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At least 37 records · Page 2

Solar heating of common lunar minerals for the production of oxygen

The purpose of this work was to demonstrate the feasibility of vapor-phase reduction (pyrolysis) of lunar materials to produce oxygen. Solar furnace experiments were conducted on two common lunar minerals, ilmenite and anorthite. Thermodynamic equilibrium calculations predicted that ilmenite should show a larger pressure increase than anorthite under conditions of the experiments and this was confirmed by the experiments. The measured mass loss of the ilmenite sample was consistent with loss of oxygen by reduction of iron in the liquid phase; this result was also predicted from equilibrium calculations. Based on preliminary experiments and equilibrium calculations, the temperatures needed for pyrolysis are expected to be in the range of 2000 to 2500 K, giving total gas pressures of 0.01 to 1 torr. Bulk regolith can be used as a feedstock without extensive beneficiation. Further, selective condensation of metal-containing species from the gas phase may yield metallic iron and silicon as byproducts from the process.

Senior, C. L.↗

Volatile Analysis by Pyrolysis of Regolith for Planetary Resource Exploration

The extraction and identification of volatile resources that could be utilized by humans including water, oxygen, noble gases, and hydrocarbons on the Moon, Mars, and small planetary bodies will be critical for future long-term human exploration of these objects. Vacuum pyrolysis at elevated temperatures has been shown to be an efficient way to release volatiles trapped inside solid samples. In order to maximize the extraction of volatiles, including oxygen and noble gases from the breakdown of minerals, a pyrolysis temperature of 1400 C or higher is required, which greatly exceeds the maximum temperatures of current state-of-the-art flight pyrolysis instruments. Here we report on the recent optimization and field testing results of a high temperature pyrolysis oven and sample manipulation system coupled to a mass spectrometer instrument called Volatile Analysis by Pyrolysis of Regolith (VAPoR). VAPoR is capable of heating solid samples under vacuum to temperatures above 1300 C and determining the composition of volatiles released as a function of temperature.

Glavin, Daniel P.↗

Development of a Robust, High Current, Low Power Field Emission Electron Gun for a Spaceflight Reflectron Time-of-Flight Mass Spectrometer

Carbon materials, including carbon nanotubes (CNTs) and nitrogen-incorporated ultrananocrystalline diamond (N-UNCD), have been of considerable interest for field emission applications for over a decade. In particular, robust field emission materials are compelling for space applications due to the low power consumption and potential for miniaturization. A reflectron time-of-flight mass spectrometer (TOF-MS) under development for in situ measurements on the Moon and other Solar System bodies uses a field emitter to generate ions from gaseous samples, using electron ionization. For these unusual environments, robustness, reliability, and long life are of paramount importance, and to this end, we have explored the field emission properties and lifetime of carbon nanotubes and nitrogen-incorporated ultrananocrystalline diamond (N-UNCD) thin films, the latter developed and patented by Argonne National Laboratory. We will present recent investigations of N-UNCD as a robust field emitter, revealing that this material offers stable performance in high vacuum for up to 1000 hours with threshold voltage for emission of about 3-4 V/lJm and current densities in the range of tens of microA. Optimizing the mass resolution and sensitivity of such a mass spectrometer has also been enabled by a parallel effort to scale up a CNT emitter to an array measuring 2 mm x 40 mm. Through simulation and experiment of the new extended format emitter, we have determined that focusing the electron beam is limited due to the angular spread of the emitted electrons. This dispersion effect can be reduced through modification of the electron gun geometry, but this reduces the current reaching the ionization region. By increasing the transmission efficiency of the electron beam to the anode, we have increased the anode current by two orders of magnitude to realize a corresponding enhancement in instrument sensitivity, at a moderate cost to mass resolution. We will report recent experimental and modeling results to describe the performance of a field emission electron gun as employed in the Volatile Analysis by Pyrolysis of Regolith (VAPoR) TOF-MS prototype.

