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Microgravity Disturbance Characterization of the Quench Module Insert (QMI) Phase Change Device (PCD)

The Materials Science Research Facility (MSRF) is a multi-user, multi-purpose facility for materials science research. One experiment within the MSRF will be the Quench Module Insert (QMI), a high-temperature furnace with unique capabilities for processing different classes of materials. The primary functions of the QMI furnace are to melt, directionally solidify, and quench metallic samples, providing data to aid in understanding the effects of the microgravity environment on the characteristics of these processed metals. The QMI houses sealed individual sample ampoules containing material to be processed. Quenching of the samples in the QMI furnace is accomplished by releasing low-melting-point metallic shoes into contact with the outside of the sample ampoule, dissipating heat and cooling the sample inside. The impact from this method of quench will induce sample vibrations which could be large enough to adversely affect sample quality. Utilizing breadboard hardware, the sample quench sequence, releasing the shoes, was conducted. Data was collected from accelerometers located on the breadboard sample cartridge, indicating the maximum acceleration achieved by the sample. The primary objective of the test described in this presentation was to determine the acceleration imparted on the sample by the shoe contact. From this information, the science community can better assess whether this method of quench will allow them to obtain the data they need.

Gattis, Christy↗

Preparation for and Performance of a Pseudomonas aeruginosa Biofilm Experiment On Board the International Space Station

Biofilms are a problem on Earth given their ability to degrade the materials upon which they grow and due to their relevance to infections. Remarkably, 65% and 80% of infections and chronic diseases on Earth are associated with biofilms, respectively. In space, these problems' impact is higher because the crew's lives and mission success depend on nominal operation of mechanical systems. Furthermore, the isolated confined environment nature of spaceflight may increase the rates of disease transmission. In the case of the International Space Station (ISS), biofilms are an identified problem on the Environmental Control and Life Support System (ECLSS), namely on the water processor assembly (WPA). In late 2019, the Space Biofilms experiment launched towards ISS to (i) characterize the mass, thickness, morphology, and gene expression of biofilms formed in space with respect to matched Earth controls, (ii) interrogate the expression of antimicrobial resistance genes, and (iii) test novel materials as potential biofilm control strategies for future ECLSS components. For this, 288 bacterial samples were prepared prior to the launch of the Northrop Grumman CRS-12 mission from NASA's Wallops Flight Facility. The samples were integrated into the spaceflight hardware, BioServe's Fluid Processing Apparatus (FPA) packed in sets of eight in Group Activation Packs (GAP). Half of these samples were activated and terminated on orbit by NASA astronauts Jessica Meir and Christina Koch, while the remaining half were processed equivalently on Earth. The spaceflight bacterial samples of Space Biofilms returned on board SpaceX' CRS-19 Dragon spacecraft, in early 2020. We here describe the test campaign implemented to verify the experiment design and confirm it would enable us to achieve the project's scientific goals. This campaign ended with the Experiment Verification Test (EVT), from which we here present example morphology and transcriptomic results. We describe in detail the sample preparation prior to flight, including cleaning and sterilization of the coupons of six materials (SS316, passivated-SS316, lubricant impregnated surface, catheter-grade silicone with and without a nanotopography, and cellulose membrane), loading and integration of growth media, bacterial inoculum, fixative and preservative to enable experiment termination on orbit. Additionally, we describe the performance of the experiment on board the ISS, including crew activities, use of assets, temperature profile, and experiment timeline; all leading to a successful spaceflight experiment.

Pamela Flores↗

Lignin content of Populus trichocarpa residues after CELF pretreatment and CBP fermentation

