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At least 775 records · Page 43

Nanoporous, Metal Carbide, Surface Diffusion Membranes for High Temperature Hydrogen Separations

Colorado School of Mines (CSM) developed high temperature, hydrogen permeable membranes that contain no platinum group metals with the goal of separating hydrogen from gas mixtures representative of gasification of carbon feedstocks such as coal or biomass in order to meet DOE NETL 2015 hydrogen membrane performance targets. We employed a dual synthesis strategy centered on transition metal carbides. In the first approach, novel, high temperature, surface diffusion membranes based on nanoporous Mo 2 C were fabricated on ceramic supports. These were produced in a two step process that consisted of molybdenum oxide deposition followed by thermal carburization. Our best Mo 2 C surface diffusion membrane achieved a pure hydrogen flux of 367 SCFH/ft 2 at a feed pressure of only 20 psig. The highest H 2 /N 2 selectivity obtained with this approach was 4.9. A transport model using “dusty gas” theory was derived to describe the hydrogen transport in the Mo 2 C coated, surface diffusion membranes. The second class of membranes developed were dense metal foils of BCC metals such as vanadium coated with thin (< 60 nm) Mo 2 C catalyst layers. We have fabricated a Mo 2 C/V composite membrane that in pure gas testing delivered a H 2 flux of 238 SCFH/ft 2 at 600 °C and 100 psig, with no detectable He permeance. This exceeds the 2010 DOE Target flux. This flux is 2.8 times that of pure Pd at the same membrane thickness and test conditions and over 79% of the 2015 flux target. In mixed gas testing we achieved a permeate purity of ≥99.99%, satisfying the permeate purity milestone, but the hydrogen permeance was low, ~0.2 SCFH/ft 2 .psi. However, during testing of a Mo 2 C coated Pd alloy membrane with DOE 1 feed gas mixture a hydrogen permeance of >2 SCFH/ft 2 .psi was obtained which was stable during the entire test, meeting the permeance associated with the 2010 DOE target flux. Lastly, the Mo 2 C/V composite membranes were shown to be stable for at least 168 hours = one week, including cycling at high temperature and alternating He/H 2 exposure.

08 HYDROGEN↗

Pre-Combustion Carbon Dioxide Capture by a New Dual Phase Ceramic-Carbonate Membrane Reactor

This report documents synthesis, characterization and carbon dioxide permeation and separation properties of a new group of ceramic-carbonate dual-phase membranes and results of a laboratory study on their application for water gas shift reaction with carbon dioxide separation. A series of ceramic-carbonate dual phase membranes with various oxygen ionic or mixed ionic and electronic conducting metal oxide materials in disk, tube, symmetric, and asymmetric geometric configurations was developed. These membranes, with the thickness of 10 μm to 1.5 mm, show CO 2 permeance in the range of 0.5-5×10 -7 mol·m -2 ·s -1 ·Pa -1 in 500-900°C and measured CO 2 /N 2 selectivity of up to 3000. CO 2 permeation mechanism and factors that affect CO 2 permeation through the dual-phase membranes have been identified. A reliable CO 2 permeation model was developed. A robust method was established for the optimization of the microstructures of ceramic-carbonate membranes. The ceramic-carbonate membranes exhibit high stability for high temperature CO 2 separations and water gas shift reaction. Water gas shift reaction in the dual-phase membrane reactors was studied by both modeling and experiments. It is found that high temperature syngas water gas shift reaction in tubular ceramic-carbonate dual phase membrane reactor is feasible even without catalyst. The membrane reactor exhibits good CO 2 permeation flux, high thermal and chemical stability and high thermal shock resistance. Reaction and separation conditions in the membrane reactor to produce hydrogen of 93% purity and CO 2 stream of >95% purity, with 90% CO 2 capture have been identified. Integration of the ceramic-carbonate dual-phase membrane reactor with IGCC process for carbon dioxide capture was analyzed. A methodology was developed to identify optimum operation conditions for a membrane tube of given dimensions that would treat coal syngas with targeted performance. The calculation results show that the dual-phase membrane reactor could improve IGCC process efficiency but the cost of the membrane reactor with membranes having current CO 2 permeance is high. Further research should be directed towards improving the performance of the membranes and developing cost-effective, scalable methods for fabrication of dual-phase membranes and membrane reactors.