Southard, Adrian E.↗

TPSAS-NF1676L-21180-DND

Ablative materials are used as the Thermal Protection System (TPS) for space vehicles that enter a planetary atmosphere. During the entry phase, the vehicle experiences high rates of aerodynamic heating. These ablative materials, acting as a heat shield, protect the vehicle from the harsh environment and ensure a safe entry. Ablative materials reduce the incoming heat flux through various phenomena such as near-surface oxidation, pyrolysis chemical reaction, vaporization, and other erosive processes, collectively known as ablation. Spallation is one such ablative process, in which solid particles are ejected from the material into the flow field. The many conditions leading to spallation, however, are not well understood and cannot be described accurately by simple phenomenological models. However, the spallation phenomenon might impact the aerodynamic heating rates of re-entry vehicles using ablative heat shields. For example, the solid particles ejected from the surface can modify the near surface chemical processes and flow field. To investigate spallation effects, a code was developed to compute the dynamics of spalled particles. The code uses a finite-rate chemistry model to study the chemical interactions of the particles with the flow field. The spallation code is dynamically coupled to a CFD solver that models the time accurate hypersonic flow field around an ablative sample. An experimental investigation was also performed at the NASA Langley HYMETS facility. HYMETS is a 400 kW arcjet that can simulate hypersonic flight and Earth or Martian entry conditions. Using high speed cameras, an IR camera, NIR and UV-VIS spectrometers, and other diagnostic instruments, test data on various graphite, LI-900, FiberForm, and PICA test samples were obtained, using target heat flux conditions of 100, 200, and 400 W/cm 2 . From the test campaign, measurements of particle velocity, acceleration and trajectory are obtained.

A Martin↗

Determining total carbon in hydrazine

Procedure incorporates modified pyrolysis train. Samples are vaporized before entering furnace to be pyrolyzed at 850 C + or - 25 C. Direct collection of pyrolyzed gas reduces loss of carbon dioxide. Infrared spectroscopy can be used to analyze samples for carbon dioxide content.

Davis, E. E.↗

Chemical vapor deposition growth

A chemical vapor deposition (CVD) reactor system with a vertical deposition chamber was used for the growth of Si films on glass, glass-ceramic, and polycrystalline ceramic substrates. Silicon vapor was produced by pyrolysis of SiH4 in a H2 or He carrier gas. Preliminary deposition experiments with two of the available glasses were not encouraging. Moderately encouraging results, however, were obtained with fired polycrystalline alumina substrates, which were used for Si deposition at temperatures above 1,000 C. The surfaces of both the substrates and the films were characterized by X-ray diffraction, reflection electron diffraction, scanning electron microscopy optical microscopy, and surface profilometric techniques. Several experiments were conducted to establish baseline performance data for the reactor system, including temperature distributions on the sample pedestal, effects of carrier gas flow rate on temperature and film thickness, and Si film growth rate as a function of temperature.

Ruth, R. P.↗

Chemical Vapor Deposition of Germanium of Silicon

Experimental work shows chemical vapor deposition (CVD) by pyrolysis of gaseous germanium tetrahydride provides epitaxial layers of germanium on silicon. Relatively low temperature of CVD process (500 degrees to 900 degrees C) reduces stresses that occur at layer/substrate interface during growth and cooling.

Aharoni, H.↗

Instrument Packages for the Cold, Dark, High Radiation Environments

We are developing a small cold temperature instrument package concept that integrates a cold temperature power system and radhard ultra low temperature ultra low power electronics components and power supplies now under development into a cold temperature surface operational version of a planetary surface instrument package. We are already in the process of developing a lower power lower tem-perature version for an instrument of mutual interest to SMD and ESMD to support the search for volatiles (the mass spectrometer VAPoR, Volatile Analysis by Pyrolysis of Regolith) both as a stand alone instrument and as part of an environmental monitoring package.

