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NASA NTRS2013

Fabrication Methods for Adaptive Deformable Mirrors

Previously, it was difficult to fabricate deformable mirrors made by piezoelectric actuators. This is because numerous actuators need to be precisely assembled to control the surface shape of the mirror. Two approaches have been developed. Both approaches begin by depositing a stack of piezoelectric films and electrodes over a silicon wafer substrate. In the first approach, the silicon wafer is removed initially by plasmabased reactive ion etching (RIE), and non-plasma dry etching with xenon difluoride (XeF2). In the second approach, the actuator film stack is immersed in a liquid such as deionized water. The adhesion between the actuator film stack and the substrate is relatively weak. Simply by seeping liquid between the film and the substrate, the actuator film stack is gently released from the substrate. The deformable mirror contains multiple piezoelectric membrane layers as well as multiple electrode layers (some are patterned and some are unpatterned). At the piezolectric layer, polyvinylidene fluoride (PVDF), or its co-polymer, poly(vinylidene fluoride trifluoroethylene P(VDF-TrFE) is used. The surface of the mirror is coated with a reflective coating. The actuator film stack is fabricated on silicon, or silicon on insulator (SOI) substrate, by repeatedly spin-coating the PVDF or P(VDFTrFE) solution and patterned metal (electrode) deposition. In the first approach, the actuator film stack is prepared on SOI substrate. Then, the thick silicon (typically 500-micron thick and called handle silicon) of the SOI wafer is etched by a deep reactive ion etching process tool (SF6-based plasma etching). This deep RIE stops at the middle SiO2 layer. The middle SiO2 layer is etched by either HF-based wet etching or dry plasma etch. The thin silicon layer (generally called a device layer) of SOI is removed by XeF2 dry etch. This XeF2 etch is very gentle and extremely selective, so the released mirror membrane is not damaged. It is possible to replace SOI with silicon substrate, but this will require tighter DRIE process control as well as generally longer and less efficient XeF2 etch. In the second approach, the actuator film stack is first constructed on a silicon wafer. It helps to use a polyimide intermediate layer such as Kapton because the adhesion between the polyimide and silicon is generally weak. A mirror mount ring is attached by using adhesive. Then, the assembly is partially submerged in liquid water. The water tends to seep between the actuator film stack and silicon substrate. As a result, the actuator membrane can be gently released from the silicon substrate. The actuator membrane is very flat because it is fixed to the mirror mount prior to the release. Deformable mirrors require extremely good surface optical quality. In the technology described here, the deformable mirror is fabricated on pristine substrates such as prime-grade silicon wafers. The deformable mirror is released by selectively removing the substrate. Therefore, the released deformable mirror surface replicates the optical quality of the underlying pristine substrate.

Toda, Risaku↗

NASA NTRS1976

Laser Doppler systems in pollution monitoring

The paper reports on a program undertaken to determine the feasibility of using a laser Doppler velocimeter (LDV) to measure smoke-stack gas exit velocity, particulate concentration, and mass flow. Measurements made with a CO2 laser Doppler radar system at a coal-burning power plant are compared with in-stack measurements made by a pitot tube. The operational principles of a LDV are briefly described along with the system employed in the present study. Data discussed include typical Doppler spectra from smoke-stack effluents at various laser elevation angles, the measured velocity profile across the stack exit, and the LDV-measured exit velocity as a function of the exit velocity measured by the in-stack instrument. The in-stack velocity is found to be about 14% higher than the LDV velocity, but this discrepancy is regarded as a systematic error. In general, linear relationships are observed between the laser data, the exit velocity, and the particulate concentration. It is concluded that an LDV has the capability of determining both the mass concentration and the mass flow from a power-plant smoke stack.

Miller, C. R.↗

NASA NTRS1985

Develop and test fuel cell powered on-site integrated total energy systems: Phase 3, full-scale power plant development

A 25 cell stack of the 13 inch x 23 inch cell size (about 4kW) remains on test after 6000 hours, using simulated reformate fuel. A similar stack was previously shut down after 7000 hours on load. These tests were carried out for the purpose of assessing the durability of fuel cell stack components developed through the end of 1983. In light of the favorable results obtained, a 25kW stack that will contain 175 cells of the same size is being constructed using the same technology base. The components for the 25kW stack have been completed. A methanol steam reformer with a design output equivalent to 50kW has been constructed to serve as a hydrogen generator for the 25kW stack. This reformer and the balance of the fuel processing sub system are currently being tested and debugged. The stack technology development program focused on cost reduction in bipolar plates, nonmetallic cooling plates, and current collecting plates; more stable cathode catalyst support materials; more corrosion resistant metal hardware; and shutdown/start up tolerance.