Here we present a dataset of lignin content from a woody energy crop (Populus trichocarpa) residues after a series of co-solvent enhanced lignocellulosic fractionation (CELF) pretreatment and consolidated bioprocessing (CBP) process. The natural poplar variant GW-9947 from the Center for Bioenergy Innovation (CBI) was used. The poplar was knife milled and passed through a 1 mm sieve and CELF pretreatment was performed in a Parr autoclave reactor with 7.5 wt % solids loading, 0.5 wt% H2SO4 as catalyst at 150°C with 5, 15, 25 and 30 minutes, respectively. Tetrahydrofuran was added in a 1:1 mass ratio with water as the pretreatment solvent. The residues from CELF pretreatment were then subjected to CBP using the bacterium C. thermocellum DSM 1313. CBP fermentations were performed at 60 °C in a shaker at 50, 75, and 100 grams/L solids loadings. The Klason lignin was measured using a two-step acid hydrolysis process. In brief, the poplar samples were first hydrolyzed by 72 wt% sulfuric acid at 30 oC for an hour. The hydrolysates were then diluted to 4 wt% sulfuric acid using deionized water and subsequently autoclaved at 121 oC for 1 h. Upon the completion of the two-step hydrolysis, the resulting solution was cooled to room temperature and the precipitate was then filtered through a G8 glass fiber filter through a crucible, dried at oven for overnight, and weighed to get the Klason lignin content. The lignin data provides information about lignin content changes after CELF and C. thermocellum CBP process.

Lignin Populus trichocarpa CELF pretreatment CBP f↗

Vanadium isotopic composition and concentrations of ferromagnesian elements in returned lunar samples

The effects are sought of an energetic charged particle irradiation of solar system material which is postulated as having taken place early in its history. A similar irradiation took place much more recently in the history of lunar samples and meteorites and this process is studied by means of a variety of monitors including highly sensitive noble gas nuclides, radionuclides, and tracks. Such monitors cannot be used to study the postulated early irradiation since it could have taken place under conditions such that these monitors were not retained or were subsequently lost. Accordingly, it is necessary that a nongaseous element be used to search for the effects of this irradiation, and one of the most sensitive of these is the vanadium isotopic composition. A comparative study is made of the 50 sub V/51 sub V ratios in 15 meteoritic, 5 terrestrial, and 11 lunar samples.

Lipschutz, M. E.↗

Preparative electrophoresis for space

A premise of continuous flow electrophoresis is that removal of buoyancy-induced thermal convection caused by axial and lateral temperature gradients results in ideal performance of these instruments in space. Although these gravity dependent phenomena disturb the rectilinear flow in the separation chamber when high voltage gradients or thick chambers are used, distortion of the injected sample stream due to electrohydrodynamic effects cause major broadening of the separated bands. The electrophoresis separation process is simple, however flow local to the sample filament produced by the applied electric field have not been considered. These electrohydrodynamic flows distort the sample stream and limit the separation. Also, electroosmosis and viscous flow combine to further distort the process. A moving wall concept is being proposed for space which will eliminate and control the disturbances. The moving wall entrains the fluid to move as a rigid body and produces a constant residence time for all samples distributed across the chamber thickness. The moving wall electrophoresis chamber can only be operated in space because there is no viscous flow in the chamber to stabilize against thermal convection.

Rhodes, Percy H.↗

Preparative electrophoresis for space

A premise of continuous flow electrophoresis is that removal of buoyance-induced thermal convection caused by axial and lateral temperature gradients results in ideal performance of these instruments in space. Although these gravity dependent phenomena disturb the rectilinear flow in the separation chamber when high voltage gradients or thick chamber are used, distortion of the injected sample stream due to electrodynamic effects cause major broadening of the separated bands. The electrophoresis separation process is simple, however flow local to the sample filament produced by the applied electric field were not considered. These electrohydrodynamic flows distort the sample stream and limit the separation. Also, electroosmosis and viscous flow combine to further distort the process. A moving wall concept is being proposed for space which will eliminate and control the disturbances. The moving wall entrains the fluid to move as a rigid body and produces a constant residence time for all samples distributed across the chamber thickness. The moving wall electrophoresis chamber can only be operated in space because there is no viscous flow in the chamber to stabilize against thermal convection.