Clark, P. E.↗

Organic solids produced by electrical discharge in reducing atmospheres - Tholin molecular analysis

The complex dark brown solid of a class called tholins, produced on passage of an electrical discharge through a roughly equimolar mixture of methane and ammonia with 2.6% water vapor, is analyzed by vacuum pyrolysis followed by gas chromatography and mass spectrometry. Pyrolyzates include a wide range of aliphatic and aromatic nitriles, alkanes, alkenes, aromatic hydrocarbons, pyrrole, and pyridine. This tholin is remarkably stable to 950 C. It and its degradation products are candidate constituents of planetary aerosols in the outer solar system and of the grains in the interstellar medium.

Khare, B. N.↗

Evaluation of Low-Energy Hydrogen Separation Method Using Metal-Organic Frameworks (MOFs) for Closed-Loop ECLSS Air Revitalization (CLEAR)

The State-of-the-Art (SOA) air revitalization architecture onboard the International Space Station (ISS) recovered approximately 50% of the oxygen (O 2 ) from metabolic carbon dioxide (CO 2 ) via the Sabatier process from 2011 to 2017. O 2 recovery is currently constrained by the limited availability of reactant hydrogen (H 2 ) preventing complete conversion of CO 2 to H 2 O. Increasing O 2 recovery within Closed-Loop ECLSS is essential to reducing resupply mass for long-duration manned missions; specifically focusing on water (H 2 O) which supplies H 2 for Sabatier via water electrolysis. Past ground test endeavors at Marshall Space Flight Center (MSFC) have attempted to recover H 2 from Sabatier-produced CH 4 using technologies such as carbon vapor deposition (CVD) and plasma pyrolysis. The byproducts of these technologies can act as a catalyst poison or reactor deadload to the Sabatier reactor. Hydrogen separation techniques must be utilized to maintain the Sabatier catalyst during gas recycling and must be scalable, non-energy intensive, and safe to operate in a habitation setting. Research indicated that metal-organic frameworks (MOFs) could meet these criteria and were tested for their capability to capture the various carbon-based gaseous products of CVD and plasma pyrolysis such as acetylene (C 2 H 2 ), ethylene (C 2 H 4 ), ethane (C 2 H 6 ), and carbon monoxide (CO) which would purify the hydrogen gas stream passing through the MOF. A sub-scale adsorption column was developed by Marshall Space Flight Center to test three MOF candidates against a synthetic gas mixture comprised of process-relevant carbonous gases and hydrogen to evaluate the separation capability of the MOFs. The results of the hydrogen separation capability, isothermal desorption capability, and demonstrated cyclic reuse of the MOF are presented in this paper.

Kagen Crawford↗

Elucidation of the organometallic vapor phase epitaxial growth mechanism for InP

A new technique for tracing the organometallic vapor epitaxial growth is reported. The pyrolysis of PH3, alone and in the presence of trimethylindium (TMIn), and of TMIn alone was studied by conducting the epitaxial growth of InP in D2 as the carrier gas, tracing growth reactions by mass spectrometric analysis of the product molecules. The TMIn alone pyrolyzes mostly homogeneously in the gas phase, while the PH3 pyrolysis is completely heterogeneous at the InP surface. Adding TMIn to PH3 results in a dramatic decrease in the pyrolysis temperature. PH3 molecules which interact with TMIn in the gas phase pyrolyze at temperatures as low as 250, and those decomposing without TMIn interaction pyrolyze at temperatures approximately 200 C higher. Similarly, the presence of PH3 lowers the TMIn pyrolysis temperature by at least 50 C. TMIn alone in D2 produces mainly CH3D molecules. For high PH3:TMIn ratios, CH4 is the only carbon-containing reaction product.

