Spark plasma sintering of tungsten-based WTaVCr refractory high entropy alloys for nuclear fusion applications
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Diagnostics of Carbon Nanotube Formation in a Laser Produced Plume: An Investigation of the Metal Catalyst by Laser Ablation Atomic Fluorescence Spectroscopy
Carbon nanotubes, elongated molecular tubes with diameters of nanometers and lengths in microns, hold great promise for material science. Hopes for super strong light-weight material to be used in spacecraft design is the driving force behind nanotube work at JSC. The molecular nature of these materials requires the appropriate tools for investigation of their structure, properties, and formation. The mechanism of nanotube formation is of particular interest because it may hold keys to controlling the formation of different types of nanotubes and allow them to be produced in much greater quantities at less cost than is currently available. This summer's work involved the interpretation of data taken last summer and analyzed over the academic year. The work involved diagnostic studies of carbon nanotube formation processes occurring in a laser-produced plume. Laser ablation of metal doped graphite to produce a plasma plume in which carbon nanotubes self assemble is one method of making carbon nanotube. The laser ablation method is amenable to applying the techniques of laser spectroscopy, a powerful tool for probing the energies and dynamics of atomic and molecular species. The experimental work performed last summer involved probing one of the metal catalysts, nickel, by laser induced fluorescence. The nickel atom was studied as a function of oven temperature, probe laser wavelength, time after ablation, and position in the laser produced plume. This data along with previously obtained data on carbon was analyzed over the academic year. Interpretations of the data were developed this summer along with discussions of future work. The temperature of the oven in which the target is ablated greatly influences the amount of material ablated and the propagation of the plume. The ablation conditions and the time scale of atomic and molecular lifetimes suggest that initial ablation of the metal doped carbon target results in atomic and small molecular species. The metal atoms survive for several milliseconds while the gaseous carbon atoms and small molecules nucleate more rapidly. Additional experiments and the development of in situ methods for carbon nanotube detection would allow these results to be interpreted from the perspective of carbon nanotube formation.
deBoer, Gary↗
Plastic flow of plasma sprayed ceramics
The plastic flow of plasma-sprayed ZrO2-8Y2O3 ceramic has been measured at temperatures up to 1250 C and compared to the plastic flow of pressed and sintered ZrO2-8Y2O3. Plasma spraying of binary oxide ceramics is found to result in a metastable state which is inelastic at high temperature but can also be stabilized or devitrified through heat treating so as to decrease plastic properties. The mechanical properties of the as-plasma sprayed and devitrified ceramic sheet material was measured. An improved algorithm that incorporates the inherently nonlinear thermomechanical field equations was used to determine the influence of inelastic material behavior on the thermomechanical response of ceramic coated seal components. Significant creep was found during the thermal shock and steady heating periods with insufficient time during thermal quench to reverse the process, thereby inducing significant residual stresses into the components.
Padovan, J.↗
Improved piston ring materials for 650 deg C service
A program to develop piston ring material systems which will operate at 650C was performed. In this program, two candidate high temperature piston ring substrate materials, Carpenter 709-2 and 440B, were hot formed into the piston ring shape and subsequently evaluated. In a parallel development effort ceramic and metallic piston ring coating materials were applied to cast iron rings by various processing techniques and then subjected to thermal shock and wear evaluation. Finally, promising candidate coatings were applied to the most thermally stable hot formed substrate. The results of evaluation tests of the hot formed substrate show that Carpenter 709-2 has greater thermal stability than 440B. Of the candidate coatings, plasma transferred arc (PTA) applied tungsten carbide and molybdenum based systems exhibit the greatest resistance to thermal shock. For the ceramic based systems, thermal shock resistance was improved by bond coat grading. Wear testing was conducted to 650C (1202F). For ceramic systems, the alumina/titania/zirconia/yttria composition showed highest wear resistance. For the PTA applied systems, the tungsten carbide based system showed highest wear resistance.