Kaufman, A.↗

NASA NTRS1986

Develop and test fuel cell powered on site integrated total energy sysems: Phase 3: Full-scale power plant development

A 25-cell stack of the 13 inch x 23 inch cell size (about 4kW) remains on test after 8300 hours, using simulated reformate fuel. A similar stack was previously shut down after 7000 hours on load. These tests have been carried out for the purpose of assessing the durability of fuel cell stack components developed through the end of 1983. A 25kW stack containing 175 cells of the same size and utilizing a technology base representative of the 25-cell stacks has been constructed and is undergoing initial testing. A third 4kW stack is being prepared, and this stack will incorporate several new technology features.

Kaufman, A.↗

NASA NTRS2012

Pressure Dome for High-Pressure Electrolyzer

A high-strength, low-weight pressure vessel dome was designed specifically to house a high-pressure [2,000 psi (approx. = 13.8 MPa)] electrolyzer. In operation, the dome is filled with an inert gas pressurized to roughly 100 psi (approx. = 690 kPa) above the high, balanced pressure product oxygen and hydrogen gas streams. The inert gas acts to reduce the clamping load on electrolyzer stack tie bolts since the dome pressure acting axially inward helps offset the outward axial forces from the stack gas pressure. Likewise, radial and circumferential stresses on electrolyzer frames are minimized. Because the dome is operated at a higher pressure than the electrolyzer product gas, any external electrolyzer leak prevents oxygen or hydrogen from leaking into the dome. Instead the affected stack gas stream pressure rises detectably, thereby enabling a system shutdown. All electrical and fluid connections to the stack are made inside the pressure dome and require special plumbing and electrical dome interfaces for this to be accomplished. Further benefits of the dome are that it can act as a containment shield in the unlikely event of a catastrophic failure. Studies indicate that, for a given active area (and hence, cell ID), frame outside diameter must become ever larger to support stresses at higher operating pressures. This can lead to a large footprint and increased costs associated with thicker and/or larger diameter end-plates, tie-rods, and the frames themselves. One solution is to employ rings that fit snugly around the frame. This complicates stack assembly and is sometimes difficult to achieve in practice, as its success is strongly dependent on frame and ring tolerances, gas pressure, and operating temperature. A pressure dome permits an otherwise low-pressure stack to operate at higher pressures without growing the electrolyzer hardware. The pressure dome consists of two machined segments. An O-ring is placed in an O-ring groove in the flange of the bottom segment and is trapped by the flange on the top dome segment when these components are bolted together with high-strength bolts. The pressure dome has several unique features. It is made (to ASME Pressure Vessel guidelines) in a high-strength aluminum alloy with the strength of stainless steel and the weight benefits of aluminum. The flange of the upper dome portion contains specially machined flats for mounting the dome, and other flats dedicated to the special feedthroughs for electrical connections. A pressure dome can be increased in length to house larger stacks (more cells) of the same diameter with the simple addition of a cylindrical segment. To aid in dome assembly, two stainless steel rings are employed. One is used beneath the heads of the high-strength bolts in lieu of individual hardened washers, and another is used instead of individual nuts. Like electrolyzers could be operated at low or high pressures simply by operating the electrolyzer outside or inside a pressurized dome.

