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NASA NTRS1999

Oxygen Generator System Mars In-Situ Propellant Production Precursor Flight

The 2001 Lander to Mars will carry the first ever In situ Resource Utilization (ISRU) payload to Mars. This payload, the Mars In-situ Propellant production Precursor (MIP), will demonstrate a variety of technologies that will be required for future ISRU Mars indigenous material processing plant designs. One of those technologies is that of extracting oxygen from the predominantly carbon dioxide atmosphere of Mars, a prerequisite for future sample return and human missions to Mars. The Oxygen Generator Subsystem (OGS) portion of the MIP will demonstrate this and is the focus of this paper. The primary objective of the OGS is to demonstrate the production of oxygen from Mars atmospheric gases. Secondary objectives are to measure the performance and reliability of oxygen generation hardware in actual mission environments over an extended time. Major constraints on the OGS design came from several sources. The Lander provides power to the system from solar power that is harnessed by photovoltaic arrays. This limited OGS to daytime only operations (six to eight hours) and a maximum power of 15W. The reliance on solar power necessitated thermal cycling of the OGS between Mars ambient and OGS operating temperatures. The Lander also limited the total mass of the MIP payload to 7.5 kg with a correspondingly small volume, and the OGS was one of six experiments in the MIP Mass and volume were to be minimized. Another constraint was cost. Mission funding, as always, was tight. Cost was to be minimized. In short the OGS design had to be low power (<15 Watts), low mass (1 kg), low volume, low cost, and be capable of cyclical operations for an extended stay on Mars. After extensive research, a zirconia based solid oxide electrolyzer design was selected.

Sridhar, K. R.↗

NASA NTRS1998

Particle Engulfment and Pushing by Solidifying Interfaces LMS Mission Results

Results of the directional solidification experiments on Particle Engulfment and Pushing by Solidifying Interfaces (PEP) conducted on the space shuttle Columbia are reported. The experiment was manifested as part of The Life and Microgravity Science Mission. Two pure aluminum (99.999%) 9 mm cylindrical rods, loaded with about 2 vol.% 500 microns diameter zirconia particles were melted and directionally solidified in the microgravity (micro-g) environment of the shuttle. The particles were non-reactive with the matrices within the temperature range of interest. The experiments were conducted such as to insure a planar solid/liquid interface during solidification. Two different cartridge - crucible - sample designs were used: a spring-piston and expansion void. Both resulted in sound samples. Samples were evaluated post-flight for soundness by X-ray computer tomography (XCT).

Juretzko, Frank R.↗

NASA NTRS1998

Particle Engulfment and Pushing by Solidifying Interfaces: Micro-Gravity Experiments and Theoretical Analysis - Pt. 2

Results of the directional solidification experiments on Particle Engulfment and Pushing by Solidifying Interfaces (PEP) conducted on the space shuttle Columbia during the Life and Microgravity Science Mission are reported. Two pure aluminum (99.999%) 9 mm cylindrical rods, loaded with about 2 vol.% 500 micrometers diameter zirconia particles were melted and resolidified in the microgravity (microg) environment of the shuttle. One sample was processed at step-wise increased solidification velocity, while the other at step-wise decreased velocity. It was found that a pushing-to-engulfment transition (PET) occurred in the velocity range of 0.5 to 1 micrometers. This is smaller than the ground PET velocity of 1.9 to 2.4 micrometers. This demonstrates that natural convection increases the critical velocity. A previously proposed analytical model for PEP was further developed. A major effort to identify and produce data for the surface energy of various interfaces required for calculation was undertaken. The predicted critical velocity for PET was of 0.775 micrometers/s.

Stefanescu, Doru M.↗

NASA NTRS1999

Chemical Vapor Deposition of Turbine Thermal Barrier Coatings

Ceramic thermal barrier coatings extend the operating temperature range of actively cooled gas turbine components, therefore increasing thermal efficiency. Performance and lifetime of existing ceram ic coatings are limited by spallation during heating and cooling cycles. Spallation of the ceramic is a function of its microstructure, which is determined by the deposition method. This research is investigating metalorganic chemical vapor deposition (MOCVD) of yttria stabilized zirconia to improve performance and reduce costs relative to electron beam physical vapor deposition. Coatings are deposited in an induction-heated, low-pressure reactor at 10 microns per hour. The coating's composition, structure, and response to the turbine environment will be characterized.

