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At least 1,045 records · Page 58

Large-Scale Additive Manufacturing of Silicon Carbide with Process Monitoring

This report summarizes new capabilities in additive manufacturing (AM) of large-scale silicon carbide (SiC) components under the Advanced Materials and Manufacturing Technologies (AMMT) program. SiC is a promising material that is being considered for many advanced reactor designs due to its high temperature strength, radiation tolerance, minimal neutron absorption, and oxidation resistance [1-8]. One of the primary limitations to using SiC as an in-core structural material is the inability to fabricate large SiC components with complex geometries. While under the former Transformational Challenge Reactor (TCR) program, ceramic AM systems at the Oak Ridge National Laboratory (ORNL) were limited in the quantity and overall size achievable for producing ceramic AM components. To address this, ORNL has improved its infrastructure for binder jet and chemical vapor infiltration (CVI) processes with cutting-edge equipment coming online in a newly renovated laboratory space capable of producing larger components and higher throughput without compromise on part size. This report details the laboratory renovation progress, focusing specifically on the DesktopMetal (formerly ExOne) X25Pro binder jet, a large scale CVI furnace, and the added functionality of a software tool called Peregrine for quality assurance and control purposes.

36 MATERIALS SCIENCE↗

Engineering Graphene-Ceramic 3D Composite Foams by Freeze Drying

A 3D graphene foam produced by the chemical vapor deposition (CVD) technique is recognized as an effective nanofiller material, as it does not agglomerate in the matrix. Though CVD facilitates pristine graphene foam production, the method poses limitations in developing large-scale 3D graphene composite foams as advanced engineering materials. In this paper, a freeze-drying (FD) process is used to produce a composite 3D foam, which is a mixture of graphene nanoplatelet (GNP) and a low-temperature co-fired ceramic (LTCC). The freeze-dried GNP-LTCC reticulated 3D composite foam has an average pore size ranging from 70 to 100 μm. Pore size is varied by regulating the heat transfer rate during the freezing process using a thermally conductive aluminum (Al) mold and a thermally insulating acrylonitrile butadiene styrene (ABS) mold. Computational thermal modeling is used to visualize the heat transfer and its effect on foam pore size. Subsequently, a freeze-dried GNP-LTCC composite foam is embedded into the LTCC matrix to form a hierarchical assembly by a spark plasma technique without compromising the 3D structure of the FD foam. This study established that a simple, eco-friendly, and scalable processing methodology can produce advanced graphene-based 3D composite foams as the future tailorable nanofillers for designing multimatrix materials.

36 MATERIALS SCIENCE↗

Development of a silicon carbide ceramic based counter-flow heat exchanger by binder jetting and liquid silicon infiltration for concentrating solar power

A silicon carbide ceramic counter-flow heat exchanger with integrated headers was printed by binder jetting additive manufacturing process. Multiple phenolic binder infiltration cycles (3 or 5) followed by pyrolysis were conducted to increase the net carbon content of the printed SiC specimens. Subsequently, to attain full densification, silicon melt infiltration was used. The microstructure and mechanical properties were comprehensively characterized on the densified material. The chemical compositions and visual distribution of the various regions in the specimens were determined via scanning electron microscopy, while X-ray diffraction and synchrotron µ-computed tomography were used to provide a quantitative assessment of the volume fractions of the identified phase regions. Microhardness measurements showed dependence on the local microstructure. The fracture strength of the material was correlated with the specimen density and agreed with the reported values in the literature. High-temperature exposure at 750 °C for up to 200h did not degrade the strength for the specimens with three phenolic-binder infiltrations; however, the strengths degraded for ones with five phenolic-binder infiltrations. The associated fracture toughnesses of the specimens were ~3.4 MPam 1/2 at room temperature and 750°C, and the thermal conductivities varied from >150 W/mK at room temperature to ~45 W/mK at 750°C. Hence, this study validated the use of the binder-jetting printed SiC ceramic materials for high-temperature heat exchanges. Lastly, we also present in this work the first successful fabrication of a binder-jetting printed one-piece dense SiC ceramic heat exchanger body with unblocked channels that can be used for the flow of heat transfer fluids.