Norman, Timothy↗

NASA NTRS2015

Simplified Methodology to Estimate the Maximum Liquid Helium (LHe) Cryostat Pressure from a Vacuum Jacket Failure

The aircraft-based Stratospheric Observatory for Infrared Astronomy (SOFIA) is a platform for multiple infrared astronomical observation experiments. These experiments carry sensors cooled to liquid helium temperatures. The liquid helium supply is contained in large (i.e., 10 liters or more) vacuum-insulated dewars. Should the dewar vacuum insulation fail, the inrushing air will condense and freeze on the dewar wall, resulting in a large heat flux on the dewar's contents. The heat flux results in a rise in pressure and the actuation of the dewar pressure relief system. A previous NASA Engineering and Safety Center (NESC) assessment provided recommendations for the wall heat flux that would be expected from a loss of vacuum and detailed an appropriate method to use in calculating the maximum pressure that would occur in a loss of vacuum event. This method involved building a detailed supercritical helium compressible flow thermal/fluid model of the vent stack and exercising the model over the appropriate range of parameters. The experimenters designing science instruments for SOFIA are not experts in compressible supercritical flows and do not generally have access to the thermal/fluid modeling packages that are required to build detailed models of the vent stacks. Therefore, the SOFIA Program engaged the NESC to develop a simplified methodology to estimate the maximum pressure in a liquid helium dewar after the loss of vacuum insulation. The method would allow the university-based science instrument development teams to conservatively determine the cryostat's vent neck sizing during preliminary design of new SOFIA Science Instruments. This report details the development of the simplified method, the method itself, and the limits of its applicability. The simplified methodology provides an estimate of the dewar pressure after a loss of vacuum insulation that can be used for the initial design of the liquid helium dewar vent stacks. However, since it is not an exact tool, final verification of the dewar pressure vessel design requires a complete, detailed real fluid compressible flow model of the vent stack. The wall heat flux resulting from a loss of vacuum insulation increases the dewar pressure, which actuates the pressure relief mechanism and results in high-speed flow through the dewar vent stack. At high pressures, the flow can be choked at the vent stack inlet, at the exit, or at an intermediate transition or restriction. During previous SOFIA analyses, it was observed that there was generally a readily identifiable section of the vent stack that would limit the flow – e.g., a small diameter entrance or an orifice. It was also found that when the supercritical helium was approximated as an ideal gas at the dewar condition, the calculated mass flow rate based on choking at the limiting entrance or transition was less than the mass flow rate calculated using the detailed real fluid model2. Using this lower mass flow rate would yield a conservative prediction of the dewar’s wall heat flux capability. The simplified method of the current work was developed by building on this observation.

Ungar, Eugene K.↗

NASA NTRS1975

A theoretical/experimental program to develop active optical pollution sensors: Quantitative remote Raman lidar measurements of pollutants from stationary sources

Typical pollutant gas concentrations at the stack exits of stationary sources can be estimated to be about 500 ppm under the present emission standards. Raman lidar has a number of advantages which makes it a valuable tool for remote measurements of these stack emissions. Tests of the Langley Research Center Raman lidar at a calibration tank indicate that night measurements of SO2 concentrations and stack opacity are possible. Accuracies of 10 percent are shown to be achievable from a distance of 300 m within 30 min integration times for 500 ppm SO2 at the stack exits. All possible interferences were examined quantitatively (except for the fluorescence of aerosols in actual stack emissions) and found to have negligible effect on the measurements. An early test at an instrumented stack is strongly recommended.

Poultney, S. K.↗

NASA NTRS1980

Cell module and fuel conditioner

The computer code for the detailed analytical model of the MK-2 stacks is described. An ERC proprietary matrix is incorporated in the stacks. The mechanical behavior of the stack during thermal cycles under compression was determined. A 5 cell stack of the MK-2 design was fabricated and tested. Designs for the next three stacks were selected and component fabrication initiated. A 3 cell stack which verified the use of wet assembly and a new acid fill procedure were fabricated and tested. Components for the 2 kW test facility were received or fabricated and construction of the facility is underway. The definition of fuel and water is used in a study of the fuel conditioning subsystem. Kinetic data on several catalysts, both crushed and pellets, was obtained in the differential reactor. A preliminary definition of the equipment requirements for treating tap and recovered water was developed.

Hoover, D. Q., Jr.↗

NASA NTRS1985

Develop and test fuel cell powered on-site integrated total energy systems: Phase 3, full-scale power plant development

Two 25 cell stacks of the 13 inch x 23 inch cell size (about 4kW) remain on test after 4000 hours and 2900 hours, respectively, using simulated reformate fuel. These tests are focusing on the durability of fuel cell stack components developed through the end of 1983. Also, these stacks are serving as forerunners of a 25kW stack that will contain 175 cells of the same size and will employ the same technology base. The stack technology development program has focused on a new, low cost bipolar plate edge seal technique and evaluation of advanced cathode catalysts, an electrolyte replenishment system, and nonmetallic cooling plates in small stacks.