Haven, Victor E.↗

NASA NTRS1998

In-Space Rapid Manufacturing

In-space manufacturing objectives are: (1) Develop and demonstrate capability to directly fabricate components in space using rapid prototyping technology - ceramics (alumina, silicon nitride, zirconia), metallics (stainless, inconel, etc.), high strength/temperature plastics (PEEK). and ABS plastics (starting point). (2) Perform material science experiments on rapid prototyping candidate materials in microgravity.

Cooper, Kenneth G.↗

NASA NTRS2000

A Dynamic Model for the Interaction Between an Insoluble Particle and an Advancing Solid/Liquid Interface

Most models that describe the interaction of an insoluble particle with an advancing solid-liquid interface are based on the assumption of steady state. However, as demonstrated by experimental work, the process does not reach steady state until the particle is pushed for a while by the interface. In this work, a dynamic mathematical model was developed. The dynamic model demonstrates that this interaction is essentially non-steady state and that steady state eventually occurs only when solidification is conducted at sub-critical velocities. The model was tested for three systems: aluminum-zirconia particles, succinonitrilepolystyrene particles, and biphenyl-glass particles. The calculated values for critical velocity of the pushing/engulfment transition were in same range with the experimental ones.

Catalina, A. V.↗

NASA NTRS1999

Thermal Shock Behavior of Single Crystal Oxide Refractive Concentrators for High Temperatures Solar Thermal Propulsion

Single crystal oxides such as yttria-stabilized zirconia (Y2O3-ZrO2), yttrium-aluminum-garnet (Y3Al5O12, or YAG), magnesium oxide (MgO) and sapphire (Al2O3) have been considered as refractive secondary concentrator materials for high temperature solar propulsion applications. However, thermal mechanical reliability of the oxide components in severe thermal environments during space mission sun/shade transitions is of great concern. In this paper, critical mechanical properties of these oxide crystals are determined by the indentation technique. Thermal shock resistance of the oxides is evaluated using a high power CO, laser under high temperature-high thermal gradients. Thermal stress fracture behavior and failure mechanisms of these oxide materials are investigated under various temperature and heating conditions.

Zhu, Dongming↗

NASA NTRS2001

Oxidation of ZrB2-SiC

In this paper the oxidation behavior of ZrB2-20 vol% SiC is examined. Samples were exposed in stagnant air in a zirconia furnace (Deltech, Inc.) at temperatures of 1327, 1627, and 1927 C for ten ten-minute cycles. Samples were removed from the furnace after one, five, and ten cycles. Oxidized material was characterized by mass change when possible, x-ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive spectroscopy (EDS). Oxidation kinetics, oxide scale development, and matrix recession were monitored as a function of time and temperature. Oxidation and recession rates of ZrB2 - 20 vol% SiC were adequately modeled by parabolic kinetics. Oxidation rates of this material are rapid, allowing only very short-term application in air or other high oxygen partial pressure environments.

Opila, Elizabeth J.↗

NASA NTRS2000

Effect of Hf Additions to Pt Aluminide Bond Coats on EB-PVD TBC Life

Small Hf additions were incorporated into a Pt aluminide coating during chemical vapor deposition (CVD) on single crystal RENE N5 substrates. Standard yttria-stabilized zirconia top coats were subsequently deposited onto the coated substrates by electron beam-physical vapor deposition (EB-PVD). The coated substrates underwent accelerated thermal cycle testing in a furnace at a temperature in excess of 1121 C (2050 F) (45 minute hot exposure, 15 minute cool to approximately 121 C (250 F)) until the thermal barrier coating (TBC) failed by spallation. Incorporating Hf in the bond coat increased the TBC life by slightly more than three times that of a baseline coating without added Hf. Scanning electron microscopy of the spalled surfaces indicated that the presence of the Hf increased the adherence of the thermally grown alumina to the Pt aluminide bond coat. The presence of oxide pegs growing into the coating from the thermally grown alumina may also partially account for the improved TBC life by creating a near-surface layer with a graded coefficient of thermal expansion.

Nesbitt, James↗

NASA NTRS2000

A Survey of Alternative Oxygen Production Technologies

Utilization of the Martian atmosphere for the production of fuel and oxygen has been extensively studied. The baseline fuel production process is a Sabatier reactor, which produces methane and water from carbon dioxide and hydrogen. The oxygen produced from the electrolysis of the water is only half of that needed for methane-based rocket propellant, and additional oxygen is needed for breathing air, fuel cells and other energy sources. Zirconia electrolysis cells for the direct reduction of CO2 are being developed as an alternative means of producing oxygen, but present many challenges for a large-scale oxygen production system. The very high operating temperatures and fragile nature of the cells coupled with fairly high operating voltages leave room for improvement. This paper will survey alternative oxygen production technologies, present data on operating characteristics, materials of construction, and some preliminary laboratory results on attempts to implement each.