36 MATERIALS SCIENCE↗

Transient Microstructure Evolutions and Local Properties of Dual-Phase 980 MPa Grade Steel Via Friction Stir Spot Processing

Friction stir processing is a novel solid-state process to modify microstructures and their properties by intense, localized plastic deformation. However, little research has been reported for microstructure evolutions of advanced high-strength steels during the process. The present work focuses on the study of transient microstructure changes and local mechanical properties for friction stir spot processed dual-phase (DP) 980 MPa grade steel (DP980) under different peak temperatures. A pinless silicon nitride ceramic tool was used to produce relatively simple material deformation and flow near the tool. Friction stir spot processed steel samples were characterized by optical and electron microscopies. Furthermore, Vickers microhardness and nano-indentation measurements were used to study local mechanical properties for correlation with microstructures. A swallow layer of refined grains (<0.6 µm) was obtained with a low peak temperature (under 400 °C), whereas higher peak temperatures (>Ac 1 ) led to a change in grain size with different microstructures (fine-grained DP or martensite). Electron back-scattered diffraction characterizations revealed a large deformation in the as-received microstructures (mixture of ferrite and tempered martensite) induced by friction stir spot processing, leading to recrystallization and grain refinement around the stirred zone. Also, nano-indentation measurements showed a higher hardness than the hardness of the as-received DP980. Friction stir processing with different process conditions effectively changed microstructures and local mechanical properties.

36 MATERIALS SCIENCE↗

High-Temperature Helical-Tube Solar Receiver

Solar-thermal receiver used with circular parabolic concentrator to supply about 58 kW thermal power to Brayton engine or industrial process. Solar radiation focused into open end of cylindrical ceramic thermal inertial sleeve 8 in. in diameter that reradiates energy to helical heatexchanger tube surrounding sleeve.

Robertson, C. S., Jr.↗

Materials research and applications at NASA Lewis Research Center

The facilities and instruments of the Lewis Research Center specialized for materials research are discussed. The main objectives of the Center are to provide R & D relevant to main propulsion plants and auxiliary power systems for aeronautics, space, and energy conversion applications. The Center is concerned with microstructure-property relations and their effect on processing; intermetallic compounds and high temperature metal matrix composites; ceramics with improved reliability for use in heat engines; polymer matrix composites for aerospace applcations; understanding the high temperature corrosive attack in the hostile environments of aircraft, rockets, and other heat engines; high temperature lubrication and wear; and microgravity materials research. The various types of schemes and techniques, provided by the Center, for analyzing data are described.

Probst, H. B.↗

Preparation for microgravity: The role of the microgravity materials science laboratory

A laboratory dedicated to ground based materials processing in preparation for space flight was established at the NASA Lewis Research Center. Experiments are performed to delineate the effects of gravity on processes of both scientific and commercial interest. Processes are modeled physically and mathematically. Transport model systems are used where possible to visually track convection, settling, crystal growth, phase separation, agglomeration, vapor transport, diffusive flow, and polymers reactions. The laboratory contains apparatus which functionally duplicates apparatus available for flight experiments and other pieces instrumented specifically to allow process characterization. Materials addressed include metals, alloys, salts, glasses, ceramics, and polymers. The Microgravity Materials Science Laboratory is staffed by engineers and technicians from a variety of disciplines and is open to users from industry and academia as well as the government. Examples will be given of the laboratory apparatus typical experiments and results.

Johnston, J. Christopher↗

Development and characterization of Powder Metallurgy (PM) 2XXX series Al alloy products and Metal Matrix Composite (MMC) 2XXX Al/SiC materials for high temperature aircraft structural applications

The results of a series of material studies performed by the Lockheed Aeronautical Systems Company over the time period from 1980 to 1991 are discussed. The technical objective of these evaluations was to develop and characterize advanced aluminum alloy materials with temperature capabilities extending to 350 F. An overview is given of the first five alloy development efforts under this contract. Prior work conducted during the first five modifications of the alloy development program are listed. Recent developments based on the addition of high Zr levels to an optimum Al-Cu-Mg alloy composition by powder metallurgy processing are discussed. Both reinforced and SiC or B4C ceramic reinforced alloys were explored to achieve specific target goals for high temperature aluminum alloy applications.