36 MATERIALS SCIENCE↗

Robotic end-effector for rewaterproofing shuttle tiles

This paper summarizes work by Rockwell International's Space Systems Division's Robotics Group at Downey, California. The work is part of a NASA-led team effort to automate Space Shuttle rewaterproofing in the Orbiter Processing Facility at the Kennedy Space Center and the ferry facility at the Ames-Dryden Flight Research Facility. Rockwell's effort focuses on the rewaterproofing end-effector, whose function is to inject hazardous dimethylethyloxysilane into thousands of ceramic tiles on the underside of the orbiter after each flight. The paper has five sections. First, it presents background on the present manual process. Second, end-effector requirements are presented, including safety and interface control. Third, a design is presented for the five end-effector systems: positioning, delivery, containment, data management, and command and control. Fourth, end-effector testing and integrating to the total system are described. Lastly, future applications for this technology are discussed.

Manouchehri, Davoud↗

On electrolyte wetting through lithium-ion battery separators

The wettability by electrolyte is a critical characteristic of lithium-ion battery separators since electrolyte absorption is essential for ionic transport. Most importantly, fast absorption of electrolyte facilitates the electrolyte filling and wetting processes during the battery assembly. However, theoretical or experimental investigation of separator wettability has rarely been reported, and thus very little quantitative data can be found in the existing literature. Here, innovative experimental techniques and associated analytical models have been developed to fully characterize the electrolyte wetting behavior through battery separators. Both in-plane and through-plane imbibition processes are investigated. The results show that, electrolyte needs significantly longer time to wet separators than it does for commercial electrodes. The wetting rate depends significantly on the pore size, porosity, and micro-structure of the separators. Electrolyte in-plane wetting is only observed in the separators manufactured by the wet process. Increasing separator porosity and pore size is shown to be substantially increasing through-plane wetting rate. In addition, ceramic coating is shown to increase in-plane wetting but retard through-plane wetting.

25 ENERGY STORAGE↗

Effect of a micro-scale dislocation pileup on the atomic-scale multi-variant phase transformation and twinning

In this paper, we perform concurrent atomistic–continuum (CAC) simulations to assess the contribution of the internal stress induced by the microscale dislocation pileup at an atomically structured interface to the atomic-scale phase transformations (PTs), reverse PTs, and twinning. The main novelty of this work is to unify the atomistic description of the interface and the coarse-grained (CG) description of the lagging dislocations away from the interface within one single framework. Our major findings are: (a) the interface dynamically responds to a pileup by forming steps/ledges, the height of which is proportional to the number of dislocations arriving at the interface; (b) the pileup-induced internal stress concentration profile follows neither the classical Eshelby model nor the super-dislocation model alone, but a combination of them; (c) when the pre-sheared sample is compressed, a direct square-to-hexagonal PT occurs ahead of the pileup tip and eventually grows into a wedge shape. The two variants of the hexagonal phases form a twin with respect to each other; (d) upon a further increase of the loading, part of the newly formed hexagonal phase transforms back to the square phase. The square product phase resulting from this reverse PT forms a twin with respect to the initial square phase. All phase boundaries (PBs) and twin boundaries (TBs) are stationary and correspond to zero thermodynamic Eshelby driving forces; and (e) the microscale dislocation pileup-induced internal shear stress and the structural change at the atomic-scale interface reduces the stress required for initiating a PT by a factor of 5.5, comparing with that in the sample containing no dislocations. This work is the first characterization of the behavior of PTs/twinning resulting from the reaction between a microscale dislocation slip and an atomically structured interface. In conclusion, the gained knowledge will advance our understanding of how the multi-phase material behaves in many complex physical processes, such as the synthesis of multi-phase high-entropy alloys or superhard ceramics under high-pressure torsion, deep mantle earthquakes in geophysics, and so on, which all involve dislocation slip, PTs, twinning, and their interactions across from the atomistic to the microscale and beyond.

