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Recent Advances in Soft Matter Characterization Capabilities Developed at NASA GRC for Lunar Exploration: Differential Dynamic Microscopy to Spectroscopy to Computer Vision

In 1991, famous French scientist Pierre-Gilles de Genes was awarded Nobel prize for his impactful research in soft matter, more specifically polymers. He is defined as the founding father of soft matter. In his Nobel lecture (https://www.nobelprize.org/uploads/2018/06/gennes-lecture.pdf ) he described soft matter aka complex fluids as materials with two primary features – (a) complexity and (b) flexibility. The sub-categories of soft matter (e.g.- granular materials, polymers, foams, colloids etc.) are defined on the basis of Pierre-Gilles de Gennes’ definition. At NASA GRC, we are pushing the boundaries for fundamental study of soft matter on Lunar Surface. With regard to Lunar surface science, we are focusing on developing capabilities pertaining to granular materials and bio-soft/active matter to facilitate future efforts in ISRU and bio-ISRU capabilities. In order to achieve fundamental goals of soft matter research within the limitations of Lunar environment, the scientific capabilities need to be small, flexible, modular, off the shelf and the focus needs to be more on developing an interdisciplinary capability that leverages the recent growth in AI/ML and Computer Vision to augment our understanding of fundamental science. This strategy would allow us to reduce our resource requirement during launch, installation, and occupied real estate footprint on Lunar surface In this talk, we will go over 3 different capabilities that we have developed in house and in close collaboration – (a) Differential Dynamic Microscopy (DDM), (b) Portable In-situ Chemical Spectroscopy (PICS) and (c) Computer Vision Enabled Observation. At very high level, Differential Dynamic Microscopy (DDM) allows us to study the structure-property-process relation (microrheology) of bio-soft/active matter using optical microscope and improved image analysis capabilities. PICS uses AI/ML-based advanced signal deconvolution and analysis technique that can work with existing portable spectroscopy tools to perform materials analysis (e.g.- granular materials and bio-soft/active matter) inspection on the go. Finally, computer vision enabled analysis allows us to use simple camera images for 3D reconstruction of experimental process and tracking of objects of interest in an experiment. We expect that this detailed process will allow us reach a thorough understanding of soft matter in Lunar environment. The capabilities developed by us will help to validate and establish fundamental understanding in Lunar environment. This will, in turn, allow us to guide future space exploration missions and expand the knowledge base of the scientific and engineering communities.

Suman Sinha Ray↗

Recent Advances in Soft Matter Characterization Capabilities Developed at NASA GRC

In 1991, famous French scientist Pierre-Gilles de Genes was awarded Nobel prize for his impactful research in soft matter, more specifically polymers. He is defined as the founding father of soft matter. In his Nobel lecture (https://www.nobelprize.org/uploads/2018/06/gennes-lecture.pdf ) he described soft matter aka complex fluids as materials with two primary features – (a) complexity and (b) flexibility. The sub-categories of soft matter (e.g.- granular materials, polymers, foams, colloids etc.) are defined on the basis of Pierre-Gilles de Gennes’ definition. At NASA GRC, we are pushing the boundaries for fundamental study of soft matter on Lunar Surface. With regard to Lunar surface science, we are focusing on developing capabilities pertaining to granular materials and bio-soft/active matter to facilitate future efforts in ISRU and bio-ISRU capabilities. In order to achieve fundamental goals of soft matter research within the limitations of Lunar environment, the scientific capabilities need to be small, flexible, modular, off the shelf and the focus needs to be more on developing an interdisciplinary capability that leverages the recent growth in AI/ML and Computer Vision to augment our understanding of fundamental science. This strategy would allow us to reduce our resource requirement during launch, installation, and occupied real estate footprint on Lunar surface In this talk, we will go over 3 different capabilities that we have developed in house and in close collaboration – (a) Differential Dynamic Microscopy (DDM), (b) Portable In-situ Chemical Spectroscopy (PICS) and (c) Computer Vision Enabled Observation. At very high level, Differential Dynamic Microscopy (DDM) allows us to study the structure-property-process relation (microrheology) of bio-soft/active matter using optical microscope and improved image analysis capabilities. PICS uses AI/ML-based advanced signal deconvolution and analysis technique that can work with existing portable spectroscopy tools to perform materials analysis (e.g.- granular materials and bio-soft/active matter) inspection on the go. Finally, computer vision enabled analysis allows us to use simple camera images for 3D reconstruction of experimental process and tracking of objects of interest in an experiment. We expect that this detailed process will allow us reach a thorough understanding of soft matter in Lunar environment. The capabilities developed by us will help to validate and establish fundamental understanding in Lunar environment. This will, in turn, allow us to guide future space exploration missions and expand the knowledge base of the scientific and engineering communities.