Bjorndahl, W. D.↗
In Situ deposition of YBCO high-T(sub c) superconducting thin films by MOCVD and PE-MOCVD
Metalorganic Chemical Vapor Deposition (MOCVD) offers the advantages of a high degree of compositional control, adaptability for large scale production, and the potential for low temperature fabrication. The capability of operating at high oxygen partial pressure is particularly suitable for in situ formation of high temperature superconducting (HTSC) films. Yttrium barium copper oxide (YBCO) thin films having a sharp zero-resistance transition with T( sub c) greater than 90 K and Jc approx. 10 to the 4th power A on YSZ have been prepared, in situ, at a substrate temperature of about 800 C. Moreover, the ability to form oxide films at low temperature is very desirable for device applications of HTSC materials. Such a process would permit the deposition of high quality HTSC films with a smooth surface on a variety of substrates. Highly c-axis oriented, dense, scratch resistant, superconducting YBCO thin films with mirror-like surfaces have been prepared, in situ, at a reduced substrate temperature as low as 570 C by a remote microwave-plasma enhanced metalorganic chemical vapor deposition (PE-MOCVD) process. Nitrous oxide was used as a reactant gas to generate active oxidizing species. This process, for the first time, allows the formation of YBCO thin films with the orthorhombic superconducting phase in the as-deposited state. The as-deposited films grown by PE-MOCVD show attainment of zero resistance at 72 K with a transition width of about 5 K. MOCVD was carried out in a commercial production scale reactor with the capability of uniform deposition over 100 sq cm per growth run. Preliminary results indicate that PE-MOCVD is a very attractive thin film deposition process for superconducting device technology.
Zhao, J.↗
In-situ deposition of YBCO high-Tc superconducting thin films by MOCVD and PE-MOCVD
Metal-Organic Chemical Vapor Deposition (MOCVD) offers the advantages of a high degree of compositional control, adaptability for large scale production, and the potential for low temperature fabrication. The capability of operating at high oxygen partial pressure is particularly suitable for in situ formation of high temperature superconducting (HTSC) films. Yttrium barium copper oxide (YBCO) thin films having a sharp zero-resistance transition with T(sub c) greater than 90 K and J(sub c) of approximately 10(exp 4) A on YSZ have been prepared, in situ, at a substrate temperature of about 800 C. Moreover, the ability to form oxide films at low temperature is very desirable for device applications of HTSC materials. Such a process would permit the deposition of high quality HTSC films with a smooth surface on a variety of substrates. Highly c-axis oriented, dense, scratch resistant, superconducting YBCO thin films with mirror-like surfaces have been prepared, in situ, at a reduced substrate temperature as low as 570 C by a remote microwave-plasma enhanced metal-organic chemical vapor deposition (PE-MOCVD) process. Nitrous oxide was used as a reactant gas to generate active oxidizing species. This process, for the first time, allows the formation of YBCO thin films with the orthorhombic superconducting phase in the as-deposited state. The as-deposited films grown by PE-MOCVD show attainment of zero resistance at 72 K with a transition width of about 5 K. MOCVD was carried out in a commercial production scale reactor with the capability of uniform deposition over 100 sq cm per growth run. Preliminary results indicate that PE-MOCVD is a very attractive thin film deposition process for superconducting device technology.
Zhao, J.↗
Development of New Rocket Engine Liner Materials Based on Copper Alloys with Diamond Particle Additions
Novel copper-diamond materials containing particulate dispersions of diamond within a copper alloy matrix have been produced as next-generation rocket engine combustion chamber liner materials. These Copper-Diamond composite materials have significantly higher thermal conductivity than conventional liner materials and have the potential to increase the engine performance significantly. Liner fabrication techniques include hot pressing and spark plasma sintering, which are capable of scale up to full-size production parts. The materials have been evaluated for thermal cycling resistance and ease of manufacturing. The results indicate great promise of these materials and associated economics to replace state-of-the-art combustion chamber liner materials such as GRCop-84 and NARloy-Z. Novel combustion chamber fabrication processes are discussed, including cladding the liner with jacket materials.