Chellman, D. J.↗

Application of materials database (MAT.DB.) to materials education

Finding the right material for the job is an important aspect of engineering. Sometimes the choice is as fundamental as selecting between steel and aluminum. Other times, the choice may be between different compositions in an alloy. Discovering and compiling materials data is a demanding task, but it leads to accurate models for analysis and successful materials application. Mat. DB. is a database management system designed for maintaining information on the properties and processing of engineered materials, including metals, plastics, composites, and ceramics. It was developed by the Center for Materials Data of American Society for Metals (ASM) International. The ASM Center for Materials Data collects and reviews material property data for publication in books, reports, and electronic database. Mat. DB was developed to aid the data management and material applications.

Liu, Ping↗

Applications of Thin Film Thermocouples for Surface Temperature Measurement

Thin film thermocouples provide a minimally intrusive means of measuring surface temperature in hostile, high temperature environments. Unlike wire thermocouples, thin films do not necessitate any machining of the surface, therefore leaving intact its structural integrity. Thin films are many orders of magnitude thinner than wire, resulting in less disruption to the gas flow and thermal patterns that exist in the operating environment. Thin film thermocouples have been developed for surface temperature measurement on a variety of engine materials. The sensors are fabricated in the NASA Lewis Research Center's Thin Film Sensor Lab, which is a class 1000 clean room. The thermocouples are platinum-13 percent rhodium versus platinum and are fabricated by the sputtering process. Thin film-to-leadwire connections are made using the parallel-gap welding process. Thermocouples have been developed for use on superalloys, ceramics and ceramic composites, and intermetallics. Some applications of thin film thermocouples are: temperature measurement of space shuttle main engine turbine blade materials, temperature measurement in gas turbine engine testing of advanced materials, and temperature and heat flux measurements in a diesel engine. Fabrication of thin film thermocouples is described. Sensor durability, drift rate, and maximum temperature capabilities are addressed.

Martin, Lisa C.↗

Preliminary Results of Field Emission Cathode Tests

Preliminary screening tests of field emission cathodes such as chemical vapor deposited (CVD) diamond, textured pyrolytic graphite, and textured copper were conducted at background pressures typical of electric thruster test facilities to assess cathode performance and stability. Very low power electric thrusters which provide tens to hundreds micronewtons of thrust may need field emission neutralizers that have a capability of tens to hundreds of microamperes. From current voltage characteristics, it was found that the CVD diamond and textured metals cathodes clearly satisfied the Fowler-Nordheim emission relation. The CVD diamond and a textured copper cathode had average current densities of 270 and 380 mA/sq cm, respectively, at the beginning-of-life. After a few hours of operation the cathode emission currents degraded by 40 to 75% at background pressures in the 10(exp -5) Pa to 10(exp -4) Pa range. The textured pyrolytic graphite had a modest current density at beginning-of-life of 84 mA/sq cm, but this cathode was the most stable of all. Extended testing of the most promising cathodes is warranted to determine if current degradation is a burn-in effect or whether it is a long-term degradation process. Preliminary experiments with ferroelectric emission cathodes, which are ceramics with spontaneous electric polarization, were conducted. Peak current densities of 30 to 120 mA/sq cm were obtained for pulse durations of about 500 ns in the 10(exp -4) Pa pressure range.

Sovey, James S.↗

Ultra-High Temperature Materials Characterization for Propulsion Applications

Propulsion system efficiency increases as operating temperatures are increased. Some very high-temperature materials are being developed, including refractory metal alloys, carbides, borides, and silicides. System design requires data for materials properties at operating temperatures. Materials property data are not available for many materials of interest at the desired operating temperatures (up to approx. 3000 K). The objective of this work is to provide important physical property data at ultra-high temperatures. The MSFC Electrostatic levitation (ESL) facility can provide measurements of thermophysical properties which include: creep strength, density and thermal expansion for materials being developed for propulsion applications. The ESL facility uses electrostatic fields to position samples between electrodes during processing and characterization studies. Because the samples float between the electrodes during studies, they are free from any contact with a container or test apparatus. This provides a high purity environment for the study of high-temperature, reactive materials. ESL can be used to process a wide variety of materials including metals, alloys, ceramics, glasses and semiconductors. The MSFC ESL has provided non-contact measurements of properties of materials up to 3400 C. Density and thermal expansion are measured by analyzing digital images of the sample at different temperatures. Our novel, non-contact method for measuring creep uses rapid rotation to deform the sample. Digital images of the deformed samples are analyzed to obtain the creep properties, which match those obtained using ASTM Standard E-139 for Nb at 1985 C. Data from selected ESL-based characterization studies will be presented. The ESL technique could support numerous propulsion technologies by advancing the knowledge base and the technology readiness level for ultra-high temperature materials. Applications include non-eroding nozzle materials and lightweight, high-temperature alloys for turbines and structures.