Suman Sinha Ray↗

Rheology of Lunar Regolith Simulant Under Varying Gravitational Conditions

Understanding structure-property-process relationship aka rheology of regolith in varying gravity conditions is critical for exploration and future missions. In this work, a framework for studying rheology of lunar regolith simulant in varying gravity conditions (Terrestrial, Lunar and Martian) is described theoretically/numerically, where the driving force of flow of simulants was gravitational acceleration. In the analysis particle-particle interaction forces were included. It was found that the dynamic behavior of granular material is extremely sensitive to external conditions by virtue of the myriad of forces present between particle grains. The results obtained were validated against results obtained in earth and Lunar gravity conditions. The theoretical/numerical and experimental results showed that the complex interaction of these forces can drastically change the dynamics of the material, which is not captured by standard design rules, generally used in industry, for variable gravity applications.

Simulation↗

Co(x)Ni(4-x)Sb(12-y)Sn(y) Ternary Skutterudites: Processing and Thermoelectric Properties

Skutterudites have proven to be a useful thermoelectric system as a result of their high figure of merit, favorable mechanical properties, and good thermal stability. Binary skutterudites have received the majority of interest in recent years, as a result of successful double and triple filling schemes. Ternary skutterudites, such as Ni4Sb7Sn5, also demonstrate good thermoelectric performance, with high power factor and low thermal conductivity. Ternary skutterudites, as contrasted to binary systems, provide more possibility for tuning electronic structure as substitutions can be studied on three elements. The Co(x)Ni(4-x)Sb(12-y)Sn(y) system has been investigated as both a p- and n-type thermoelectric material, stable up to 200 C. The system is processed through a combination of solidification, mechanical alloying, and hot pressing steps. Rietveld structure refinement has revealed an interesting occupancy of Sn on both the 24g Wyckoff position with Sb as well as the 2a position as a rattler. In addition to thermoelectric properties, detailed processing routes have been investigated on the system.

Seebeck effect↗

Filled Co (sub X) Ni (sub 4-x) Sb (sub 12-y) Sn (sub Y) Skutterudites: Processing and Thermoelectric Properties

Skutterudites have proven to be a useful thermoelectric system as a result of their enhanced figure of merit (ZT1), cheap material cost, favorable mechanical properties, and good thermal stability. The majority of skutterudite interest in recent years has been focused on binary skutterudites like CoSb3 or CoAs3. Binary skutterudites are often double and triple filled, with a range of elements from the lanthanide series, in order to reduce the lattice component of thermal conductivity. Ternary and quaternary skutterudites, such as Co4Ge6Se6 or Ni4Sb8Sn4, provide additional paths to tune the electronic structure. The thermal conductivity can further be improved in these complex skutterudites by the introduction of fillers. The Co (sub X) Ni (sub 4-x) Sb (sub 12-y) Sn (sub Y) system has been investigated as both a p- and n-type thermoelectric material, and is stable up to 200 degrees Centigrade. Yb, Ce, and Dy fillers have been introduced into the skutterudite to study the influence of both the type and the quantity of fillers on processing conditions and thermoelectric properties. The system was processed through a multi-step technique that includes solidification, mechano-chemical alloying, and hot pressing which will be discussed along with thermoelectric transport properties.