Bhat, Biliyar N.↗
Development of New Rocket Engine Liner Materials Based on Copper Alloys with Diamond Particle Additions
Novel copper-diamond materials containing particulate dispersions of diamond within a copper alloy matrix have been produced as next-generation rocket engine combustion chamber liner materials. These Copper-Diamond (Cu-D) composite materials have significantly higher thermal conductivity than conventional liner materials and have the potential to increase the engine performance significantly. Liner fabrication techniques include hot pressing and spark plasma sintering (SPS), which are capable of scale up to full-size production parts. The materials have been evaluated for thermal cycling resistance and ease of manufacturing. The results indicate great promise of these materials and associated economics to replace state-of-the-art combustion chamber liner materials such as GRCop-84 and NARloy-Z. Combustion chamber fabrication processes are also discussed, including SPS and additive manufacturing.
Bhat, Biliyar N.↗
Tetrafluoroboric Acid Digestion for Accurate Determination of Rare Earth Elements in Coal and Fly Ash by ICP-MS Analysis
Coal and coal-related fly ash often contain rare earth elements (REEs) that have the potential to be utilized as valuable mineral resources. Accurately determining the REE content in coal and fly ash is crucial for resource evaluation. The conventional approach involves using hydrofluoric acid (HF) to dissolve silicates and release REEs, which, however, prolongs the digestion process due to the additional step of complexing fluoride ions (F−) with boric acid (H3BO3). Determining the correct amount of H3BO3 for neutralization can be challenging, and in some instances, the binding of fluoride ions with certain lanthanides (Lns) hampers the accurate determination of all 14 naturally occurring rare earth elements in a single digestion batch by inductively coupled plasma mass spectrometry (ICP-MS). In this study, we present an alternative method that achieves the accurate determination of all 14 naturally occurring REEs using tetrafluoroboric acid (HBF4) followed by ICP-MS analysis. This approach eliminates the need for an F− complexing step. We tested this method on certified REE reference materials, including NIST 1632e (coal) and NIST 1633c (fly ash), as well as the REE geological reference material USGS AGV-1 (andesite). Our results demonstrated excellent recovery rates (relative standard deviation, RSD < ±10%), with a correlation coefficient (r2) exceeding 0.99. Using this method, we investigated the concentrations of all 14 REEs in coal and fly ash samples collected from various locations in the southwestern USA. This improved digestion technique streamlines the analysis process and enhances the accuracy of REE determination, facilitating a more comprehensive evaluation of REE-rich coal and fly ash deposits for resource exploration.
58 GEOSCIENCES↗
Microstructure and Mechanical Properties of Vacuum Plasma Sprayed Cu-8Cr-4Nb
This paper compares the tensile properties of Cu-8Cr-4Nb material produced by VPS to material previously produced by extrusion. The microstructure of the VPS material is also presented. The combustion chamber liner of rocket motors represents an extreme materials application. The liner hot wall is exposed to a 2760 C (5000 F) flame while the cold side is exposed to cryogenic hydrogen liquid. Materials for use in the combustion chamber liner require a combination of high temperature strength, creep resistance, and low cycle fatigue resistance along with high thermal conductivity. The hot side is also subject to localized cycles between reducing and oxidizing environments that degrade the liner by a process called blanching. A new Cu-8 at.% Cr-4 at% Nb (Cu-8Cr-4Nb) alloy has been developed at NASA Lewis Research Center as a replacement for the currently used alloy, NARloy-z (Cu-3 wt.% Ag-0.5 wt.% Zr). The alloy is strengthened by a fine dispersion of Cr2Nb particles. The alloy has better mechanical properties than NARloy-Z while retaining most of the thermal conductivity of pure copper. The alloy has been successfully consolidated by extrusion and hot isostatic pressing (HIPing). However, vacuum plasma spraying (VPS) offers several advantages over prior consolidation methods. VPS can produce a near net shape piece with the profile of the liner. In addition, oxidation resistant and thermal barrier coatings can be incorporated as an integral part of the liner hot wall during the VPS deposition. The low oxygen VPS Cu-8Cr-4Nb exhibits a higher strength than Cu-8Cr-4Nb produced by extrusion at elevated temperatures and a comparable strength at room temperature. Moduli and ductility were not significantly different. However, the ability to produce parts to near-net shape and maintain the good elevated temperature tensile properties of the extruded Cu-8Cr-4Nb makes VPS an attractive processing method for fabricating rocket engine combustion liners.
