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NASA NTRS1997

Ceramic Aerogel Composite Materials and Characterization

Aerogels a.k.a "Solid Smoke" are gels with the liquid phase replaced by gas, leaving behind a highly porous material with a nanoscale framework. Due to the porous, nanoscale structure, aerogels have the lowest known density and conductivity of solids. Aerogels have the potential for being a breakthrough material because of their extremely light weight and unique properties. In this paper, we address overcoming their most profound weaknesses: mechanical fragility and very high surface activity, which leads to a lowered sintering temperature. A matrix of ceramic aerogel composite materials was produced to investigate their properties and functionality. Mechanical property measurements and Scanning Electron Micrographs are used to identify trends and structure of these ceramic composite materials. Thermal cycling was used to identify the sintering points of the materials.

White, Susan↗

NASA NTRSDate not supplied

Risk Reduction Testing of Superconducting Coils for the High Efficiency Megawatt Motor

Second generation high temperature superconducting coils provide a very attractive level of performance for use in the field winding of electric machines for aircraft. Aside from maintaining these coils at cryogenic temperatures, much care must be taken to prevent damaging these relatively fragile materials due to excessive stress. Thermal stresses due to temperature cycling and mechanical stresses due to centrifugal forces are the most critical for the High Efficiency Megawatt Motor. This paper summarizes two test campaigns that were undertaken to reduce the risks posed by these loads. In one campaign, several superconducting coils were fabricated, thermally cycled up to 50~times, and electrically tested in liquid nitrogen to assess the change in superconductivity metrics throughout thermal cycling. In the other campaign, a full-scale superconducting coil was fabricated, a test article was designed to produce a representative stress environment in the coil, the test article and coil were rotated at room temperature up to a speed of 11,800~rpm, and the superconductivity metrics were measured in liquid nitrogen before and after each rotation. The experimental results demonstrate that the superconducting coils manufactured in house can survive both thermal cycling and high speed rotation with no appreciable degradation in superconducting performance.

partially superconducting electric machine↗

NASA NTRS1996

Crystallization of amorphous water ice in the solar system

Electron diffraction studies of vapor-deposited water ice have characterized the dynamical structural changes during crystallization that affect volatile retention in cometary materials. Crystallization is found to occur by nucleation of small domains, while leaving a significant part of the amorphous material in a slightly more relaxed amorphous state that coexists metastably with cubic crystalline ice. The onset of the amorphous relaxation is prior to crystallization and coincides with the glass transition. Above the glass transition temperature, the crystallization kinetics are consistent with the amorphous solid becoming a "strong" viscous liquid. The amorphous component can effectively retain volatiles during crystallization if the volatile concentration is approximately 10% or less. For higher initial impurity concentrations, a significant amount of impurities is released during crystallization, probably because the impurities are trapped on the surfaces of micropores. A model for crystallization over long timescales is described that can be applied to a wide range of impure water ices under typical astrophysical conditions if the fragility factor D, which describes the viscosity behavior, can be estimated.

NASA Center ARC↗

NASA NTRS2001

A Survey of Alternative Oxygen Production Technologies

Utilization of the Martian atmosphere for the production of fuel and oxygen has been extensively studied. The baseline fuel production process is a Sabatier reactor, which produces methane and water from carbon dioxide and hydrogen. The oxygen produced from the electrolysis of the water is only half of that needed for methane-based rocket propellant, and additional oxygen is needed for breathing air, fuel cells and other energy sources. Zirconia electrolysis cells for the direct reduction of CO2 arc being developed as an alternative means of producing oxygen, but present many challenges for a large-scale oxygen production system. The very high operating temperatures and fragile nature of the cells coupled with fairly high operating voltages leave room for improvement. This paper will survey alternative oxygen production technologies, present data on operating characteristics, materials of construction, and some preliminary laboratory results on attempts to implement each. Our goal is to significantly improve upon the characteristics of proposed zirconia cells for oxygen production. To achieve that goal we are looking at electrolytic systems that operate at significantly lower temperatures, preferably below 31C to allow the incorporation of liquid CO2 in the electrolyte. Our preliminary results indicate that such a system will have much higher current densities and have simpler cathode construction than a porous gas feed electrode system. Such a system could be achieved based on nonaqueous electrolytes or ionic liquids. We are focusing our research on the anode reaction that will produce oxygen from a product generated at the cathode using CO2 as the feed. Operation at low temperatures also will open up the full range of polymer and metal materials, allowing a more robust system design to withstand the rigors of flight, landing, and long term unattended operation on the surface of Mars.