Rhodes, Percy H.↗

Experiments on Nucleation in Different Flow Regimes

The vast majority of metallic engineering materials are solidified from the liquid phase. Understanding the solidification process is essential to control microstructure, which in turn, determines the properties of materials. The genesis of solidification is nucleation, where the first stable solid forms from the liquid phase. Nucleation kinetics determine the degree of undercooling and phase selection. As such, it is important to understand nucleation phenomena in order to control solidification or glass formation in metals and alloys. Early experiments in nucleation kinetics were accomplished by droplet dispersion methods. Dilitometry was used by Turnbull and others, and more recently differential thermal analysis and differential scanning calorimetry have been used for kinetic studies. These techniques have enjoyed success; however, there are difficulties with these experiments. Since materials are dispersed in a medium, the character of the emulsion/metal interface affects the nucleation behavior. Statistics are derived from the large number of particles observed in a single experiment, but dispersions have a finite size distribution which adds to the uncertainty of the kinetic determinations. Even though temperature can be controlled quite well before the onset of nucleation, the release of the latent heat of fusion during nucleation of particles complicates the assumption of isothermality during these experiments. Containerless processing has enabled another approach to the study of nucleation kinetics. With levitation techniques it is possible to undercool one sample to nucleation repeatedly in a controlled manner, such that the statistics of the nucleation process can be derived from multiple experiments on a single sample. The authors have fully developed the analysis of nucleation experiments on single samples following the suggestions of Skripov. The advantage of these experiments is that the samples are directly observable. The nucleation temperature can be measured by noncontact optical pyrometry, the mass of the sample is known, and post-processing analysis can be conducted on the sample. The disadvantages are that temperature measurement must have exceptionally high precision, and it is not possible to isolate specific heterogeneous sites as in droplet dispersions. Levitation processing of refractory materials in ultra high vacuum provides an avenue to conduct these kinetic studies on single samples. Two experimental methods have been identified where ultra high vacuum experiments are possible; electrostatic levitation in ground-based experiments and electromagnetic processing in low earth orbit on TEMPUS. Such experiments, reported here, were conducted on zirconium. Liquid zirconium is an excellent solvent and has a high solubility for contaminants contained in the bulk material as well as those contaminants found in the vacuum environment. Oxides, nitrides, and carbides do not exist in the melt, and do not form on the surface of molten zirconium, for the materials and vacuum levels used in this study. Ground-based experiments with electrostatic levitation have shown that the statistical nucleation kinetic experiments are viable and yield results which are consistent with classical nucleation theory. The advantage of low earth orbit experiments is the ability to vary the flow conditions in the liquid prior to nucleation. The put-pose of nucleation experiments in TEMPUS was to examine.

Bayuzick, R. J.↗

A high speed implementation of the random decrement algorithm

The algorithm is useful for measuring net system damping levels in stochastic processes and for the development of equivalent linearized system response models. The algorithm works by summing together all subrecords which occur after predefined threshold level is crossed. The random decrement signature is normally developed by scanning stored data and adding subrecords together. The high speed implementation of the random decrement algorithm exploits the digital character of sampled data and uses fixed record lengths of 2(n) samples to greatly speed up the process. The contributions to the random decrement signature of each data point was calculated only once and in the same sequence as the data were taken. A hardware implementation of the algorithm using random logic is diagrammed and the process is shown to be limited only by the record size and the threshold crossing frequency of the sampled data. With a hardware cycle time of 200 ns and 1024 point signature, a threshold crossing frequency of 5000 Hertz can be processed and a stably averaged signature presented in real time.

Kiraly, L. J.↗

A high-speed implementation of the random decrement algorithm

The algorithm is useful for measuring net system damping levels in stochastic processes and for the development of equivalent linearized system response models. The algorithm works by summing together all subrecords which occur after predefined threshold level is crossed. The random decrement signature is normally developed by scanning stored data and adding subrecords together. The high speed implementation of the random decrement algorithm exploits the digital character of sampled data and uses fixed record lengths of 2(n) samples to greatly speed up the process. The contributions to the random decrement signature of each data point was calculated only once and in the same sequence as the data were taken. A hardware implementation of the algorithm using random logic is diagrammed and the process is shown to be limited only by the record size and the threshold crossing frequency of the sampled data. With a hardware cycle time of 200 ns and 1024 point signature, a threshold crossing frequency of 5000 Hertz can be processed and a stably averaged signature presented in real time.