Thermoelectricity↗

Investigation of Thermal Processing on the Properties of PS304: A Solid Lubricant Coating

The effect of thermal processing on PS304, a solid lubricant coating, was investigated. PS304 is a plasma sprayed solid lubricant consisting of 10% Ag and 10% BaF2 and CaF2 in a eutectic mixture for low and high temperature lubricity respectively. In addition, PS304 contains 20% Cr2O3 for increased hardness and 60% NiCr which acts as a binder. All percents are in terms of weight not volume. Previous research on thermal processing (NAG3-2245) of PS304 revealed that substrate affected both the pre- and post-anneal hardness of the plasma spray coating. The objective of this grant was to both quantify this effect and determine whether the root cause was an artifact of the substrate or an actual difference in hardness due to interaction between the substrate and the coating. In addition to clarifying past research developments new data was sought in terms of coating growth due to annealing.

Benoy, Patricia A.↗

Celion/Larc-160 graphite/polyimide composite processing techniques and properties

Weight savings in the range from 25 to 35 percent could be achieved on Space Shuttle orbiter components and the thermal protection system (TPS) by employing a suitable graphite/polyimide (Gr/Pi) composite material system as a substitute for the baseline aluminum structural material. Predicted weight savings are based on the superior strength and stiffness-to-density ratios of Gr/Pi composite material over metallic counterparts. Specific strength and stiffness properties of Celion/Larc-160 composite laminates are compared with aluminum and titanium alloys. Aspects of materials and processes development are discussed, taking into account Celion/Larc-160 composite cure cycle and tooling evolution, complex shaped component process development, mechanical and physical properties testing and results, and structural element design fabrication, testing, and results. Attention is given to a demonstration of materials and processing technology, and a Celion/Larc-160 materials and processes summary is presented.

Jones, J. S.↗

Containerless high temperature property measurements

Containerless processing in the low gravity environment of space provides the opportunity to increase the temperature at which well controlled processing of and property measurements on materials is possible. This project was directed towards advancing containerless processing and property measurement techniques for application to materials research at high temperatures in space. Containerless high temperature material property studies include measurements of the vapor pressure, melting temperature, optical properties, and spectral emissivities of solid boron. The reaction of boron with nitrogen was also studied by laser polarimetric measurement of boron nitride film growth. The optical properties and spectral emissivities were measured for solid and liquid silicon, niobium, and zirconium; liquid aluminum and titanium; and liquid Ti-Al alloys of 5 to 60 atomic pct. titanium. Alternative means for noncontact temperature measurement in the absence of material emissivity data were evaluated. Also, the application of laser induced fluorescence for component activity measurements in electromagnetic levitated liquids was studied, along with the feasibility of a hybrid aerodynamic electromagnetic levitation technique.

Nordine, Paul C.↗

Game-Theoretic Modeling of Vegetation Composition, Structure, and Dynamics: Physical Constraints, Fundamental Processes, and Emergent Properties

Vegetation structural and compositional dynamics emerge from plant physiological and demographic processes, individual-based competition, vegetation-soil feedbacks, and environmental variations and disturbance events. Predicting long-term changes in vegetation requires scaling plant individual behavior to large scale ecosystem processes. In this presentation, we summarize our studies in the modeling of vegetation demographic processes, competitively dominant plant traits, plant hydraulic processes, and stochastic disturbance effects on ecosystems, and illustrate the roles of the underlying ecological processes and eco-evolutionary optimization in vegetation modeling. With the case studies of evolutionarily stable strategy of allocation, leaf traits, and plant hydraulic processes, we show how the ecosystem processes and vegetation dynamics are determined by the individual-based plant competition and variations of soil and climate conditions. The predictions of ecosystem carbon dynamics can be greatly different with those from the traditional “single-tree” models. We also discuss the tradeoffs of plant traits and evolutionarily optimal strategies in the modeling of terrestrial ecosystem dynamics in an Earth system model.

vegetation models↗

Sample fields of the Viking landers, physical properties, and aeolian processes

Surface sampler activities on Mars during the Viking extended mission are considered, including excavation of deep trenches, construction of conical piles of materials, backhoe touchdown experiments, and acquisition of contiguous pictures of the surface beneath number 2 terminal descent engines using mirrors. Results of the Physical Properties Investigation that are relevant to aeolian processes are also discussed. Both pictures and surface sampler data indicate that the surface materials in the sample fields of the Viking landers may be grouped, in order of increasing strength, into drift material, crusty to cloddy material, blocky material and rocks.