Rogers, Jan↗

Ultra-High Temperature Materials Characterization for Space and Missile Applications

Numerous advanced space and missile technologies including propulsion systems require operations at high temperatures. Some very high-temperature materials are being developed to meet these needs, including refractory metal alloys, carbides, borides, and silicides. System design requires data for materials properties at operating temperatures. Materials property data are not available at the desired operating temperatures for many materials of interest. The objective of this work is to provide important physical property data at ultra-high temperatures. The MSFC Electrostatic Levitation (ESL) facility can provide measurements of thermophysical properties which include: creep strength, emissivity, density and thermal expansion. ESL uses electrostatic fields to position samples between electrodes during processing and characterization experiments. Samples float between the electrodes during studies and are free from any contact with a container or test apparatus. This provides a high purity environment for the study of high-temperature, reactive materials. ESL can be used to process a wide variety of materials including metals, alloys, ceramics, glasses and semiconductors. A system for the determination of total hemispherical emissivity is being developed for the MSFC ESL facility by AZ Technology Inc. The instrument has been designed to provide emissivity measurements for samples during ESL experiments over the temperature range 700-3400K. A novel non-contact technique for the determination of high-temperature creep strength has been developed. Data from selected ESL-based characterization studies will be presented. The ESL technique could advance space and missile technologies by advancing the knowledge base and the technology readiness level for ultra-high temperature materials. Applications include non-eroding nozzle materials and lightweight, high-temperature alloys for turbines and structures.

Rogers, Jan↗

Portable Device Analyzes Rocks and Minerals

inXitu Inc., of Mountain View, California, entered into a Phase II SBIR contract with Ames Research Center to develop technologies for the next generation of scientific instruments for materials analysis. The work resulted in a sample handling system that could find a wide range of applications in research and industrial laboratories as a means to load powdered samples for analysis or process control. Potential industries include chemical, cement, inks, pharmaceutical, ceramics, and forensics. Additional applications include characterizing materials that cannot be ground to a fine size, such as explosives and research pharmaceuticals.

Source record↗

ZnO buffer layer for metal films on silicon substrates

Dramatic improvements in metallization integrity and electroceramic thin film performance can be achieved by the use of the ZnO buffer layer to minimize interfacial energy between metallization and adhesion layers. In particular, the invention provides a substrate metallization method utilizing a ZnO adhesion layer that has a high work of adhesion, which in turn enables processing under thermal budgets typically reserved for more exotic ceramic, single-crystal, or metal foil substrates. Embodiments of the present invention can be used in a broad range of applications beyond ferroelectric capacitors, including microelectromechanical systems, micro-printed heaters and sensors, and electrochemical energy storage, where integrity of metallized silicon to high temperatures is necessary.

36 MATERIALS SCIENCE↗

Development, Characterization, and Testing of Solid-State Electrolytes for Batteries

Traditional liquid electrolytes used in lithium (Li) metal batteries (LMBs) have severe safety issues, poor power density, as well as thermal and electrochemical instability that prevents their scaling to newer applications, such as electric vehicles. Using sulfide-based solid-state electrolytes (SSEs) is a viable method to address many of the issues that plague LMBs. However, the key issue preventing the expansion of sulfide-based SSEs is an interplay between poor interfacial stability with the electrodes and massive external stack pressure required to maintain electrode-electrolyte contact. The need for extensive pressure requires large system-level (i.e., battery pack used in an electric vehicle) housing that causes a disconnect between performance at a smaller scale and actual application. Secondary prevention to sulfide-based SSE adoption are difficulties in manufacturing, as toxic deterioration occurs when these materials are exposed to humidity, as well as drastic reduction in SSE performance at low temperature. This work hypothesizes that unique interfacial designs of electrodes and the modification of the sulfide-based SSE will enable reduction of necessary external cell pressure, and therefore support the design of practical LMBs. This will be done through collaboration within Idaho National Laboratory (INL), where manufacturing practices will be parameterized to produce low defect, low porosity SSEs with slight modifications. Next, artificial interfaces will be produced on electrodes to observe the conformality and mass transport properties between the modified SSE and pre-treated anode. External pressure on Li-metal cells will also be parameterized to reduce interfacial impedance while a reduction in the pressure will allot reasonable housing design for larger scale applications. Focus on novelty in this work occurs by modifications to the solid-solid interfaces between electrolyte and electrode, done through doping of the electrolyte and production of artificial interfaces on the Li-metal anode. The modifications at these interfaces, in addition to modified external pressure could identify and address the poor interfacial impedance that hinders high performance SSEs. Fundamental understanding on how to reduce the key hindrances of all-solid-state batteries (ASSBs) will support the advancement for larger scale production and performance, of which will be held in perspective for future works. Beyond battery development, the knowledge gained from process control and defect analysis is applicable to other ceramic systems, such as nuclear fuel coatings and high temperature electrolyzers.