Lueck, Dale E.↗

NASA NTRS2001

Calculation of Phase Equilibria in the Y2O3-Yb2O3-ZrO2 System

Rare earth oxide stabilized zirconias find a wide range of applications. An understanding of phase equilibria is essential to all applications. In this study, the available phase boundary data and thermodynamic data is collected and assessed. Calphad-type databases are developed to completely describe the Y2O3-ZrO2, Yb2O3-ZrO2, and Y2O3-Yb2O3 systems. The oxide units are treated as components and regular and subregular solution models are used. The resultant calculated phase diagrams show good agreement with the experimental data. Then the binaries are combined to form the database for the Y2O3-Yb2O3-ZrO2 psuedo-ternary.

Jacobson, Nathan S.↗

NASA NTRS2002

Quasistatic vs. Dynamic Modulus Measurements Of Plasma-Sprayed Thermal Barrier Coatings

Plasma-sprayed 8wt% yttria-stabilized zirconia (8YSZ) thermal barrier coatings (TBCs) have been demonstrated to exhibit nonlinear hysteretic elastic behavior by quasistatic cyclic compression and cylindrical punch indentation measurements. In particular, the instantaneous (tangential) elastic modulus increases with applied stress and exhibits significant hysteresis during cycling. Sound velocity (dynamic) measurements also show an increase in TBC modulus with applied compressive stress, but in contrast show no significant hysteresis for the modulus during cycling. The nonlinear elastic behavior of the TBCs evidenced by these tests is attributed to coating compaction and internal sliding. The differences between the quasistatic and dynamic measurements are explained by the relative absence of the effect of internal sliding in the dynamic modulus measurements. By incorporating short load reversals into the larger loading cycle and measuring the instantaneous modulus at the start of each load reversal, the effects of internal sliding can be substantially reduced in the quasistatic measurements, and the resulting modulus values show good agreement with the modulus values determined by dynamic sound velocity measurements.

Eldridge, J. I.↗

NASA NTRS1999

Information Technology and the Autonomous Control of a Mars In-Situ Propellant Production System

With the rapidly increasing performance of information technology, i.e., computer hardware and software systems, as well as networks and communication systems, a new capability is being developed that holds the clear promise of greatly increased exploration capability, along with dramatically reduced design, development, and operating costs. These new intelligent systems technologies, utilizing knowledge-based software and very high performance computer systems, will provide new design and development tools, scheduling mechanisms, and vehicle and system health monitoring capabilities. In addition, specific technologies such as neural nets will provide a degree of machine intelligence and associated autonomy which has previously been unavailable to the mission and spacecraft designer and to the system operator. One of the most promising applications of these new information technologies is to the area of in situ resource utilization. Useful resources such as oxygen, compressed carbon dioxide, water, methane, and buffer gases can be extracted and/or generated from planetary atmospheres, such as the Martian atmosphere. These products, when used for propulsion and life-support needs can provide significant savings in the launch mass and costs for both robotic and crewed missions. In the longer term the utilization of indigenous resources is an enabling technology that is vital to sustaining long duration human presence on Mars. This paper will present the concepts that are currently under investigation and development for mining the Martian atmosphere, such as temperature-swing adsorption, zirconia electrolysis etc., to create propellants and life-support materials. This description will be followed by an analysis of the information technology and control needs for the reliable and autonomous operation of such processing plants in a fault tolerant manner, as well as the approach being taken for the development of the controlling software. Finally, there will be a brief discussion of the verification and validation process so crucial to the implementation of mission-critical software.

Gross, Anthony R.↗

NASA NTRS2002

Processing and Mechanical Properties of Various Zirconia/Alumina Composites for Fuel Cell Applications

Various electrolyte materials for solid oxide fuel cells were fabricated by hot pressing 10 mol% yttria-stabilized zirconia (10-YSZ) reinforced with two different forms of alumina, particulates and platelets, each containing 0 to 30 mol% alumina. Flexure strength and fracture toughness of both particulate and platelet composites at ambient temperature increased with increasing alumina content, reaching a maximum at 30 mot% alumina. For a given alumina content, strength of particulate composites was greater than that of platelet composites, whereas, the difference in fracture toughness between the two composite systems was negligible. No virtual difference in elastic modulus and density was observed for a given alumina content between particulate and platelet composites. Thermal cycling up to 10 cycles between 200 to 1000 C did not show any effect on strength degradation of the 30 mol% platelet composites, indicative of negligible influence of CTE mismatches between YSZ matrix and alumina grains.