Moore, H. J.↗

Processing and Mechanical Properties of NiAl-Based In-Situ Composites

In-situ composites based on the NiAl-Cr eutectic system were successfully produced by containerless processing and evaluated. The NiAl-Cr alloys had a fibrous microstructure while the NiAl-(Cr,Mo) alloys containing 1 at. percent or more molybdenum exhibited a lamellar structure. The NiAl-28Cr-6Mo eutectic displays promising high temperature strength while still maintaining a reasonable room temperature fracture toughness when compared to other NiAl-based materials. The Laves phase NiAlTa was used to strengthen NiAl and very promising creep strengths were found for the directionally solidified NiAl-NiAlTa eutectic. The eutectic composition was found to be near NiAl-15.5Ta (at. percent) and well aligned microstructures were produced at this composition. An off-eutectic composition of NiAl-14.5Ta was also processed, consisting of NiAl dendrites surrounded by aligned eutectic regions. The room temperature toughness of these two phase alloys was similar to that of polycrystalline NiAl even with the presence of the brittle Laves phase NiAlTa. Polyphase in-situ composites were generated by directional solidification of ternary eutectics. The systems investigated were the Ni-Al-Ta-X (X=Cr, Mo, or V) alloys. Ternary eutectics were found in each of these systems and both the eutectic composition and temperature were determined. Of these ternary eutectics, the one in the NiAl-Ta-Cr system was found to be the most promising. The fracture toughness of the NiAl-(Cr,Al)NiTa-Cr eutectic was intermediate between those of the NiAl-NiAlTa eutectic and the NiAl-Cr eutectic. The creep strength of this ternary eutectic was similar to or greater than that of the NiAl-Cr eutectic.

Johnson, David Ray↗

WSi2 in Si(1-x)Ge(x) Composites: Processing and Thermoelectric Properties

Traditional SiGe thermoelectrics have potential for enhanced figure of merit (ZT) via nano-structuring with a silicide phase, such as WSi2. A second phase of nano-sized silicides can theoretically reduce the lattice component of thermal conductivity without significantly reducing the electrical conductivity. However, experimentally achieving such improvements in line with the theory is complicated by factors such as control of silicide size during sintering, dopant segregation, matrix homogeneity, and sintering kinetics. Samples were prepared using powder metallurgy techniques; including mechano-chemical alloying, via ball milling, and spark plasma sintering for densification. Processing, micro-structural development, and thermoelectric properties will be discussed. Additionally, couple and device level characterization will be introduced.

Thermoelectric Power Generation↗

Polysiloxanes derived from the controlled hydrolysis of tetraethoxysilane as precursors to silica for use in ceramic processing

Synthesis, properties, and potential applications in ceramic processing for two polysiloxane silica precursors derived from the controlled hydrolysis of tetraethoxysilane (TEOS) are presented. The higher molecular weight TEOS-A is a thick adhesive liquid of viscosity 8000 to 12,000 c.p. having a SiO2 char yield of about 55 percent. The lower molecular weight TEOS-B is a more fluid liquid of viscosity 150 to 200 c.p. having a SiO2 char yield of about 52 percent. The acid catalyzed hydrolysis of TEOS to hydrated silica gel goes through a series of polysiloxane intermediates. The rate of this transition increases with the quantity of water added to the TEOS; thus, for ease of polymer isolation, the amount of water added must be carefully determined so as to produce the desired polymer in a reasonable time. The water to TEOS mole ratio falls in the narrow range of 1.05 for TEOS-A and 0.99 for TEOS-B. Further polymerization or gelation is prevented by storing at -5 C in a freezer. Both polysiloxanes thermoset to a glassy solid at 115 C. The liquid polymers are organic in nature in that they are miscible with toluene and ethanol, slightly souble in heptane, but immiscible with water. For both polymers, results on viscosity versus time are given at several temperatures and water additions. Based on these results, some examples of practical utilization of the precursors for ceramic fabrication are given.