Kiraly, L. J.↗

Effect of Processing Route on Strain Controlled Low Cycle Fatigue Behavior of Polycrystalline NiAl

The present investigation examines the effects of manufacturing process on the total axial strain controlled low cycle fatigue behavior of polycrystalline NiAl at 1000 K, a temperature above the monotonic Brittle-to-Ductile Transition Temperature (BDTT). The nickel aluminide samples were produced by three different processing routes: hot isostatic pressing of pre- alloyed powders, extrusion of prealloyed powders, and extrusion of vacuum induction melted ingots. The LCF behavior of the cast plus extruded material was also determined at room temperature (below the BD77) for comparison to the high temperature data. The cyclic stress response, cyclic stress-strain behavior, and strain-life relationships were influenced by the alloy preparation technique and the testing temperature. Detailed characterization of the LCF tested samples was conducted by optical and electron microscopy to determine the variations in fracture and deformation modes and to determine any microstructural changes that occurred during LCF testing. The dependence of LCF properties on processing route was rationalized on the basis of starting microstructure, brittle-to-ductile transition temperature, deformation induced changes in the basic microstructure, deformation substructure, and synergistic interaction between the damage modes.

Rao, K. Bhanu Sankara↗

Space processing of composite materials

Materials and processes for the testing of aluminum-base fiber and particle composites, and of metal foams under extended-time low-g conditions were investigated. A wetting and dispersion technique was developed, based on the theory that under the absence of a gas phase all solids are wetted by liquids. The process is characterized by a high vacuum environment and a high temperature cycle. Successful wetting and dispersion experiments were carried out with sapphire fibers, whiskers and particles, and with fibers of silicon carbide, pyrolytic graphite and tungsten. The developed process and facilities permit the preparation of a precomposite which serves as sample material for flight experiments. Low-g processing consists then merely in the uniform redistribution of the reinforcements during a melting cycle. For the preparation of metal foams, gas generation by means of a thermally decomposing compound was found most adaptable to flight experiments. For flight experiments, the use of compacted mixture of the component materials limits low-g processing to a simple melt cycle.

Steurer, W. H.↗

Coplanar back contacts for thin silicon solar cells

A process for fabricating 2 to 3 mil wraparound solar cells was formulated. Sample thin wraparound cells were fabricated using this process. The process used a reinforced perimeter construction to reduce the breakage that occurs during handling of the wafers. A retracting piston post was designed and fabricated to help minimize the breakage that occurs during the screen printing process. Two alternative methods of applying the aluminum back surface field were investigated. In addition to the standard screen printed back surface field, both spin-on and evaporated aluminum techniques were researched. Neither spin-on nor evaporated aluminum made any noticeable improvement over the screen printing technique. A fine screen mesh was chosen for the application of the aluminum paste back surface field. The optimum time and temperature for firing the aluminum turned out to be thirty seconds at 850 C. The development work on the dielectric included looking at three dielectrics for the wraparound application. Transene 1000, Thick Film Systems 1126RCB and an in house formulation 61-2-2A were all tested. Cells with pre-dielectric thickness of 3.0-0-3.5 mils using Transene 1000 as the wraparound dielectric and the procedure outlined above showed an average efficiency of 10.7 percent. Thinner cells were fabricated, but had an unacceptable yield and efficiency.

Thornhill, J. W.↗

Electron Spin Resonance (ESR) studies of returned comet nucleus samples

The most important objective of the Comet Nucleus Sample Returm Mission is to return samples which could reflect formation conditions and evolutionary processes in the early solar nebula. It is expected that the returned samples will consist of fine-grained silicate materials mixed with ices composed of simple molecules such as H2O, NH3, CH4 as well as organics and/or more complex compounds. Because of the exposure to ionizing radiation from cosmic-ray, gamma-ray, and solar wind protons at low temperature, free radicals are expected to be formed and trapped in the solid ice matrices. The kind of trapped radical species together with their concentration and thermal stability can be used as a dosimeter as well as a geothermometer to determine thermal and radiation histories as well as outgassing and other possible alternation effects since the nucleus material was formed. Since free radicals that are known to contain unpaired electrons are all paramagnetic in nature, they can be readily detected and characterized in their native form by the Electron Spin Resonance (ESR) method. In fact, ESR has been shown to be a non-destructive, highly sensitive tool for the detection and characterization of paramagnetic, ferromagnetic, and radiation damage centers in terrestrial and extraterrestrial geological samples. The potential use of ESR as an effective method in the study of returned comet nucleus samples, in particular, in the analysis of fine-grained solid state icy samples is discussed.