Holmes, Richard↗
Sequential infiltration synthesis for enhancing multiple-patterning lithography
Simplified methods of multiple-patterning photolithography using sequential infiltration synthesis to modify the photoresist such that it withstands plasma etching better than unmodified resist and replaces one or more hard masks and/or a freezing step in MPL processes including litho-etch-litho-etch photolithography or litho-freeze-litho-etch photolithography.
36 MATERIALS SCIENCE↗
Discovering tungsten-based composites as plasma facing materials for future high-duty cycle nuclear fusion reactors
Abstract Despite of excellent thermal properties and high sputtering resistance, pure tungsten cannot fully satisfy the requirements for plasma facing materials in future high-duty cycle nuclear fusion reactions due to the coupled extreme environments, including the high thermal loads, plasma exposure, and radiation damage. Here, we demonstrated that tungsten-based composite materials fabricated using spark-plasma sintering (SPS) present promising solutions to these challenges. Through the examination of two model systems, i.e., tungsten-zirconium composite for producing porous tungsten near the surface and dispersoid-strengthened tungsten, we discussed both the strengths and limitations of the SPS-fabricated materials. Our findings point towards the need for future studies aimed at optimizing the SPS process to achieve desired microstructures and effective control of oxygen impurities in the tungsten-based composite materials.
21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗
Nonlinear X-ray Optics
Novel X-ray free-electron lasers (XFELs) are capable of producing radiation with unprecedented properties. Specifically, their ultrashort coherent X-ray pulses can generate extreme peak intensities where ordinary rules of light-matter interaction may no longer apply, and nonlinear processes start to become important. XFELs have made it possible to observe some of the most important coherent non-sequential nonlinearities, including X-ray-optical sum frequency generation (SFG), X-ray second harmonic generation (XSHG), two-photon absorption (TPA) and nonlinear two-photon Compton scattering (2PCS). In particular, the 2PCS experiment has led to unexpected results, namely the observation of a substantial anomalous red shift in the energy of photons generated by nonlinear two-photon X-ray Compton scattering in beryllium. The energy shift is in addition to the predicted nonlinear Compton shift and was neither expected from extrapolations from linear X-ray interactions nor from nonlinear effects at optical wavelengths. Our results suggest a novel nonlinear scattering mechanism that can only be observed at high fields at X-ray wavelengths, where the photon energy is a significant fraction of the electron rest mass (and thus a significant momentum transfer to the electron occurs during the scattering) and where the interaction is not dominated by the quiver motion of the electron in the field (ponderomotive potential) as is usually the case at longer (optical) wavelengths. The goal of this research project was the investigation of fundamental nonlinear X-ray-matter interactions. As these processes are typically weak, part of this research is the exploration of more efficient nonlinear X-ray processes by studying novel mechanisms including solid-state effects, the assistance of optical radiation and novel phase-matching techniques. These experiments require extremely large X-ray field strengths, such as produced by XFELs. Nonlinear X-ray effects can lead to important applications in many research fields. For example, it could lead to instantaneous plasma diagnostics for materials in extreme conditions, as a method for combining atomic-scale structural sensitivity with chemical specificity, or as a probe of electron dynamics in solids on the attosecond (1 as = 10 -18 s) time- and Ångstrom (10 -10 m) length scales. In addition, a detailed understanding of nonlinear X-ray matter interactions is crucial for understanding and extending the limits of structural determination at high intensity such as in serial femto-crystallography. The results could have a profound impact on advanced XFEL light sources such as the LCLS-II.
47 OTHER INSTRUMENTATION↗
Combination Thermal Barrier And Wear Coatings For Engines
Thermal-barrier layers covered with self-lubricating surface layers. Zirconia thermal-barrier coat applied to surface of combustion chamber in engine by plasma-arc spraying. Then PS-200 plasma-arc sprayed onto zirconia. Self-lubricating coat prevents sliding contact between thermal barrier and piston ring, effectively preventing both wear and production of additional heat via friction. Other combinations of thermal-barrier and self-lubricating, wear-resistant coating materials used as long as two materials adhere to each other, applied by use of similar or compatible processes, have similar coefficients of thermal expansion, sufficiently strong at high temperatures, and affordable.