36 MATERIALS SCIENCE↗

Structure, Chemistry, and Charge Transfer Resistance of the Interface between Li 7 La 3 Zr 2 O 12 Electrolyte and LiCoO 2 Cathode

All-solid-state batteries promise significant safety and energy density advantages over liquid-electrolyte batteries. The interface between the cathode and the solid electrolyte is an important contributor to charge transfer resistance. Strong bonding of solid oxide electrolytes and cathodes requires sintering at elevated temperatures. Knowledge of the temperature dependence of the composition and charge transfer properties of this interface is important for determining the ideal sintering conditions. To understand the interfacial decomposition processes and their onset temperatures, model systems of LiCoO 2 (LCO) thin films deposited on cubic Al-doped Li 7 La 3 Zr 2 O 12 (LLZO) pellets were studied as a function of temperature using interface-sensitive techniques. X-ray photoelectron spectroscopy, secondary ion mass spectroscopy, and energy-dispersive X-ray spectroscopy data indicated significant cation interdiffusion and structural changes starting at temperatures as low as 300 °C. La 2 Zr 2 O 7 and Li 2 CO 3 were identified as decomposition products after annealing at 500 °C by synchrotron X-ray diffraction. X-ray absorption spectroscopy results indicate the presence of also LaCoO 3 in addition to La 2 Zr 2 O 7 and Li 2 CO 3 . On the basis of electrochemical impedance spectroscopy and depth profiling of the Li distribution upon potentiostatic hold experiments on symmetric LCO|LLZO|LCO cells, the interfaces exhibited significantly increased impedance, up to 8 times that of the as-deposited samples after annealing at 500 °C. Here, our results indicate that lower-temperature processing conditions, shorter annealing time scales, and CO 2 -free environments are desirable for obtaining ceramic cathode|electrolyte interfaces that enable fast Li transfer and high capacity.

25 ENERGY STORAGE↗

Elucidation of Local Ordering and Atomic-Scale Structure in Polymer-Derived SiOC

Silicon oxycarbide (SiOC) is a versatile ceramic material with tunable microstructure and compositions that can be modulated through precursor chemistry and processing conditions. Though there are several noteworthy uses of SiOC across a range of application spaces, the difficulties in elucidating the short- to medium-range order within these materials have limited the maturation of strategies to precisely control SiC x O 4–x compositions for user-tailored applications. In this contribution, we implement a range of synchrotron scattering and spectroscopy methods coupled with stochastic modeling techniques to elucidate changes in local chemistry and structure associated with the pyrolysis of a commercially available SiOC polymer precursor. Stochastic modeling approaches provide valuable insights into decoupling local Si–O and Si–C environments while confirming predominate heterogeneous phases in materials. Using pyrolysis temperatures between 250 to 800 °C results in a heterogeneous material predominately composed of SiOC and amorphous SiO 2 domains. At 1100 °C, redistribution of Si–C pairs in the SiOC network and Si–O from the SiO 2 domains create a more ordered SiOC phase with local cubic SiC-like ordering. In addition, residual carbon leads to a detectable carbon phases at 1100 °C that persist at higher temperatures. These efforts address the difficulties of obtaining atomic-scale insights into the local structure and nanoscale heterogeneities in SiOC, providing pathways toward establishing structure–property relationships for future materials development.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Unusual structural-disorder stability of mechanochemically derived-Pb(Sc 0.5 Nb 0.5 )O 3

This study demonstrates the important effect of processing on the B-site ordering in Pb(Sc 0.5 Nb 0.5 )O 3 ceramics. In contradiction to previous observations on ceramics prepared from solid state synthesis powders, which show a distinctive B-site cation ordering when annealed below ~1200 °C, in mechanochemically derived ceramics sintered 200 °C below this temperature, we do not observe such ordering, regardless of the conditions of thermal post-annealing. Accordingly, atomic-scale transmission electron microscopy revealed nanometer-sized B-site ordered regions in mechanochemically derived ceramics contrary to the larger regions extending through the whole grains in solid-state derived ceramics.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