Tsay, Fun-Dow↗

Solidification of eutectic system alloys in space (M-19)

It is well known that in the liquid state eutectic alloys are theoretically homogeneous under 1 g conditions. However, the homogeneous solidified structure of this alloy is not obtained because thermal convection and non-equilibrium solidification occur. The present investigators have clarified the solidification mechanisms of the eutectic system alloys under 1 g conditions by using the in situ observation method; in particular, the primary crystals of the eutectic system alloys never nucleated in the liquid, but instead did so on the mold wall, and the crystals separated from the mold wall by fluid motion caused by thermal convection. They also found that the equiaxed eutectic grains (eutectic cells) are formed on the primary crystals. In this case, the leading phase of the eutectic must agree with the phase of the primary crystals. In space, no thermal convection occurs so that primary crystals should not move from the mold wall and should not appear inside the solidified structure. Therefore no equiaxed eutectic grains will be formed under microgravity conditions. Past space experiments concerning eutectic alloys were classified into two types of experiments: one with respect to the solidification mechanisms of the eutectic alloys and the other to the unidirectional solidification of this alloy. The former type of experiment has the problem that the solidified structures between microgravity and 1 g conditions show little difference. This is why the flight samples were prepared by the ordinary cast techniques on Earth. Therefore it is impossible to ascertain whether or not the nucleation and growth of primary crystals in the melt occur and if primary crystals influence the formation of the equiaxed eutectic grains. In this experiment, hypo- and hyper-eutectic aluminum copper alloys which are near eutectic point are used. The chemical compositions of the samples are Al-32.4mass%Cu (Hypo-eutectic) and Al-33.5mass%Cu (hyper-eutectic). Long rods for the samples are cast by the Ohno Continuous Casting Process and they show the unidirectionally solidified structure. Each flight and ground sample was made of these same rods. The dimensions of all samples are 4.5 mm in diameter and 23.5 mm in length. Each sample is put in a graphite capsule and then vacuum sealed in a double silica ampoule. Then the ampoule is put in the tantalum cartridge and sealed by electron beam welding. For onbard experiments, a Continuous Heating Furnance (CHF) will be used for melting and solidifying samples under microgravity conditions. Six flight samples will be used. Four samples are hypo-eutectic and two are hyper-eutectic alloys. The surface of the two hypo-eutectic alloy samples are covered with aluminum oxide film to prevent Marangoni convection expected under microgravity conditions. Each sample will be heated to 700 C and held at that temperature for 5 min. After that the samples will be allowed to cool to 500 C in the furnace and they will be taken out of the furnace for He gas cooling. The heating and cooling diagrams for the flight experiments are shown. After collecting the flight samples, the solidified structures of the samples will be examined and the mechanisms of eutectic solidification under microgravity conditions will be determined. It is likely that successful flight experiment results will lead to production of high quality eutectic alloys and eutectic composite materials in space.

Ohno, Atsumi↗

Realistic Covariance Generation for the GPM Spacecraft

We present several different methods for generating realistic predictive covariance, including Monte-Carlo simulations and more direct linear methods which require the addition of process noise. The Monte-Carlo simulation starts with an epoch uncertainty sample basis and propagates each trial to a time of interest in the future. The variance-covariance of the state elements as well as other higher order sample statistics can be readily computed from the propagated sample. While this method preserves the nonlinear effects on the propagated uncertainty, it is computationally intensive as a statistically significant sample size must be considered in the propagation process. Moreover, if the epoch covariance is optimistic, this can result in an underestimation of the prediction error. Another method is to propagate a state sensitivity matrix simultaneously with the satellite state, which allows the epoch covariances to be propagated forward in a linear fashion. This method does not preserve the non-linearity of the satellite state uncertainty but is much less computationally intensive. The propagated state covariance is the scaled to represent the realistic level of GPM state uncertainty via a "e-tuning process." The tuning process generates an inflation factor based on the observed error statistics of the predictive satellite trajectories when compared to the definitive ones. Difference tuning strategies are considered and compared via Goodness-of-Fit method testing for the Gaussian properties of the scaled covariance.