Philipp, Warren H.↗

Effect of thermal processing practices on the properties of superplastic Al-Li alloys

The effect of thermal processing on the mechanical properties of superplastically formed structural components fabricated from three aluminum-lithium alloys was evaluated. The starting materials consisted of 8090, 2090, and X2095 (Weldalite(TM) 049), in the form of commercial-grade superplastic sheet. The experimental test matrix was designed to assess the impact on mechanical properties of eliminating solution heat treatment and/or cold water quenching from post-forming thermal processing. The extensive hardness and tensile property data compiled are presented as a function of aging temperature, superplastic strain and temper/quench rate for each alloy. The tensile properties of the materials following superplastic forming in two T5-type tempers are compared with the baseline T6 temper. The implications for simplifying thermal processing without degradation in properties are discussed on the basis of the results.

Hales, Stephen J.↗

Irradiating of Bulk Soybeans: Influence on Their Functional and Sensory Properties for Soyfood Processing

Soybeans were chosen for lunar and planetary missions, where soybeans will be supplied in bulk or grown locally, due to their nutritive value and ability to produce oil and protein for further food applications. However, soybeans must be processed into foods prior to consumption. Radiation that soybeans would be exposed to during bulk storage prior to and during a Mars mission may influence their germination and functional properties. The influence of radiation includes the affect of surface pasteurization to ensure the astronauts safety from food-borne illnesses (HACCP, CCP), and the affect of the amount of radiation the soybeans receive during a Mars mission. Decreases in the amount of natural antioxidants free radical formation, and oxidation-induced changes in the soybean will influence the nutritional value, texture, color, and aroma of soyfoods. The objective of this study was to determine the influence of pasteurization and sterilization surface radiation on whole soybeans using gamma and electron beam radiation. The influence of 0, 1, 5, 10, and 30kGy on microbial load, germination rate, ease of processing, and quality of soymilk and tofu were determined. Surface radiation of whole dry soybeans using electron beam or gamma rays from 1-30kGy did provide microbial safety for the astronauts. However, the lower dose levels had surviving yeasts and molds. These doses caused oxidative changes that resulted in soymilk and tofu with rancid aromas. GC-MS of the aroma compounds using SPME Headspace confirmed the presence of lipid oxidation compounds. Soybean germination ability was reduced as radiation dosage increased. While lower doses may reduce these problems, the ability to insure microbial safety of bulk soybeans will be lost. Counter measures could include vacuum packaging, nitrogen flushing, added antioxidants, and radiating under freezing conditions. Doses below 1kGy need to be investigated further to determine the influence of the radiation encountered during Mars missions.

Chia, Chiew-Ling↗

Preparation Process and Dielectric Properties of Ba(0.5)Sr(0.5)TiO3-P(VDF-CTFE) Nanocomposites

Ceramic-polymer 0-3 nanocomposites, in which nanosized Ba(0.5)Sr(0.5)TiO3 (BST) powders were used as ceramic filler and P(VDF-CTFE) 88/12 mol% [poly(vinylidene fluoridechlorotrifluoroethylene)] copolymer was used as matrix, were studied over a concentration range from 0 to 50 vol.% of BST powders. It is found that the solution cast composites are porous and a hot-press process can eliminate the porosity, which results in a dense composite film. Two different configurations used in the hot-press process are studied. Although there is no clear difference in the uniformity and microstructure of the composites prepared using these two configurations, the composite prepared using one configuration exhibit a higher dielectric constant with a lower loss. For the composite with 40 vol. BST, a dielectric constant of 70 with a loss of 0.07 at 1 kHz is obtained at room temperature. The composites exhibit a lower dielectric loss than the polymer matrix at high frequency. However, at low frequency, the composites exhibit a higher loss than the polymer matrix due to a low frequency relaxation process that appears in the composites. It is believed that this relaxation process is related to the interfacial layer formed between BST particle and the polymer matrix. The temperature dependence of the dielectric property of the composites was studied. It is found that the dielectric constant of these composites is almost independent of the temperature over a temperature range from 20 to 120 C. Key words: A. Polymer-matrix composites (PMCs); B. Electrical Properties; E. Casting; E. Heat treatment; Dielectric properties.