Lueck, Dale E.↗

DOE OSTI2023

Polymer-based microfluidic device for on-chip counter-diffusive crystallization and in situ X-ray crystallography at room temperature

Proteins are long chains of amino acid residues that perform a myriad of functions in living organisms, including enzymatic reactions, signalling, and maintaining structural integrity. Protein function is determined directly by the protein structure. X-ray crystallography is the primary technique for determining the 3D structure of proteins, and facilitates understanding the effects of protein structure on function. The first step towards structure determination is crystallizing the protein of interest. We have developed a centrifugally-actuated microfluidic device that incorporates the fluid handling and metering necessary for protein crystallization. Liquid handling takes advantage of surface forces to control fluid flow and enable metering, without the need for any fluidic or pump connections. Our approach requires only the simple steps of pipetting the crystallization reagents into the device followed by either spinning or shaking to set up counter-diffusive protein crystallization trials. The use of thin, UV-curable polymers with a high level of X-ray transparency allows for in situ X-ray crystallography, eliminating the manual handling of fragile protein crystals and streamlining the process of protein structure analysis. We demonstrate the utility of our device using hen egg white lysozyme as a model system, followed by the crystallization and in situ, room temperature structural analysis of the hub domain of calcium–calmodulin dependent kinase II (CaMKIIβ).

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS2004

Zeolite Formation and Weathering Processes in Dry Valleys of Antartica: Martian Analogs

Terrestrial weathering processes in cold-desert climates such as the Dry Valleys of Antarctica may provide an excellent analog to chemical weathering and diagenesis of soils on Mars. Detailed studies of soil development and the chemical and mineralogical alterations occurring within soil columns in Wright Valley, Antarctica show incredible complexity in the upper meter of soil. Previous workers noted the ice-free Dry Valleys are the best terrestrial approximations to contemporary Mars. Images returned from the Pathfinder and Spirit landers show similarities to surfaces observed within the Dry Valleys. Similarities to Mars that exist in these valleys are: mean temperatures always below freezing (-20 C), no rainfall, sparse snowfall-rapidly removed by sublimation, desiccating winds, diurnal freeze-thaw cycles (even during daylight hours), low humidity, oxidative environment, relatively high solar radiation and low magnetic fields . The Dry Valley soils contain irregular distributions and low abundances of soil microorganisms that are somewhat unusual on Earth. Physical processes-such as sand abrasion-are dominant mechanisms of rock weathering in Antarctica. However, chemical weathering is also an important process even in such extreme climates. For example, ionic migration occurs even in frozen soils along liquid films on individual soil particles. It has also been shown that water with liquid-like properties is present in soils at temperatures on the order of approx.-80 C and it has been observed that the percentage of oxidized iron increases with increasing soil age and enrichments in oxidized iron occurs toward the surface. The presence of evaporates is evident and appear similar to "evaporite sites" within the Pathfinder and Spirit sites. Evaporites indicate ionic migration and chemical activity even in the permanently frozen zone. The presence of evaporates indicates that chemical weathering of rocks and possibly soils has been active. Authogenic zeolites have been identified within the soil columns because they are fragile; i.e. they are euhedral, unabraded, and unfractured, strongly suggesting in situ formation. Their presence in Antarctic samples is another indication that diagenic processes are active in cold-desert environments. The presence of zeolites, and other clays along with halites, sulfates, carbonates, and hydrates are to be expected within the soil columns on Mars at the Gusev and Isidis Planitia regions. The presence of such water-bearing minerals beneath the surface supplies one of the requirements to support biological activity on Mars.