Choi, Sung R.↗

NASA NTRS2002

Mullite+CAS Bond Coat for Environmental Barrier Coatings for Si-Based Ceramics

Current environmental barrier coatings (EBCs) for silicon-based ceramics consist of a bond coat and a top coat. Mullite bond coat modified by adding low CTE glass ceramics, such as BSAS (xBaO.1xSrO.Al2O3.2SiO2) or CAS (CaO.Al2O3.2SiO2), was developed in the NASA Enabling Propulsion Materials (EPM) Program. EBCs based on mullite+CAS bond coat were characterized using high steam thermal cycling test and high steam isothermal thermogravemitry (TGA) at 1225 C - 13,000 C. The Mullite+CAS bond coat showed far superior durability compared to mullite bond coat, due to enhanced crack resistance. A BSAS top coat provided further improved durability compared to EBCs with a yttria-stabilized zirconia (YSZ) top coat. Still further improvement in the durability was achieved by adding a silicon bond coat between the mullite and the substrate. However, the silicon/mullite+CAS/BSAS EBC showed inferior long-term durability compared to the current state-of-the art EBC (silicon/mullite+BSAS/BSAS EBC), presumably due to the higher CAS-silica chemical reactivity.

Lee, Kang N.↗

NASA NTRS2002

Environmental Barrier Coatings Having a YSZ Top Coat

Environmental barrier coatings (EBCs) with a Si bond coat, a yttria-stabilized zirconia (YSZ) top coat, and various intermediate coats were investigated. EBCs were processed by atmospheric pressure plasma spraying. The EBC durability was determined by thermal cycling tests in water vapor at 1300 C and 1400 C, and in air at 1400 C and 1500 C. EBCs with a mullite (3Al2O3 (dot) 2SiO2) + BSAS (1 - xBaO (dot) xSrO (dot) Al2O3 (dot) 2SiO2) intermediate coat were more durable than EBCs with a mullite intermediate coat, while EBCs with a mullite/BSAS duplex intermediate coat resulted in inferior durability. The improvement with a mullite + BSAS intermediate coat was attributed to enhanced compliance of the intermediate coat due to the addition of a low modulus BSAS second phase. Mullite + BSAS/YSZ and BSAS/YSZ interfaces produced a low melting (less than 1400 C) reaction product, which is expected to degrade the EBC performance by increasing the thermal conductivity. EBCs with a mullite + BSAS / graded mullite + YSZ intermediate coat showed the best durability among the EBCs investigated in this study. This improvement was attributed to diffused CTE (Coefficient of Thermal Expansion) mismatch stress and improved chemical stability due to the compositionally graded mullite+YSZ layer.

Lee, Kang N.↗

NASA NTRS2003

Pt and Hf Additions to NiAl Bond Coats and Their Effect on the Lifetime of Thermal Barrier Coatings

The lifetimes of thermal barrier coatings (TBC's) with various NiAlPt(HfZr) bond coats were determined by cyclic oxidation testing at 1163 C (2125 F). The bond coats were sprayed from powders by low pressure plasma spraying onto Rene N5 superalloy substrates. Yttria stabilized zirconia (8YSZ) top coats were applied by air plasma spraying. Surprisingly, there was not a strong correlation between TBC lifetime and Pt or Hf content although Zr additions decreased lifetimes. TBC failure morphologies and bond coat microstructures were examined and are discussed with respect to the bond coat compositions.

Nesbitt, J. A.↗

NASA NTRS2002

Health Monitoring of Thermal Barrier Coatings by Mid-Infrared Reflectance

Mid-infrared (MIR) reflectance is shown to be a powerful tool for monitoring the integrity of 8wt% yttria-stabilized zirconia (8YSZ) thermal barrier coatings (TBCs). Because of the translucent nature of plasma-sprayed 8YSZ TBCs, particularly at MIR wavelengths (3 to 5 microns), measured reflectance does not only originate from the TBC surface, but contains strong contributions from internal scattering within the coating as well as reflectance from the underlying TBC/substrate interface. Therefore, changes in MIR reflectance measurements can be used to monitor the progression of TBC delamination. In particular, MIR reflectance is shown to reproducibly track the progression of TBC delamination produced by repeated thermal cycling (to 1163 C) of plasma-sprayed 8YSZ TBCs on Rene N5 superalloy substrates. To understand the changes in MIR reflectance with the progression of a delamination crack network, a four-flux scattering model is used to predict the increase in MIR reflectance produced by the introduction of these cracks.

Eldridge, J. I.↗