Kaufman, A.↗

NASA NTRS2004

Evaporator Development for an Evaporative Heat Pipe System

As fossil fuel resources continue to deplete, research for alternate power sources continues to develop. One of these alternate technologies is fuel cells. They are a practical fuel source able to provide significant amounts of power for applications from laptops to automobiles and their only byproduct is water. However, although this technology is over a century old and NASA has been working with it since the early 1960 s there is still room for improvement. The research I am involved in at NASA's Glenn Research Center is focusing on what is called a regenerative fuel cell system. The unique characteristic of this type of system is that it used an outside power source to create electrolysis of the water it produces and it then reuses the hydrogen and oxygen to continue producing power. The advantage of this type of system is that, for example, on space missions it can use solar power to recharge its gas supplies between periods when the object being orbited blocks out the sun. This particular system however is far from completion. This is because of the many components that are required to make up a fuel cell that need to be tested individually. The specific part of the system that is being worked on this summer of 2004 is the cooling system. The fuel cell stack, that is the part that actually creates the power, also produces a lot of heat. When not properly cooled, it has been known to cause fires which, needless to say are not conducive to the type of power that is trying to be created. In order to cool the fuel cell stack in this system we are developing a heat pipe cooling system. One of the main components of a heat pipe cooling system is what is known as the evaporator, and that is what happens to be the part of the system we are developing this summer. In most heat pipe systems the evaporator is a tube in which the working fluid is cooled and then re-circulated through the system to absorb more heat energy from the fuel cell stack. For this system, instead of a tube, the evaporator is made up of a stack-up of screen material and absorbent membranes inside a stainless steel shell and held together by a film adhesive and epoxy. There is an initial design for this flat plate evaporator, however is has not yet been made. The components of the stack-up are known, so all testing is focused on how it will all go together. This includes finding an appropriate epoxy to make the evaporator conductive all the way through and finding a way to hold the required tight tolerances as the stainless steel outer shell is put together. By doing the tests on smaller samples of the stack-ups and then testing the fill size component, the final flat plate evaporator will reach its final design so that research can continue on other parts of the regenerative fue1 cell system, and another step in the improvement of fue1 cell technology can be made.

Peters, Leigh C.↗

NASA NTRS2004

Progress in High Power Density SOFC Material Development for Aerospace Applications

Solid oxide fuel cell (SOFC) systems for aircraft applications require order of magnitude increase in specific power density and long life under aircraft operating conditions. Advanced SOFC materials and fabrication processes are being developed at NASA GRC to increase specific power density and durability of SOFC cell and stack. Initial research efforts for increasing specific power density are directed toward increasing the operating temperature for the SOFC system and reducing the weight of the stack. While significant research is underway to develop anode supported SOFC system operating at temperatures in the range of 650 - 850 C for ground power generation applications, such temperatures may not yield the power densities required for aircraft applications. For electrode-supported cells, SOFC stacks with power densities greater than 1.0 W/sq cm are favorable at temperatures in excess of 900 C. The performance of various commercial and developmental anode supported cells is currently being evaluated in the temperature range of 900 to 1000 C to assess the performance gains and materials reliability. The results from these studies will be presented. Since metal interconnects developed for lower temperature operation are not practical at these high temperatures, advanced perovskite based ceramic interconnects with high electronic conductivity and lower sintering temperatures are being developed. Another option for increasing specific power density of SOFC stacks is to decrease the stack weight. Since the interconnect contributes to a significant portion of the stack weight, considerable weight benefits can be derived by decreasing its thickness. Eliminating the gas channels in the interconnect by engineering the pore structure in both anode and cathode can offer significant reduction in thickness of the ceramic interconnect material. New solid oxide fuel cells are being developed with porous engineered electrode supported structures with a 10 - 20 micron thin electrolyte. The performance data for advanced SOFC cells with engineered porosity in both electrodes will be presented.

