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Ultrapure copper fluoride synthesis, analytical techniques, and production of one kilogram for cathode material
Space Flight Hardware (SFH) experiences intense vibratory loading during flight, which only lasts a few minutes. When determining the appropriate size of these components to withstand such loading without becoming damaged (plastically deforming or breaking), standard design practice is to assume that the peak dynamic loads are applied statically. In doing so, the resulting stress is compared against a material strength parameter obtained from a quasi-static experiment. Since the near-peak stresses are only experienced over a small fraction of time in reality, this approach leads to design conservatism that unnecessarily increases structural mass as well as the associated inefficiency and financial cost. In an effort to modernize engineering design standards to appropriately consider the higher practical strength of dynamically loaded structures, this overarching research project seeks to develop an experimental test procedure for quantifying the dynamic strength of metallic alloys as a function of excitation frequency. In the ideal case, the characterization test would include an in-situ method for monitoring the onset and progression of plastic deformation of the test specimen undergoing vibratory loading. These new tests are designed to be high intensity (forcing amplitude), short term (60 seconds at full amplitude), and cyclic in nature (sinusoidal excitation via attached stinger to an otherwise cantilevered beam). In addition, the initial metallic alloy under investigation is 6061 aluminum, due to its wide use and applicability for SFH. Thus far, the most promising monitoring method under development with live-capacity is to track hysteresis behavior of the beam from power dissipation trends, calculated via force (from transducer on excitation stinger) and velocity (measurements from Laser Doppler Vibrometer) data and work to distinguish between elastic and plastic features. As a key component of this ongoing method development, any pseudo-live indication of plasticity can be corroborated against the outcome of a pre-post assessment of damage via macroscopic evaluation of beam geometry (i.e. assessing any permanent change in the beam’s tip deflection). Support for experimental design decisions as well as dynamic strength data from tests with excitation frequencies of 10, 40, and 55 Hz will be discussed. This work contributes to the foundation for a new type of vibration-based characterization experiments and generates initial data on the functional strength of 6061 aluminum under the conditions considered. Keywords: vibrations, plastic deformation, aluminum
This report describes the efforts completed during the contract period beginning November 1, 1990 and ending April 30, 1991. Samples of product hygiene and potable water from WRT 3A were supplied by NASA/MSFC prior to contract award on July 24, 1990. Humidity condensate samples were supplied on August 3, 1990. During the course of this contract chemical analyses were performed on these samples to qualitatively determine specific components comprising, the measured organic carbon concentration. In addition, these samples and known standard solutions were used to identify and develop methodology useful to future comprehensive characterization of similar samples. Standard analyses including pH, conductivity, and total organic carbon (TOC) were conducted. Colorimetric and enzyme linked assays for total protein, bile acid, B-hydroxybutyric acid, methylene blue active substances (MBAS), urea nitrogen, ammonia, and glucose were also performed. Gas chromatographic procedures for non-volatile fatty acids and EPA priority pollutants were also performed. Liquid chromatography was used to screen for non-volatile, water soluble compounds not amenable to GC techniques. Methods development efforts were initiated to separate and quantitate certain chemical classes not classically analyzed in water and wastewater samples. These included carbohydrates, organic acids, and amino acids. Finally, efforts were initiated to identify useful concentration techniques to enhance detection limits and recovery of non-volatile, water soluble compounds.