25 ENERGY STORAGE↗

Development, Characterization, and Testing of Solid-State Electrolytes for Batteries

Traditional liquid electrolytes used in lithium (Li) metal batteries (LMBs) have severe safety issues, poor power density, as well as thermal and electrochemical instability that prevents their scaling to newer applications, such as electric vehicles. Using sulfide-based solid-state electrolytes (SSEs) is a viable method to address many of the issues that plague LMBs. However, the key issue preventing the expansion of sulfide-based SSEs is an interplay between poor interfacial stability with the electrodes and massive external stack pressure required to maintain electrode-electrolyte contact. The need for extensive pressure requires large system-level (i.e., battery pack used in an electric vehicle) housing that causes a disconnect between performance at a smaller scale and actual application. Secondary prevention to sulfide-based SSE adoption are difficulties in manufacturing, as toxic deterioration occurs when these materials are exposed to humidity, as well as drastic reduction in SSE performance at low temperature. This work hypothesizes that unique interfacial designs of electrodes and the modification of the sulfide-based SSE will enable reduction of necessary external cell pressure, and therefore support the design of practical LMBs. This will be done through collaboration within Idaho National Laboratory (INL), where manufacturing practices will be parameterized to produce low defect, low porosity SSEs with slight modifications. Next, artificial interfaces will be produced on electrodes to observe the conformality and mass transport properties between the modified SSE and pre-treated anode. External pressure on Li-metal cells will also be parameterized to reduce interfacial impedance while a reduction in the pressure will allot reasonable housing design for larger scale applications. Focus on novelty in this work occurs by modifications to the solid-solid interfaces between electrolyte and electrode, done through doping of the electrolyte and production of artificial interfaces on the Li-metal anode. The modifications at these interfaces, in addition to modified external pressure could identify and address the poor interfacial impedance that hinders high performance SSEs. Fundamental understanding on how to reduce the key hindrances of all-solid-state batteries (ASSBs) will support the advancement for larger scale production and performance, of which will be held in perspective for future works. Beyond battery development, the knowledge gained from process control and defect analysis is applicable to other ceramic systems, such as nuclear fuel coatings and high temperature electrolyzers.

25 ENERGY STORAGE↗

CO Oxidation and Subsequent CO 2 Chemisorption on Alkaline Zirconates: Li 2 ZrO 3 and Na 2 ZrO 3

Here, two different alkaline zirconates (Li 2 ZrO 3 and Na 2 ZrO 3 ) were studied as possible bifunctional catalytic-captor materials for CO oxidation and the subsequent CO 2 chemisorption process. Initially, CO oxidation reactions were analyzed in a catalytic reactor coupled to a gas chromatograph, using Li 2 ZrO 3 and Na 2 ZrO 3 , under different O 2 partial flows. We found results clearly showed that Na 2 ZrO 3 possesses much better catalytic properties than Li 2 ZrO 3 . After the CO-O 2 oxidation catalytic analysis, CO2 chemisorption process was analyzed by thermogravimetric analysis, only for the Na 2 ZrO 3 ceramic. The results confirmed that Na 2 ZrO 3 is able to work as a bifunctional material (CO oxidation and subsequent CO 2 chemisorption), although the kinetic CO 2 capture process was not the best one under the physicochemical condition used in this case. For Na 2 ZrO 3 , the best CO conversions were found between 445 and 580 °C (100%), while Li 2 ZrO 3 only showed a 35% of efficiency between 460 and 503 °C. However, in the Na 2 ZrO 3 case, at temperatures higher than 580 °C its catalytic activity gradually decreases as a result of CO 2 capture process. Finally, all these experiments were compared and supported with theoretical thermodynamic data.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