Gibson, E. K., Jr.↗

NASA NTRS2007

Protective Skins for Aerogel Monoliths

A method of imparting relatively hard protective outer skins to aerogel monoliths has been developed. Even more than aerogel beads, aerogel monoliths are attractive as thermal-insulation materials, but the commercial utilization of aerogel monoliths in thermal-insulation panels has been inhibited by their fragility and the consequent difficulty of handling them. Therefore, there is a need to afford sufficient protection to aerogel monoliths to facilitate handling, without compromising the attractive bulk properties (low density, high porosity, low thermal conductivity, high surface area, and low permittivity) of aerogel materials. The present method was devised to satisfy this need. The essence of the present method is to coat an aerogel monolith with an outer polymeric skin, by painting or spraying. Apparently, the reason spraying and painting were not attempted until now is that it is well known in the aerogel industry that aerogels collapse in contact with liquids. In the present method, one prevents such collapse through the proper choice of coating liquid and process conditions: In particular, one uses a viscous polymer precursor liquid and (a) carefully controls the amount of liquid applied and/or (b) causes the liquid to become cured to the desired hard polymeric layer rapidly enough that there is not sufficient time for the liquid to percolate into the aerogel bulk. The method has been demonstrated by use of isocyanates, which, upon exposure to atmospheric moisture, become cured to polyurethane/polyurea-type coats. The method has also been demonstrated by use of commercial epoxy resins. The method could also be implemented by use of a variety of other resins, including polyimide precursors (for forming high-temperature-resistant protective skins) or perfluorinated monomers (for forming coats that impart hydrophobicity and some increase in strength).

Leventis, Nicholas↗

NASA NTRS2013

Lessons Learned from the Stardust Sample Return Mission

These are science and mission design and operations lessons learned from the Stardust Mission, which returned grains from comet Wild-2 and fresh interstellar dust to Earth in 2006 [1]. Science Lessons: Major discoveries of the Stardust Wild-2 samples include the presence of numerous chondrules and CAI in a comet, which requires a much more dynamic early solar system than many had envisaged, and verified predictions made by models requiring outward flow of early solar system solids before the early nebular gas had dissipated [1-3]. No evidence has been found for the presence of live Al-26 in the comet, suggesting late accretion [4]. Carbonates and unusual sulfides were found which potentially require activity of liquid water within the comet, but to only a minor degree at best [5-6]. The presence of abundant thermally-metamorphosed silicates in Wild-2 appears to require assembly from an earlier generation of bodies [7]. The abundance of presolar grains in the Wild-2 samples appears to be below what has been found in most chondritic IDPs and primitive chondrites [1]. The bulk mineralogy of Wild-2 grains does not match the mineralogy from any single other known astromaterial [7], and is also strikingly unlike that inferred from Spitzer Telescope spectra of Comet Temple 1 dust [8]. Amino acids and other fragile organics have been detected among the Wild-2 samples [9], which highlights the critical importance of further developing techniques for organic analysis in small samples, and cleaning outbound spacecraft.

Zolensky, M. E.↗

NASA NTRSDate not supplied

Ryugu-Like Phyllosilicate Clast from A Giant Cluster IDP of Probable Cometary Origin: Evidence for Material Exchange Between Asteroidal and Cometary Regions

The presence of hydrous minerals in comets is currently an open question. They were commonly produced inside primitive meteorite parent bodies but apparently not inside the active comets that never contained liquid water. Despite examination of hundreds of particles returned from the Jupiter Family comet Wild 2 by the Stardust(SD) spacecraft, no phyllosilicates have yet been found. Near IR spectra obtained by the Rosetta spacecraft of short-period comet 67P Churyumov-Gerasimenko (67P CG) similarly did not reveal the presence of phyllosilicate minerals. IR spectral features in ejecta from comet Temple 1were interpreted as hydrated minerals but this match is controversial. Studies of a giant cluster interplanetary dust particle (IDP) have demonstrated that the IDP has a large number of chemical and physical properties consistent with its derivation from a comet including 1) its porous aggregate morphology similar to fragile aggregate particles imaged from comet 67P CG, 2) an unequilibrated mineral assemblage, 3) mineral isotopic compositions similar to like minerals in comet Wild 2, 4) uncorrelated Fe-Mn ratios of olivines that mimic those from Wild 2, 5) high presolar silicate abundance [8] and 6) Kool grains which are observed in comet Wild 2 but not in chondrites. Our examination of 70+>5 μm fragments from the IDP have shown that it is overwhelmingly composed of anhydrous silicates. We have observed, however, a 5 x 15 μm porous aggregate fragment (LT10), which contains a rare phyllosilicate clast encased in anhydrous mineral and rock fragments. We conducted detailed TEM and O isotopic analyses of this particle to constrain its origin.