Various investigators propose the lunar surface contains widely distributed volatiles, especially water- like species, i.e. OH and H2O. Surface volatiles are theorized to exist as a hydrated regolith layer, concentrated in extremely cold polar permanently shadowed regions (PSR), and/or solar wind implantation reservoirs in lunar glasses. The proposed sources of lunar surface volatiles range from cometary impacts, solar wind, or a supply present during moon formation. Future Artemis missions aim to collect and return the samples containing volatiles collected near lunar polar craters or PSRs. We, as advanced curation scientists, are responsible for developing techniques and methodologies for preserving returned sample integrity as much as possible. Pristine volatile-bearing samples are invaluable to the scientific community seeking to unravel the history of the solar system. Realistically, a sample will experience alteration during collection, transportation back to earth, and storage. The Planetary Exploration and Astromaterials Research Lab (PEARL) seeks to understand temperature and pressure effects on high-fidelity volatile-containing regolith simulants, the foundation for the future of cold curation. This abstract outlines the separation, identification, and quantification of headspace gases over volatile ice feed stock material using gas chromatography/mass spectrometry (GC/MS). Preliminary objectives concentrated on sample handling, reproducibility, and understanding the elution characteristics for each analyte. Initial GC/MS method development experiments utilized diluted static headspace sample preparation. Diluted samples were used because sampling headspace gases directly from a vial containing liquid analyte resulted in overloading of the column and detector. Overloading is evident based on chromatogram peak shapes and instrument contamination, or carry over, between experiments. A mixture of three alcohols were used for a majority of the sample handling and reproducibility studies. Reproducibility was tested via multiple users, calibration curves, and check standards. Stock solutions of condensed lunar volatile analytes included methanol, ammonia in methanol, hydrogen sulfide in water, and an equal volume mixture of methanol, ethanol, and isopropanol. Current samples use room air as the headspace sample matrix, however future experiments will incorporate an inert purge gas, such as argon or nitrogen. Three mL of each analyte solution were capped in separate 20 mL crimp top GC vials. Dilutions were carried out by removing an aliquot of headspace gases with a calibrated 1 mL gastight syringe and immediately transferring to a 20 mL capped crimp top vial. The GC/MS is a Thermo Fisher Trace 1310/ISQ 7000 with a TriPlus RSH autosampler and split/splitless injector module. The experiments outlined in this abstract use the following hardware: a 2.5 mL gastight headspace syringe tool, 1 mm ID x 78.5 mm length ultra-inert straight injection liner, and a TG-BondQ 30 m × 0.32 mm × 10 μm column. Various parameters, such as hardware selection and the temperature, pressure, and split ratio set points, continue to evolve as the overall experiment is refined. Diluted headspace chromatograms were collected for the individual stock solutions. Retention times, peak shapes, and mass spectra were evaluated and added to the data processing method for each molecule of interest. Figure 1 shows the total ion chromatograms for the three major lunar volatile simulant stock solutions: methanol, 7 N ammonia in methanol, and 0.4% hydrogen sulfide in water. Tailing peak shapes for ammonia (2.98 min rt) and water (4.06 min rt) indicate the molecules are not properly eluting from the selected column with the current separation method. Additionally, hydrogen sulfide and ammonia have overlapping peak windows, which could impact quantification. Ongoing experiments aim to address the peak shape and overlapping via the separation method and hardware selection. Sample preparation reproducibility experiments used stock solution containing equal volumes of a non- interactive mixture of methanol, ethanol, and isopropanol. Mass spectrum ion traces were used to identify and quantify all three alcohols. Peaks were automatically detected, identified, and integrated through the mass spectra detection and processing parameters. Calibration response curves and check standards were used to evaluate the validity of the sample preparation procedure. Figure 2 shows the methanol chromatogram peak area versus total headspace dilution volume transferred from the alcohol mixture vial. The calibration response curves and check standards validate sample preparation procedure. Continuing data analysis efforts are working towards correlating the peak area and instrument response factor to the headspace analyte concentration and condensed phase composition. Static headspace gas chromatography theory relies on Dalton’s law, Raoult’s law, Henry’s Law, and the Kolb and Ettre equation to associate peak area to the analyte composition in a non-ideal solution. Equation 1 is a simplified expression derived from the aforementioned theories. Future experiments involve liquid injections of the individual stock solutions, liquid and headspace analysis of various stock solution combinations, and the addition of regolith simulants to the mixtures. Temperature is another variable expected to affect reaction rates and will be explored.
The development of computational fluid dynamics (CFD) methods for unsteady aerodynamic analysis is described. Special emphasis is placed on considerations that are required for application of the methods to unsteady aerodynamic flow problems. Two broad categories of topics are presented to illustrate the major points. Although primary application of these CFD methods is to relatively low frequency oscillatory phenomena such as flutter, the ideas that are presented may be of value to developers of computational aeroacoustic methods for predicting high frequency acoustics.