Weingart, Mike↗
Cost Models for MMC Manufacturing Processes
Processes for the manufacture of advanced metal matrix composites are rapidly approaching maturity in the research laboratory and there is growing interest in their transition to industrial production. However, research conducted to date has almost exclusively focused on overcoming the technical barriers to producing high-quality material and little attention has been given to the economical feasibility of these laboratory approaches and process cost issues. A quantitative cost modeling (QCM) approach was developed to address these issues. QCM are cost analysis tools based on predictive process models relating process conditions to the attributes of the final product. An important attribute, of the QCM approach is the ability to predict the sensitivity of material production costs to product quality and to quantitatively explore trade-offs between cost and quality. Applications of the cost models allow more efficient direction of future MMC process technology development and a more accurate assessment of MMC market potential. Cost models were developed for two state-of-the art metal matrix composite (MMC) manufacturing processes: tape casting and plasma spray deposition. Quality and Cost models are presented for both processes and the resulting predicted quality-cost curves are presented and discussed.
Elzey, Dana M.↗
Space Weathering Investigations Enabled by NASA's Virtual Heliophysical Observatories
Structural and chemical impact of the heliospheric space environment on exposed planetary surfaces and interplanetary dust grains may be generally defined as space weathering . In the inner solar system, from the asteroid belt inwards towards the Sun, the surface regolith structures of airless bodies are primarily determined by cumulative meteoritic impacts over billions of years, but the molecular composition to meters in depth can be substantially modified by irradiation effects. Plasma ions at eV to keV energies may both erode uppermost surfaces by sputtering, and implant or locally produce exogenic material, e.g. He-3 and H2O, while more energetic ions drive molecular change through electronic ionization. Galactic cosmic ray ions and more energetic solar ions can impact chemistry to meters in depth. High energy cosmic ray interactions produce showers of secondary particles and energetic photons that present hazards for robotic and human exploration missions but also enable detection of potentially useable resources such as water ice, oxygen, and many other elements. Surface sputtering also makes ejected elemental and molecular species accessible for in-situ compositional analysis by spacecraft with ion and neutral mass spectrometers. Modeling of relative impacts for these various space weathering processes requires knowledge of the incident species-resolved ion flux spectra at plasma to cosmic ray energies and as integrated over varying time scales. Although the main drivers for investigations of these processes come from NASA's planetary science and human exploration programs, the NASA heliophysics program provides the requisite data measurement and modeling resources to enable specification of the field & plasma and energetic particle irradiation environments for application to space weather and surface weathering investigations. The Virtual Heliospheric Observatory (VHO), Virtual Energetic Particle Observatory (VEPO), Lunar Solar Origins Exploration (LunaSOX), and Space Physics Data Facility (SPDF) services now provide a wide range of inner heliospheric spacecraft data that can be applied to space weathering of potential exploration destinations including the Moon, asteroids, and the moons of Mars, as well to radiation hazard assessment for the spacecraft and human explorers. For example, the new VEPO service for time-averaging of multi-source ion flux spectra enables the specification of composite flux spectra from a variety of ongoing and legacy missions for applications to surface interaction modeling. Apollo to Artemis data resources of LunaSOX enable specific space weathering investigations for the Moon, while VHO more generally covers the space field and plasma environments of the inner and outer solar system from the sunward-most perihelia of the twin Helios spacecraft to the ongoing heliosheath passages of the twin Voyagers. Composite multi-source spectra from VEPO can also be applied to the continuing compilation of accumulated 1-AU fluence spectra, mostly contributed by solar wind plasma and energetic particle events, for determination of time-averaged particle compositional and kinetic energy output from the Sun and for modeling of long-term irradiation impacts on planetary surfaces.