Zhang, Lin↗

Laboratory Studies of the Optical Properties and Condensation Processes of Cosmic Dust Grains

A laboratory facility for conducting a variety of experiments on single isolated dust particles of astrophysical interest levitated in an electrodynamics balance has been developed at NASA/Marshall Space Flight Center. The objective of the research is to employ this experimental technique for studies of the physical and optical properties of individual cosmic dust grains of 0.1-100 micron size in controlled pressure/temperatures environments simulating astrophysical conditions. The physical and optical properties of the analogs of interstellar and interplanetary dust grains of known composition and size distribution will be investigated by this facility. In particular, we will carry out three classes of experiments to study the micro-physics of cosmic dust grains. (1) Charge characteristics of micron size single dust grains to determine the photoelectric efficiencies, yields, and equilibrium potentials when exposed to UV radiation. (2) Infrared optical properties of dust particles (extinction coefficients and scattering phase functions) in the 1-30 micron region using infrared diode lasers and measuring the scattered radiation. (3) Condensation experiments to investigate the condensation of volatile gases on colder nucleated particles in dense interstellar clouds and lower planetary atmospheres. The condensation experiments will involve levitated nucleus dust grains of known composition and initial mass (or m/q ratio), cooled to a temperature and pressure (or scaled pressure) simulating the astrophysical conditions, and injection of a volatile gas at a higher temperature from a controlled port. The increase in the mass due to condensation on the particle will be monitored as a function of the dust particle temperature and the partial pressure of the injected volatile gas. The measured data will permit determination of the sticking coefficients of volatile gases and growth rates of dust particles of astrophysical interest. Some preliminary results based on measurements of photoelectric emission and radiation pressure on single isolated 0.2 to 6.6 micron size silica particles exposed to UV radiation at 120-200 nm and green laser light at 532 nm are presented.

Abbas, M. M.↗

Laboratory Studies of the Optical Properties and Condensation Processes of Cosmic Dust Particles

A laboratory facility for levitating single isolated dust particles in an electrodynamics balance has been developing at NASA/Marshall Space Flight Center for conducting a variety of experimental, of astrophysical interest. The objective of this research is to employ this innovative experimental technique for studies of the physical and optical properties of the analogs of cosmic grains of 0.2-10 micron size in a chamber with controlled pressure/temperatures simulating astrophysical environments. In particular, we will carry out three classes of experiments to investigate the microphysics of the analogs of interstellar and interplanetary dust grains. (1) Charge characteristics of micron size single dust grains to determine the photoelectric efficiencies, yields, and equilibrium potentials when exposed to UV radiation. These measurements will provide the much-needed photoelectric emission data relating to individual particles as opposed to that for the bulk materials available so far. (2) Infrared optical properties of dust particles obtained by irradiating the particles with radiation from tunable infrared diode lasers and measuring the scattered radiation. Specifically, the complex refractive indices, the extinction coefficients, the scattering phase functions, and the polarization properties of single dust grains of interest in interstellar environments, in the 1-25 micron spectral region will be determined. (3) Condensation experiments to investigate the deposition of volatile gases on colder nucleated particles in dense interstellar clouds and lower planetary atmospheres. The increase in the mass or m/q ratio due to condensation on the particle will be monitored as a function of the dust particle temperature and the partial pressure of the injected volatile gas. The measured data wild permit determination of the sticking efficiencies of volatile gases of astrophysical interest. Preliminary results based on photoelectric emission experiments on 0.2-6.6 micron size silica particles exposed to UV radiation in the 120-200 nm spectral region will be presented.

Abbas, Mian M.↗