Several noise sources combine to make up the total helicopter noise spectrum. The sources that are most important to community annoyance are the tail rotor (discrete), main rotor (unsteady), and engine (unsteady). The periodic and broadband noise components of the helicopter rotor were enumerated, and an approach to rotorcraft noise prediction was discussed. Helicopter noise sources were prioritized, and design improvements to reduce noise were reviewed. Main rotor noise is believed to be the key to quieter helicopters since there are proven and relatively inexpensive ways to handle the tail rotor. Blade Vortex Interaction (BVI) noise is a problem to some extent with all helicopters, particularly in the descent mode. Methodology must be developed to allow forecast and control of this type of noise. Additional means of controlling it, such as reduced rotor speeds for terminal operations should also be pursued because they may be the most effective means of control and they apply to all helicopter models. Main rotor broadband noise is the limiting factor in overall helicopter noise generation. Development of semi-empirical methods to predict its behavior is necessary if results are to be achieved in the short time period available.
The development of probabilistic structural analysis methods is a major part of the SSME Structural Durability Program and consists of three program elements: composite load spectra, probabilistic finite element structural analysis, and probabilistic structural analysis applications. Recent progress includes: (1) the effects of the uncertainties of several factors on the HPFP blade temperature pressure and torque, (2) the evaluation of the cumulative distribution function of structural response variables based on assumed uncertainties on primitive structural variables, and (3) evaluation of the failure probability. Collectively, the results obtained demonstrate that the structural durability of critical SSME components can be probabilistically evaluated.
The development of unstructured-grid methods for the solution of the equations of fluid flow and what was learned over the course of the research are summarized. The focus of the discussion is on the solution of the time-dependent Euler equations including spatial discretizations, temporal discretizations, and boundary conditions. An example calculation with an implicit upwind method using a CFL number of infinity is presented for the Boeing 747 aircraft. The results were obtained in less than one hour CPU time on a Cray-2 computer, thus, demonstrating the speed and robustness of the capability. Additional calculations for the ONERA M6 wing demonstrate the accuracy of the method through the good agreement between calculated results and experimental data for a standard transonic flow case.
This report discusses the development and application of metrology methods called photogrammetry and videogrammetry that make accurate measurements from photographs. These methods have been adapted for the static and dynamic characterization of gossamer structures, as four specific solar sail applications demonstrate. The applications prove that high-resolution, full-field, non-contact static measurements of solar sails using dot projection photogrammetry are possible as well as full-field, non-contact, dynamic characterization using dot projection videogrammetry. The accuracy of the measurement of the resonant frequencies and operating deflection shapes that were extracted surpassed expectations. While other non-contact measurement methods exist, they are not full-field and require significantly more time to take data.
During fabrication, assembly, and testing of spacecraft and flight hardware it is vital to avoid contaminants that can cause degradation and could result in significant failure. Yet, there is no existing contamination monitoring method that provides the identity of airborne particles in a cleanroom facility. Knowing the particle identities, would allow scientists and engineers to determine the source of the contaminants and prevent setbacks before they occur or cause damage. Current cleanliness monitoring methods include airborne particle counters (APCs), fallout filters, and visual inspections. Particle counts from APCs are the primary metric used to define a cleanroom class and hence its level of cleanliness, but do not provide identification nor can they differentiate between large and small sizes of particles. In addition, using fallout filters is not a proactive, timely, or representative approach to cleanroom contamination monitoring because these samples are only retrieved after 30 days and are placed away from spacecraft processing to avoid interference with operations. In contrast, the forced air sampling method can collect a sample within an hour at any location required and provide results in less than a day. This system uses a cassette and filter sample medium to capture airborne particles which are then taken to a scanning electron microscope with energy dispersive spectroscopy (SEM/EDS) to identify and size the captured particles. Development of forced air sampling into an established laboratory capability will allow for fast sampling and routine identification of unknown contamination sources within the cleanroom. The test method development required market research for an air sampling cassette that increases sample collection efficiency and a filter with low enough background contamination to allow differentiation between a blank (control) and the collected sample. It was determined that a conductive black cassette and a polycarbonate filter were the best options. Conductive black cassettes, in comparison to the standard styrene, are manufactured using polypropylene filled with carbon. This makes the cassette conductive and minimizes the tendency of particles to stick to the wall of the cassette due to electrostatic force. In previous trials a mixed cellulose ester (MCE) filter was used to capture the contaminants, however the rougher surface of the filter contributed to entrapment of the particles within the filter structure and made it harder to identify the particles. In comparison, track etched polycarbonate filters have random cylindrical pores and a smooth surface which contributes to uniform sample distribution on the surface of the filter. Future work includes: testing the system using control samples to determine the efficiency and suitability of the medium, performing sample collection in various environments to establish ideal operating parameters and analyzing contaminant particles using SEM/EDS and assistant characterization techniques. Once fully developed, employing the forced air sampling method will help to prevent damage to spacecraft, avoid schedule delays, and allow for mission success.
