows up at frequencies below 1 kHz. The relaxation frequency increases with increasing temperature. Also, the real permittivity increases up to about a factor of four between room temperature and 650K. Likewise, the resistivity (related to the imaginary permittivity) decreases up to five orders of magnitude over the same temperature interval, but still remains an insulator. This data was collected to support a NASA Engineering and Safety Center (NESC) assessment team investigating the source of thermocouple anomalies in both Shuttle TPS material and AVCOAT used for on the Orion spacecraft for Exploration Flight Test 1 (EFT-1). The details of their findings will be documented in a separate report with this document serving as a reference.
Mark A Nurge↗