Cable, Thomas L.↗

NASA NTRS2004

Bearingless Switched-Reluctance Motor Improved

The Morrison rotor, named after its inventor, is a hybrid rotor for use in a switched reluctance electric motor. The motor is characterized as bearingless in the sense that it does not rely on conventional mechanical bearings: instead, it functions as both a magnetic bearing and a motor. Bearingless switched-reluctance motors are attractive for use in situations in which large variations in temperatures and/or other extreme conditions preclude the use of conventional electric motors and mechanical bearings. In the Morrison motor, as in prior bearingless switched-reluctance motors, a multipole rotor is simultaneously levitated and rotated. In the prior motors, simultaneous levitation and rotation are achieved by means of two kinds of stator windings: (1) main motor windings and (2) windings that exert levitating forces on a multipole rotor. The multipole geometry is suboptimum for levitation because it presents a discontinuous surface to the stator pole faces, thereby degrading the vibration suppression capability of the magnetic bearing. The Morrison rotor simplifies the stator design in that it contains only one type of winding. The rotor is a hybrid that includes both (1) a circular lamination stack for levitation and (2) a multipole lamination stack for rotation. Simultaneous levitation and rotation at 6000 rpm were achieved with a prototype that included six rotor poles and eight stator poles. During normal operation, two of the four pairs of opposing stator poles (each pair at right angles to the other pair) levitate the rotor. The remaining two pairs of stator poles exert torque on the six-pole rotor lamination stack to produce rotation. The relative length of the circular and multipole lamination stacks on the rotor can be chosen to tailor the performance of the motor for a specific application. For a given overall length, increasing the length of the multipole stack relative to the circular stack results in an increase in torque relative to the levitation load capacity and vice versa.

Morrison, Carlos R.↗

NASA NTRS2003

Improved Bearingless Switched-Reluctance Motor

The Morrison rotor, named after its inventor, is a hybrid rotor for use in a bearingless switched-reluctance electric motor. The motor is characterized as bearingless in the sense that it does not rely on conventional mechanical bearings: instead, it functions as both a magnetic bearing and a motor. Bearingless switched-reluctance motors are attractive for use in situations in which large variations in temperatures and/or other extreme conditions preclude the use of conventional electric motors and mechanical bearings. In the Morrison motor, as in a prior bearingless switched-reluctance motor, a multipole rotor is simultaneously levitated and rotated. In the prior motor, simultaneous levitation and rotation are achieved by means of two kinds of stator windings: (1) main motor windings and (2) windings that exert levitating forces on a multipole rotor. The multipole geometry is suboptimum for levitation in that it presents a discontinuous surface to the stator pole faces, thereby degrading the vibration-suppression capability of the magnetic bearing. The Morrison rotor simplifies the stator design in that the stator contains only one type of winding. The rotor is a hybrid that includes both (1) a circular lamination stack for levitation and (2) a multipole lamination stack for rotation. A prototype includes six rotor poles and eight stator poles (see figure). During normal operation, two of the four pairs of opposing stator poles (each pair at right angles to the other pair) levitate the rotor. The remaining two pairs of stator poles exert torque on the six-pole rotor lamination stack to produce rotation. The relative lengths of the circular and multipole lamination stacks on the rotor can be chosen to tailor the performance of the motor for a specific application. For a given overall length, increasing the length of the multipole stack relative to the circular stack results in an increase in torque relative to levitation load capacity and stiffness, and vice versa.

Morrison, Carlos R.↗

NASA NTRS2012

Demonstration of Passive Fuel Cell Thermal Management Technology

The NASA Glenn Research Center is developing advanced passive thermal management technology to reduce the mass and improve the reliability of space fuel cell systems for the NASA Exploration program. The passive thermal management system relies on heat conduction within highly thermally conductive cooling plates to move the heat from the central portion of the cell stack out to the edges of the fuel cell stack. Using the passive approach eliminates the need for a coolant pump and other cooling loop components within the fuel cell system which reduces mass and improves overall system reliability. Previous development demonstrated the performance of suitable highly thermally conductive cooling plates and integrated heat exchanger technology to collect the heat from the cooling plates (Ref. 1). The next step in the development of this passive thermal approach was the demonstration of the control of the heat removal process and the demonstration of the passive thermal control technology in actual fuel cell stacks. Tests were run with a simulated fuel cell stack passive thermal management system outfitted with passive cooling plates, an integrated heat exchanger and two types of cooling flow control valves. The tests were run to demonstrate the controllability of the passive thermal control approach. Finally, successful demonstrations of passive thermal control technology were conducted with fuel cell stacks from two fuel cell stack vendors.