Buchan, N. I.↗

Fuel-rich catalytic combustion: A fuel processor for high-speed propulsion

Fuel-rich catalytic combustion of Jet-A fuel was studied over the equivalence ratio range 4.7 to 7.8, which yielded combustion temperatures of 1250 to 1060 K. The process was soot-free and the gaseous products were similar to those obtained in the iso-octane study. A carbon atom balance across the catalyst bed calculated for the gaseous products accounted for about 70 to 90 percent of the fuel carbon; the balance was condensed as a liquid in the cold trap. It was shown that 52 to 77 percent of the fuel carbon was C1, C2, and C3 molecules. The viability of using fuel-rich catalytic combustion as a technique for preheating a practical fuel to very high temperatures was demonstrated. Preliminary results from the scaled up version of the catalytic combustor produced a high-temperature fuel containing large amounts of hydrogen and carbon monoxide. The balance of the fuel was completely vaporized and in various stages of pyrolysis and oxidation. Visual observations indicate that there was no soot present.

Brabbs, Theodore A.↗

Fuel-rich catalytic combustion - A fuel processor for high-speed propulsion

Fuel-rich catalytic combustion of Jet-A fuel was studied over the equivalence ratio range 4.7 to 7.8, which yielded combustion temperatures of 1250 to 1060 K. The process was soot-free and the gaseous products were similar to those obtained in the iso-octane study. A carbon atom balance across the catalyst bed calculated for the gaseous products accounted for about 70 to 90 percent of the fuel carbon; the balance was condensed as a liquid in the cold trap. It was shown that 52 to 77 percent of the fuel carbon was C1, C2, and C3 molecules. The viability of using fuel-rich catalytic combustion as a technique for preheating a practical fuel to very high temperatuers was demonstrated. Preliminary results from the scaled up version of the catalytic combustor produced a high-temperature fuel containing large amounts of hydrogen and carbon monoxide. The balance of the fuel was completely vaporized and in various stages of pyrolysis and oxidation. Visual observations indicate that there was no soot present.

Brabbs, Theodore A.↗

Chemical-Vapor Deposition Of Silicon Carbide

Report describes experiments in chemical-vapor deposition of silicon carbide by pyrolysis of dimethyldichlorosilane in hydrogen and argon carrier gases. Directed toward understanding chemical-kinetic and mass-transport phenomena affecting infiltration of reactants into, and deposition of SiC upon, fabrics. Part of continuing effort to develop method of efficient and more nearly uniform deposition of silicon carbide matrix throughout fabric piles to make improved fabric/SiC-matrix composite materials.

Cagliostro, D. E.↗

Influence of Constituents on Creep Properties of SiC/SiC Composites

SiC-SiC composites are being considered as potential candidate materials for next generation turbine components such as combustor liners, nozzle vanes and blades because of their low density, high temperature capability, and tailorable mechanical properties. These composites are essentially fabricated by infiltrating matrix into a stacked array of fibers or fiber preform by one or a combination of manufacturing methods such as, Melt Infiltration (MI) of molten silicon metal, Chemical Vapor Infiltration (CVI), Polymer Infiltration and Pyrolysis (PIP). To understand the influence of constituents, the SiC-SiC composites fabricated by MI, CVI, and PIP methods were creep tested in air between 12000 and 14500 degrees Centigrade for up to 500 hours. The failed specimens were analyzed under a scanning electron microscope to assess damage mechanisms. Also, knowing the creep deformation parameters of the fiber and the matrix under the testing conditions, the creep behavior of the composites was modeled and compared with the measured data. The implications of the results on the long term durability of these composites will be discussed.

modeling↗

Creep and Cyclic Fatigue Durability of 3D Woven SiC/SiC Composites with (CVI+PIP) Hybrid Matrix