The high speed civil transport is a commercial aircraft that is expected to carry 300 passengers at Mach 2.4 over a range of more than 6000 nautical miles. With the existing commercial structural material technology (i.e., aluminum) the performance characteristics of the high speed civil transport would not be realized. Therefore there has been a concerted effort in the development of light weight materials capable of withstanding elevated temperatures for long duration. Thermoplastic composite materials are such candidate materials and the understanding of how these materials perform over the long term under harsh environments is essential to safe and effective design. The matrix dominated properties of thermoplastic composites are most affected by both time and temperature. There is currently an effort to perform short term testing to predict long term behavior of in-plane mechanical properties E22 (transverse modulus of elasticity) and G12 (shear modulus). Out-of-plane properties such as E33, G13, and G23 are inherently more difficult to characterize. This is especially true for the out-of-plane shear modulus G23 and hence there is no existing acceptable standard test method. Since G23 is the most matrix dominated property, it is essential that a test method be developed. A shear test methodology is developed to do just that. The test method, called the double notched specimen, along with the previously developed shear gage was tested at room temperature. Mechanical testing confirmed the attributes of the methodology. A finite element parametric study was conducted for specimen optimization. Moire interferometry, a high sensitivity laser optical method, was used for full-field analysis of the specimen. From this work, material parameters will be determined and thus enable the prediction of long term material behavior of laminates subjected to general loading states.
On-orbit testing of a large space structure will be required to complete the certification of any mathematical model for the structure dynamic response. The process of establishing a mathematical model that matches measured structure response is referred to as model correlation. Most model correlation approaches have an identification technique to determine structural characteristics from the measurements of the structure response. This problem is approached with one particular class of identification techniques - matrix adjustment methods - which use measured data to produce an optimal update of the structure property matrix, often the stiffness matrix. New methods were developed for identification to handle problems of the size and complexity expected for large space structures. Further development and refinement of these secant-method identification algorithms were undertaken. Also, evaluation of these techniques is an approach for model correlation and damage location was initiated.
Main stream industry software development practice has gone from a traditional waterfall process to agile iterative development that allows for fast response to customer inputs and produces higher quality software at lower cost. How can we, the space ops community, adopt state of the art software development practice, achieve greater productivity at lower cost, and maintain safe and effective space flight operations? At NASA Ames, we are developing Mission Control Technologies Software, in collaboration with Johnson Space Center (JSC) and, more recently, the Jet Propulsion Laboratory (JPL).
Monitoring of the atmosphere for fission products ( 131m Xe, 133m Xe, 133 Xe, and 135 Xe) is performed by various laboratories to detect nuclear explosions. Quantification of 127 Xe is not routinely performed by laboratories measuring atmospheric radioxenon because it is not a fission product. 127 Xe was recently detected by a ground-based beta-gamma air monitoring system. When measured using beta-gamma coincidence detector systems, such as those in use on the International Monitoring System (IMS) of the Comprehensive Nuclear-Test-Ban Treaty (CTBT), 127 Xe can interfere with the quantification of fission product radioxenon due to overlap of the 127 Xe beta-gamma coincidence signatures with those of fission product radioxenon. Here, this work demonstrates quantification of 127 Xe at different laboratories with different measurement techniques. Production and purification of 127 Xe was performed by neutron activation of enriched 126 Xe. The purified 127 Xe was then split between laboratories, and detection and quantification methods were developed. At Idaho National Laboratory, a quantification method involving high purity germanium detectors was devised that included self-attenuation correction. At AWE, a beta-gamma coincidence counting method, as used in support of the IMS, was modified to enable the measurement and analysis of the 127 Xe samples. Corrections were made for self-attenuation, which showed a strong xenon volume dependency, for some coincidence signatures. The gas sample activity concentration was used as the comparison metric and it showed excellent agreement between the methods.