High power THz sources for nonlinear imaging

Many biological and chemical compounds have unique absorption features in the THz (0.1 - 10 THz) region, making the use of THz waves attractive for imaging in defense, security, biomedical imaging, and monitoring of industrial processes. Unlike optical radiation, THz frequencies can pass through many substances such as paper, clothing, ceramic, etc. with little attenuation. The use of currently available THz systems is limited by lack of highpower, sources as well as sensitive detectors and detector arrays operating at room temperature. Here we present a novel, high power THz source based on intracavity downconverison of optical pulses. The source delivers 6 ps pulses at 1.5 THz, with an average power of >300 μW and peak powers >450 mW. We propose an imaging method based on frequency upconverison that is ideally suited to use the narrow bandwidth and high peak powers produced by the source. By upconverting the THz image to the infrared, commercially available detectors can be used for real time imaging.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Mechanisms of Enhanced Thermal Stability of Polarization in Lead-Free (Bi 1/2 Na 1/2 ) 0.94 Ba 0.06 TiO 3 /ZnO Ceramic Composites

(Bi 1/2 Na 1/2 )TiO 3 -based solid solutions, one of the major systems of lead-free piezoelectric ceramics, exhibit a low thermal depolarization temperature ( T d ~100°C). It was reported that by incorporating 30 mol% ZnO particles to form a ceramic composite of (Bi 1/2 Na 1/2 ) 0.94 Ba 0.06 TiO 3 /ZnO, the depolarization process can be shifted up to ~250 °C. In the present work, a variety of advanced transmission electron microscopy techniques, including in situ heating, annular bright-field, high-angle annular dark-field, geometric phase analysis, energy-dispersive spectrum and electron energy-loss spectroscopy, are employed to investigate the underlying mechanisms for the enhanced thermal stability of polarization in the composite. Furthermore, it is found that the abrupt depolarization in (Bi 1/2 Na 1/2 ) 0.94 Ba 0.06 TiO 3 at T d becomes diffused over a wide temperature window up to the temperature at maximum dielectric constant ( T m ) under the combined actions of the incorporation of Zn into the perovskite lattice, the presence of residual stresses, and the pinning effect on micron-sized domains provided by ZnO particles.

36 MATERIALS SCIENCE↗

Materials for advanced rocket engine turbopump turbine blades

A study program was conducted to identify those materials that will provide the greatest benefits as turbine blades for advanced liquid propellant rocket engine turbines and to prepare technology plans for the development of those materials for use in the 1990 through 1995 period. The candidate materials were selected from six classes of materials: single-crystal (SC) superalloys, oxide dispersion-strengthened (ODS) superalloys, rapid solidification processed (RSP) superalloys, directionally solidified eutectic (DSE) superalloys, fiber-reinforced superalloy (FRS) composites, and ceramics. Properties of materials from the six classes were compiled and evaluated and property improvements were projected approximately 5 years into the future for advanced versions of materials in each of the six classes.

Chandler, W. T.↗

Solid-state combustion synthesis of ceramics and alloys in reduced gravity

Possible microgravity effects are explored in the combustion synthesis of ceramics and alloys from their constituent elements. Molten intermediates are typically present during the combustion process, thereby offering the chance for natural convection to take place. Numerical simulations suggest that the combustion front in concert with gravity may act as a partial zone-refinement mechanism which is attempting to sweep out porosity in the sample. Contrary to suggestions by dimensional analysis, no effects on the combustion rate are seen. An analytical model of the combustion velocity as a function of the gravitational field and the spreading rate of molten material gives the correct order of magnitude of the gravity effect as measured by centrifuge experiments.

Valone, S. M.↗

Chemical vapor deposition for silicon cladding on advanced ceramics

Polycrystalline Si was used to clad several advanced ceramic materials such as SiC, Si3N4, sapphire Al2O3, pyrolytic BN, and Si by a CVD process. The thickness of Si cladding ranged from 0.025 to 3.0 mm. CVD Si adhered quite well to all the above materials except Al3O, where the Si cladding was highly stressed and cracked or delaminated. A detailed material characterization of Si-clad SiC samples showed that Si adherence to SiC does not depend much on the substrate surface preparation; that the thermal cycling and polishing of the samples do not cause delamination; and that, in four-point bend tests, the Si-SiC bond remains intact, with the failure occurring in the Si.