prediction error↗

Space ultra-vacuum facility and method of operation

A wake shield facility providing an ultrahigh vacuum level for space processing is described. The facility is in the shape of a truncated, hollow hemispherical section, one side of the shield convex and the other concave. The shield surface is preferably made of material that has low out-gassing characteristics such as stainless steel. A material sample supporting fixture in the form of a carousel is disposed on the convex side of the shield at its apex. Movable arms, also on the convex side, are connected by the shield in proximity to the carousel, the arms supporting processing fixtures, and providing for movement of the fixtures to predetermined locations required for producing interations with material samples. For MBE processes a vapor jet projects a stream of vaporized material onto a sample surface. The fixtures are oriented to face the surface of the sample being processed when in their extended position, and when not in use they are retractable to a storage position. The concave side of the shield has a support structure including metal struts connected to the shield, extending radially inward. The struts are joined to an end plate disposed parallel to the outer edge of the shield. This system eliminates outgassing contamination.

Naumann, Robert J.↗

NASA Bioculture System: From Experiment Definition to Flight Payload

Starting in 2015, the NASA Bioculture System will be available to the science community to conduct cell biology and microbiology experiments on ISS. The Bioculture System carries ten environmentally independent Cassettes, which house the experiments. The closed loop fluids flow path subsystem in each Cassette provides a perfusion-based method for maintain specimen cultures in a shear-free environment by using a biochamber based on porous hollow fiber bioreactor technology. Each Cassette contains an incubator and separate insulated refrigerator compartment for storage of media, samples, nutrients and additives. The hardware is capable of fully automated or manual specimen culturing and processing, including in-flight experiment initiation, sampling and fixation, up to BSL-2 specimen culturing, and the ability to up to 10 independent cultures in parallel for statistical analysis. The incubation and culturing of specimens in the Bioculture System is a departure from standard laboratory culturing methods. Therefore, it is critical that the PI has an understanding the pre-flight test required for successfully using the Bioculture System to conduct an on-orbit experiment. Overall, the PI will conduct a series of ground tests to define flight experiment and on-orbit implementation requirements, verify biocompatibility, and determine base bioreactor conditions. The ground test processes for the utilization of the Bioculture System, from experiment selection to flight, will be reviewed. Also, pre-flight test schedules and use of COTS ground test equipment (CellMax and FiberCell systems) and the Bioculture System will be discussed.

Bioculture System↗

Experiments on Nucleation in Different Flow Regimes

The vast majority of metallic engineering materials are solidified from the liquid phase. Understanding the solidification process is essential to control microstructure, which in turn, determines the properties of materials. The genesis of solidification is nucleation, where the first stable solid forms from the liquid phase. Nucleation kinetics determine the degree of undercooling and phase selection. As such, it is important to understand nucleation phenomena in order to control solidification or glass formation in metals and alloys. Early experiments in nucleation kinetics were accomplished by droplet dispersion methods. Dilatometry was used by Turnbull and others, and more recently differential thermal analysis and differential scanning calorimetry have been used for kinetic studies. These techniques have enjoyed success; however, there are difficulties with these experiments. Since materials are dispersed in a medium, the character of the emulsion/metal interface affects the nucleation behavior. Statistics are derived from the large number of particles observed in a single experiment, but dispersions have a finite size distribution which adds to the uncertainty of the kinetic determinations. Even though temperature can be controlled quite well before the onset of nucleation, the release of the latent heat of fusion during nucleation of particles complicates the assumption of isothermality during these experiments. Containerless processing has enabled another approach to the study of nucleation kinetics. With levitation techniques it is possible to undercool one sample to nucleation repeatedly in a controlled manner, such that the statistics of the nucleation process can be derived from multiple experiments on a single sample. The authors have fully developed the analysis of nucleation experiments on single samples following the suggestions of Skripov. The advantage of these experiments is that the samples are directly observable. The nucleation temperature can be measured by noncontact optical pyrometry, the mass of the sample is known, and post processing analysis can be conducted on the sample. The disadvantages are that temperature measurement must have exceptionally high precision, and it is not possible to isolate specific heterogeneous sites as in droplet dispersions.

Bayuzick, R. J.↗