The development is summarized of unstructured grid methods for the solution of the equations of fluid flow and some of the lessons learned are shared. The 3-D Euler equations are solved, including spatial discretizations, temporal discretizations, and boundary conditions. An example calculation with an upwind implicit method using a CFL (Courant Friedricks Lewy) number of infinity is presented for the Boeing 747 aircraft. The results obtained in less than one hour of CPU time on a Cray-2 computer, thus demonstrating the speed and robustness of the present capability.
This viewgraph presentation outlines the development at Ames Research Center of advanced computational methods to provide appropriate fidelity computational analysis/design capabilities. Current thrusts of the Ames research include: 1) methods to enhance/accelerate viscous flow simulation procedures, and the development of hybrid/polyhedral-grid procedures for viscous flow; 2) the development of real time transonic flow simulation procedures for a production wind tunnel, and intelligent data management technology; and 3) the validation of methods and the flow physics study gives historical precedents to above research, and speculates on its future course.
Historically, advances in aerospace engine performance and durability have been linked to improvements in materials. Recent developments in ceramic matrix composites (CMCs) have led to increased interest in CMCs to achieve revolutionary gains in engine performance. The use of CMCs promises many advantages for advanced turbomachinery engine development and may be especially beneficial for aerospace engines. The most beneficial aspects of CMC material may be its ability to maintain its strength to over 2500 F, its internal material damping, and its relatively low density. Ceramic matrix composites reinforced with two-dimensional woven and braided fabric preforms are being considered for NASA s next-generation reusable rocket turbomachinery applications (for example, see the preceding figure). However, the architecture of a textile composite is complex, and therefore, the parameters controlling its strength properties are numerous. This necessitates the development of engineering approaches that combine analytical methods with limited testing to provide effective, validated design analyses for the textile composite structures development.
Space Flight Hardware (SFH) experiences intense vibratory loading during flight, which only lasts a few minutes. When determining the appropriate size of these components to withstand such loading without becoming damaged, standard design practice is to assume that the peak dynamic loads are applied statically. In doing so, the resulting stress is compared against a material strength parameter obtained from a quasi-static experiment. Since the near-peak stresses are only experienced over a small fraction of time in reality, this approach leads to design conservatism that unnecessarily increases structural mass as well as the associated inefficiency and financial cost. In an effort to modernize engineering design standards to appropriately consider the higher practical strength of dynamically loaded structures, this overarching research project seeks to develop an experimental test procedure for quantifying the dynamic strength of metallic alloys as a function of excitation frequency. In the ideal case, the characterization test would include an in-situ method for monitoring the onset and progression of plastic deformation of the test specimen undergoing vibratory loading. These new tests are designed to be high intensity (forcing amplitude), short term (60 seconds at full amplitude), and cyclic in nature (sinusoidal excitation via attached stinger to an otherwise cantilevered beam). In addition, the initial alloy under investigation is 6061 aluminum, due to its wide use and applicability for SFH. Thus far, the primary candidate under development with live-capacity is to track hysteresis behavior of the beam from power dissipation trends, calculated via force (from transducer on excitation stinger) and velocity (measurements from Laser Doppler Vibrometer) data and work to distinguish between elastic and plastic features. As a key component of this ongoing method development, any pseudo-live indication of plasticity could be corroborated against the outcome of a pre-post assessment of damage via macroscopic evaluation of beam geometry (i.e. assessing any permanent change in the beam’s tip deflection). Support for experimental design decisions as well as dynamic strength data from tests with excitation frequencies of 10, 40, and 55 Hz will be discussed. This work contributes to the foundation for a new type of vibration-based characterization experiments and generates initial data on the functional strength of 6061 aluminum under the conditions considered.