Goela, Jitendra S.↗

Development of superconducting YBa2Cu3O(x) wires with low resistance electrical contacts

Materials exhibiting superconductivity above liquid nitrogen temperatures (77 K) will enable new applications of this phenomena. One of the first commercial applications of this technology will be superconducting magnets for medical imaging. However, a large number of aerospace applications of the high temperature superconducting materials have also been identified. These include magnetic suspension and balance of models in wind tunnels and resistanceless leads to anemometers. The development of superconducting wires fabricated from the ceramic materials is critical for these applications. The progress in application of a patented fiber process developed by Clemson University for the fabrication of superconducting wires is reviewed. The effect of particle size and heat treatment on the quality of materials is discussed. Recent advances made at Christopher Newport College in the development of micro-ohm resistance electrical contacts which are capable of carrying the highest reported direct current to this material is presented.

Buoncristiani, A. M.↗

Low-Heat-Leak Electrical Leads For Cryogenic Systems

Electrical leads offering high electrical conductivity and low thermal conductivity developed for use in connecting electronic devices inside cryogenic systems to power supplies, signal-processing circuits, and other circuitry located in nearby warmer surroundings. Strip of superconductive leads on ceramic substrate, similar to ribbon cable, connects infrared detectors at temperature of liquid helium with warmer circuitry. Electrical leads bridging thermal gradient at boundary of cryogenic system designed both to minimize conduction of heat from surroundings through leads into system and to minimize resistive heating caused by electrical currents flowing in leads.

Wise, Stephanie A.↗

Manufacturing and NDE of Large Composite Aerospace Structures at MSFC

NASA's vision for transportation to orbit calls for new vehicles built with new materials technology. The goals of this new launch system development are to improve safety, dramatically reduce cost to orbit, and improve vehicle turn around time. Planned Space Shuttle upgrades include new reusable liquid propellant boosters to replace the solid propellant boosters. These boosters are to have wings and return to the launch site for a horizontal landing on an airport runway. New single and two stages to orbit concepts are being investigated. To reduce weight and improve performance composite materials are proposed for fuel and oxidizer tanks, fuel feedlines, valve bodies, aerostructures, turbomachinery components. For large composite structures new methods of fabrication are being proposed and developed. Containment of cryogenic fuel or oxidizer requires emphases on composite material densification and chemical compatibility. Ceramic matrix and fiber composites for hot rotating turbomachinery have been developed with new fabrication processes. The new requirements on the materials for launcher components are requiring development of new manufacturing and inspection methods. This talk will examine new and proposed manufacturing methods to fabricate the revolutionary components. New NDE methods under consideration include alternative X-ray methods, X-ray laminagraphy, advanced CT, Thermography, new ultrasonic methods, and imbedded sensors. The sizes, complexity, use environment, and contamination restrictions will challenge the inspection process. In flight self-diagnosis and rapid depot inspection are also goals of the NDE development.

Whitaker, Ann↗

Demonstration of Plasma Arc Environmental Technology Applications for the Demilitrization of DOD Stockpiles

Since 1989 the US Army Construction Engineering Research Laboratories (USACERL) have been active participants in the research and development towards establishing Plasma Arc Technology (PAT) as an efficient, economical, and safe hazardous waste immobilization tool. A plasma torch capable of generating high temperatures makes this technology a viable and powerful tool for the thermal destruction of various military industrial waste streams into an innocuous ceramic material no longer requiring hazardous waste landfill disposal. The emerging plasma environmental thermal treatment process has been used to safely and efficiently meet the waste disposal needs for various demilitarized components disposal needs, such as: (1) pyrotechnic smoke assemblies, (2) thermal batteries, (3) proximity fuses, (4) cartridge actuated devices (CADs), and (5) propellant actuated devices (PADs). MSE Technology Applications, Inc., (MSE) has proposed and fabricated a Mobile Plasma Treatment System to be a technology demonstrator for pilotscale mobile plasma waste processing. The system is capable of providing small-scale waste remediation services, and conducting waste stream applicability demonstrations. The Mobile Plasma Treatment System's innovative concept provides the flexibility to treat waste streams at numerous sites and sites with only a limited quantity of waste, yet too hazardous to transport to a regional fixed facility. The system was designed to be operated as skid mounted modules; consisting of a furnace module, controls module, offgas module, and ancillary systems module. All system components have been integrated to be operated from a single control station with both semi-continuous feeding and batch slag-pouring capability.

Smith, Ed↗