SiC-SiC composites are potential candidate materials for turbine components such as combustor liners, nozzle vanes and blades because of their low density, high temperature capability, and tailorable mechanical properties. The first generation of SiC-SiC composites fabricated by melt infiltration are being introduced in current engines. These materials are limited to 1315 degrees Centigrade applications because of the presence of residual silicon in the SiC matrix. Currently there is an increasing interest in developing SiC-SiC composites without silicon for structural aerospace applications above 1315 degrees Centigrade. The developmental 3D woven SiC-SiC composites with Chemical Vapor Infiltration plus Polymer Impregnation and Pyrolysis (CVI+PIP) hybrid matrix show potential for 1482 degrees Centigrade applications. In this study 3D woven SiC-SiC composite specimens were creep tested at 1482 degrees Centigrade at different stress levels until failure or for 1000 hours without failure. The failed specimens were analyzed for under a scanning electron microscope to assess the damage mechanisms. The creep data of 3D woven SiC-SiC composites with (CVI+PIP) hybrid matrix were compared with those of full CVI SiC-SiC composites and sintered SiC from the literature. The potential benefits limitations and durability of 3D woven SiC-SiC composites for turbine applications will be discussed.

creep durability↗

Characterization of SiC/SiC Composites Subjected to Sequential Tensile Creep and Dwell Fatigue in Air under Thermal Gradient Conditions

Uncoated SiC/SiC composites, with 2D and 3D fiber architectures, were investigated under steady state thermal gradient conditions with sequential tensile creep and dwell fatigue. Melt infiltration (MI), chemical vapor infiltration (CVI), polymer impregnation and pyrolysis (PIP), and hybrid (CVI and PIP) techniques were used to fabricate ceramic matrix composites (CMCs) with a 2D balanced fiber architecture. CMCs with 3D fiber weaves were also fabricated using MI and hybrid methods. Steady state through the thickness thermal gradients were generated for the tensile specimens using laser heating on the front (hot side) and forced air cooling on the back (cold side). Hot side and cold side temperatures of 2400 and 2200 °F, respectively, were used for testing CMCs fabricated with the MI process, whereas hot side and cold side temperatures of 2700 and 2400 °F, respectively, were used for CMCs fabricated with CVI, PIP, and hybrid processes. Each CMC specimen was initially tested under tensile creep at 69 MPa (10 ksi) for 80 hours, which was then followed by tensile dwell fatigue testing at a maximum stress of 69 MPa (10 ksi) for another 80 hours for a total of 160 hours. This type of sequential tensile creep followed by tensile dwell fatigue testing was performed to ascertain the integrity of uncoated CMCs under steady state thermal gradient conditions. Tensile creep and dwell fatigue test results, generated under steady state thermal gradient conditions on different types of SiC/SiC composites, are compared with corresponding creep behaviors observed under isothermal conditions to determine the influence of both monotonic creep (static fatigue) and dwell fatigue on accumulated strains and deformation behaviors of the CMCs.

Kalluri, Sreeramesh↗

Vacuum Pyrolysis and Related ISRU Techniques

A number of ISRU-related techniques have been developed at NASA Goddard Space Flight Center. The focus of the team has been on development of the vacuum pyrolysis technique for the production of oxygen from the lunar regolith. However, a number of related techniques have also been developed, including solar concentration, solar heating of regolith, resistive heating of regolith, sintering, regolith boiling, process modeling, parts manufacturing, and instrumentation development. An initial prototype system was developed to vaporize regolith simulants using a approx. l square meter Fresnel lens. This system was successfully used to vaporize quantities of approx. lg, and both mass spectroscopy of the gasses produced and Scanning Electron Microscopy (SEM) of the slag were done to show that oxygen was produced. Subsequent tests have demonstrated the use of a larger system With a 3.8m diameter reflective mirror to vaporize the regolith. These results and modeling of the vacuum pyrolysis reaction have indicated that the vaporization of the oxides in the regolith will occur at lower temperature for stronger vacuums. The chemical modeling was validated by testing of a resistive heating system that vaporized quantities of approx. 10g of MLS-1A. This system was also used to demonstrate the sintering of regolith simulants at reduced temperatures in high vacuum. This reduction in the required temperature prompted the development of a small-scale resistive heating system for application as a scientific instrument as well as a proof-of principle experiment for oxygen production.

Cardiff, Eric H.↗