Burke, Kenneth A.↗

NASA NTRS2012

Fuel Cell/Electrochemical Cell Voltage Monitor

A concept has been developed for a new fuel cell individual-cell-voltage monitor that can be directly connected to a multi-cell fuel cell stack for direct substack power provisioning. It can also provide voltage isolation for applications in high-voltage fuel cell stacks. The technology consists of basic modules, each with an 8- to 16-cell input electrical measurement connection port. For each basic module, a power input connection would be provided for direct connection to a sub-stack of fuel cells in series within the larger stack. This power connection would allow for module power to be available in the range of 9-15 volts DC. The relatively low voltage differences that the module would encounter from the input electrical measurement connection port, coupled with the fact that the module's operating power is supplied by the same substack voltage input (and so will be at similar voltage), provides for elimination of high-commonmode voltage issues within each module. Within each module, there would be options for analog-to-digital conversion and data transfer schemes. Each module would also include a data-output/communication port. Each of these ports would be required to be either non-electrical (e.g., optically isolated) or electrically isolated. This is necessary to account for the fact that the plurality of modules attached to the stack will normally be at a range of voltages approaching the full range of the fuel cell stack operating voltages. A communications/ data bus could interface with the several basic modules. Options have been identified for command inputs from the spacecraft vehicle controller, and for output-status/data feeds to the vehicle.

Vasquez, Arturo↗

NASA NTRS2014

Development and Experimental Evaluation of Passive Fuel Cell Thermal Control

To provide uniform cooling for a fuel cell stack, a cooling plate concept was evaluated. This concept utilized thin cooling plates to extract heat from the interior of a fuel cell stack and move this heat to a cooling manifold where it can be transferred to an external cooling fluid. The advantages of this cooling approach include a reduced number of ancillary components and the ability to directly utilize an external cooling fluid loop for cooling the fuel cell stack. A number of different types of cooling plates and manifolds were developed. The cooling plates consisted of two main types; a plate based on thermopyrolytic graphite (TPG) and a planar (or flat plate) heat pipe. The plates, along with solid metal control samples, were tested for both thermal and electrical conductivity. To transfer heat from the cooling plates to the cooling fluid, a number of manifold designs utilizing various materials were devised, constructed, and tested. A key aspect of the manifold was that it had to be electrically nonconductive so it would not short out the fuel cell stack during operation. Different manifold and cooling plate configurations were tested in a vacuum chamber to minimize convective heat losses. Cooling plates were placed in the grooves within the manifolds and heated with surface-mounted electric pad heaters. The plate temperature and its thermal distribution were recorded for all tested combinations of manifold cooling flow rates and heater power loads. This testing simulated the performance of the cooling plates and manifold within an operational fuel cell stack. Different types of control valves and control schemes were tested and evaluated based on their ability to maintain a constant temperature of the cooling plates. The control valves regulated the cooling fluid flow through the manifold, thereby controlling the heat flow to the cooling fluid. Through this work, a cooling plate and manifold system was developed that could maintain the cooling plates within a minimal temperature band with negligible thermal gradients over power profiles that would be experienced within an operating fuel cell stack.

Fuel Cells↗

NASA NTRS2014

Method for Making a Fuel Cell from a Solid Oxide Monolithic Framework

The invention is a novel solid oxide fuel cell (SOFC) stack comprising individual bi-electrode supported fuel cells in which a thin electrolyte is supported between electrodes of essentially equal thickness. Individual cell units are made from graded pore ceramic tape that has been created by the freeze cast method followed by freeze drying. Each piece of graded pore tape later becomes a graded pore electrode scaffold that subsequent to sintering, is made into either an anode or a cathode by means of appropriate solution and thermal treatment means. Each cell unit is assembled by depositing of a thin coating of ion conducting ceramic material upon the side of each of two pieces of tape surface having the smallest pore openings, and then mating the coated surfaces to create an unsintered electrode scaffold pair sandwiching an electrolyte layer. The opposing major outer exposed surfaces of each cell unit is given a thin coating of electrically conductive ceramic, and multiple cell units are stacked, or built up by stacking of individual cell layers, to create an unsintered fuel cell stack. Ceramic or glass edge seals are installed to create flow channels for fuel and air. The cell stack with edge sealants is then sintered into a ceramic monolithic framework. Said solution and thermal treatments means convert the electrode scaffolds into anodes and cathodes. The thin layers of electrically conductive ceramic become the interconnects in the assembled stack.