Cooper, John F.↗
Low Cost, High Volume, Carbon Fiber Precursor for Plasma Oxidation
Light weighting with carbon fiber is critical to improving the energy efficiency of wind turbines, airplanes, and automobiles, but the high cost of carbon fiber continues to limit market growth and applications. Half of this cost is in the raw materials. For the carbon fiber market to reach the next level of adoption, the cost of both the raw materials and conversion must be reduced. This project considered the combination of low-cost, textile-grade precursors combined with the increased efficiency of plasma oxidation to greatly reduce the cost of carbon fiber. The primary objective of this project was to make industrial-grade carbon fiber (550 ksi tensile strength, 35 Msi tensile modulus) from textile-grade PAN precursors, something that cannot be achieved with conventional oxidation and to date has not been achieved with any technology. To accomplish this, the project team iteratively optimized the process conditions in the plasma oxidation and carbonization stages to maximize the tensile properties of the resultant carbon fibers. This involved implementing experimental designs for both stages, whereby process conditions (e.g. temperature) were varied and correlated to fiber properties. Samples of oxidized PAN fibers (OPFs) were prepared using a small pilot-scale plasma oxidation oven at 4XTechnologies (4XT). The thermal, chemical, and physical properties of OPF samples were analyzed by the University of Tennessee (UTK) and Oak Ridge National Laboratory (ORNL). The OPF samples were then converted to carbon fiber by subsequent low- and high-temperature carbonization using a lab-scale furnace at ORNL. The resultant carbon fibers were tested for tensile strength also at ORNL, and the results were fed back into the experimental design. Of the hundreds of carbon fiber samples produced over the course of the project, the best sample had an average break strength of 479 ksi and modulus of 33 Msi. While the best tensile properties achieved fell short of the final project targets of 550 ksi for break strength and 35 Msi for modulus, the team demonstrated the potential to produce industrial-grade carbon fiber using textile-grade precursors. The best performing fiber samples had tensile properties that are 87% of the goal for tensile strength and 94% of the goal for tensile modulus. With additional optimization work, it is likely that the targets could be achieved, since only a fraction of the process parameter space was explored during this project. 4XT and its affiliate (4M) have already secured funding through private equity, and there is a CRADA (Cooperative Research and Development Agreement) project currently underway with the Carbon Fiber Technology Center (CFTF) at ORNL to continue this research. Additionally, while not an original goal of the project, the carbon fibers for most samples had diameters >8.5μm. This is considerably larger than commercially available carbon fiber products, which can impart unique properties to the composites (e.g. increased compressive strength) and decrease manufacturing costs even further. Moreover, these fibers were oxidized with plasma oxidation using residence times ranging <60mins, which would be considered fast for normal diameter fibers, but it is as much as 5x faster when factoring in the diameter of the fibers.
36 MATERIALS SCIENCE↗
Recent Advances in LIBS for Real-Time Detection of Silicone Contaminants on CFRP Surfaces
Laser induced breakdown spectroscopy (LIBS) is a materials characterization technique that has been advanced and refined to provide in situ, real-time quality control of carbon fiber reinforced polymer (CFRP) surfaces. As part of an effort to improve process control for adhesive bonding, a LIBS system was designed and assembled at NASA Langley Research Center (LaRC) to enable detection of ultralow concentrations of silicone contamination on CFRP adherends. The LIBS instrument provides high sensitivity detection and quasi-nondestructive surface characterization of CFRP adherends prior to adhesive bonding. This review focuses on the advancements at LaRC using LIBS as a quality control tool for the detection of silicone contaminants for improved adhesive bonding reliability of CFRP materials. This work describes how the LIBS technique was advanced by analyzing the laser parameters, studying the laser-matter interactions, and performing time-resolved measurements to determine the optimal plasma conditions for elemental detection. In addition, LIBS results were compared to X-ray photoelectron spectroscopy data to enable quantitative analysis from analytical calibration curves. Examples are shown of how to perform surface mapping of silicone contamination. Finally, a brief discussion is also presented on LIBS instrumentation, recommendations for laser parameters and instrumentation components, and LIBS technique maturity.
Surface characterization, Carbon fiber reinforced ↗