Cable, Thomas L.↗

NASA NTRS2017

Correlations Among Microstructure, Morphology, Chemistry, and Isotopic Systematics of Hibonite in CM Chondrites

Introduction: Hibonite is a primary refractory phase occurring in many CAIs, typically with spinel and perovskite. Our microstructural studies of CAIs from carbonaceous chondrites reveal a range of stacking defect densities and correlated non-stoichiometry in hibonite. We also conducted a series of annealing experiments, demonstrating that the Mg-Al substitution stabilized the formation of defect-structured hibonite. Here, we continue a detailed TEM analysis of hibonite-bearing inclusions from CM chondrites that have been well-characterized isotopically. We examine possible correlations of microstructure, morphology, mineralogy, and chemical and isotopic systematics of CM hibonites in order to better understand the formation history of hibonite in the early solar nebula. Methods: Fifteen hibonite-bearing inclusions from the Paris CM chondrite were analyzed using a JEOL 7600F SEM and a JEOL 8530F electron microprobe. In addition to three hibonite-bearing inclusions from the Murchison CM chondrite previously reported, we selected three inclusions from Paris, Pmt1-6, 1-9, and 1-10, representing a range of 26Al/27Al ratios and minor element concentrations for a detailed TEM study. We extracted TEM sections from hibonite grains using a FEI Quanta 3D field emission gun SEM/FIB. The sections were then examined using a JEOL 2500SE field-emission scanning TEM equipped with a Thermo-Noran thin window EDX spectrometer. Results and Discussion: A total of six hibonite-bearing inclusions, including two platy hibonite crystals (PLACs) and four spinel-hibonite inclusions (SHIBs), were studied. There are notable differences in chemical and isotopic compositions between the inclusions (Table 1), indicative of their different formation environment or timing. Our TEM observations show perfectly-ordered, stoichiometric hibonite crystals without stacking defects in two PLACs, 2-7-1 and 2-8-2, and in three SHIBs, Pmt1-6, 1-9, and 1-10. In contrast, SHIB 1-9-5 hibonite grains contain a low density of stacking defects linked to an increase in MgO contents, indicating complex, disordered intergrowths of stoichiometric and MgO-enriched hibonites. From the data collected to date, we find no clear correlation between the microstructures of hibonite and its morphological and mineralogical types that reflect distinct chemical and isotopic systematics [6-8,10]. Interestingly, the presence of no or few stacking defects in hibonite from the PLACs and SHIBs are in contrast to our experimental studies that produced very high densities of stacking defects in hibonite [3-5]. Unlike our experi-ments, electron microprobe data from the PLACs and SHIBs hibonite grains show a strong correlation between (Ti4++Si4+) and Mg2+ cations, suggesting that coupled substitutions of (Ti4++Mg2+) and (Si4++Mg2+) for 2Al3+ inhibit the formation of defect-structured hibonite. However, our experimental studies suggest that kinetics (e.g., cooling rate) or other thermal effects also exert a strong control on the microstructures and chemical compositions of hibonite. In Pmt1-6, elongated perovskite grains present at the hibonite grain boundaries display (121) twinning, indicative of a fast cooling (>50degC/min) after high-temperature events. Therefore, the nebular microstructural characteristics of hibonite, at least in this inclusion, would not have destroyed by subsequent high-temperature annealing. Conclusions: Our TEM observations thus far show no clear correlation in microstructures, morphological and mineralogical characteristics, and chemical and isotopic systematics of hibonites from CM chondrites. The observed variation in stacking defect densities in the hibonites may be controlled by thermal processes in the early solar nebula. A detailed TEM analysis of additional CM hibonite samples is underway to evaluate this hypothesis.

Han, J.↗