D J Joswiak↗

NASA NTRS1997

Application of NASA's Advanced Life Support Technologies in Polar Regions

The problems of obtaining adequate pure drinking water and disposing of liquid and solid waste in the U.S Arctic, a region where virtually all water is frozen solid for much of the year, has led to unsanitary solutions. Sanitation and a safe water supply are particularly problems in rural villages. These villages are without running water and use plastic buckets for toilets. The outbreak of diseases is believed to be partially attributable to exposure to human waste and lack of sanitation. Villages with the most frequent outbreaks of disease are those in which running water is difficult to obtain. Waste is emptied into open lagoons, rivers, or onto the sea coast. It does not degrade rapidly and in addition to affecting human health, can be harmful to the fragile ecology of the Arctic and the indigenous wildlife and fish populations. Current practices for waste management and sanitation pose serious human hazards as well as threaten the environment. NASA's unique knowledge of water/wastewater treatment systems for extreme environments, identified in the Congressional Office of Technology Assessment report entitled An Alaskan Challenge: Native Villagt Sanitation, may offer practical solutions addressing the issues of safe drinking water and effective sanitation practices in rural villages. NASA's advanced life support technologies are being combined with Arctic science and engineering knowledge to address the unique needs of the remote communities of Alaska through the Advanced Life Systems for Extreme Environments (ALSEE) project. ALSEE is a collaborative effort involving the NASA, the State of Alaska, the University of Alaska, the North Slope Borough of Alaska, Ilisagvik College in Barrow and the National Science Foundation (NSF). The focus is a major issue in the State of Alaska and other areas of the Circumpolar North; the health and welfare of its people, their lives and the subsistence lifestyle in remote communities, economic opportunity, and care for the environment. As advanced technologies are transferred to the commercial sector the ALSEE project Offers the potential for development of new industries in Alaska to supply the products to support remote communities of the globe.

Bubenheim, David L.↗

DOE OSTI2021

Operator learning for predicting multiscale bubble growth dynamics

We report simulating and predicting multiscale problems that couple multiple physics and dynamics across many orders of spatiotemporal scales is a great challenge that has not been investigated systematically by deep neural networks (DNNs). Herein, we develop a framework based on operator regression, the so-called deep operator network (DeepONet), with the long-term objective to simplify multiscale modeling by avoiding the fragile and time-consuming “hand-shaking” interface algorithms for stitching together heterogeneous descriptions of multiscale phenomena. To this end, as a first step, we investigate if a DeepONet can learn the dynamics of different scale regimes, one at the deterministic macroscale and the other at the stochastic microscale regime with inherent thermal fluctuations. Specifically, we test the effectiveness and accuracy of the DeepONet in predicting multirate bubble growth dynamics, which is described by a Rayleigh–Plesset (R–P) equation at the macroscale and modeled as a stochastic nucleation and cavitation process at the microscale by dissipative particle dynamics (DPD). First, we generate data using the R–P equation for multirate bubble growth dynamics caused by randomly time-varying liquid pressures drawn from Gaussian random fields (GRFs). Our results show that properly trained DeepONets can accurately predict the macroscale bubble growth dynamics and can outperform long short-term memory networks. We also demonstrate that the DeepONet can extrapolate accurately outside the input distribution using only very few new measurements. Subsequently, we train the DeepONet with DPD data corresponding to stochastic bubble growth dynamics. Although the DPD data are noisy and we only collect sparse data points on the trajectories, the trained DeepONet model is able to predict accurately the mean bubble dynamics for time-varying GRF pressures. Taken together, our findings demonstrate that DeepONets can be employed to unify the macroscale and microscale models of the multirate bubble growth problem, hence providing new insight into the role of operator regression via DNNs in tackling realistic multiscale problems and in simplifying modeling with heterogeneous descriptions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS2005

Lightweight Thermal Insulation for a Liquid-Oxygen Tank

A proposed lightweight, reusable thermal-insulation blanket has been designed for application to a tank containing liquid oxygen, in place of a non-reusable spray-on insulating foam. The blanket would be of the multilayer-insulation (MLI) type and equipped with a pressure-regulated nitrogen purge system. The blanket would contain 16 layers in two 8-layer sub-blankets. Double-aluminized polyimide 0.3 mil (.0.008 mm) thick was selected as a reflective shield material because of its compatibility with oxygen and its ability to withstand ionizing radiation and high temperature. The inner and outer sub-blanket layers, 1 mil (approximately equals 0.025 mm) and 3 mils (approximately equals 0.076 mm) thick, respectively, would be made of the double-aluminized polyimide reinforced with aramid. The inner and outer layers would provide structural support for the more fragile layers between them and would bear the insulation-to-tank attachment loads. The layers would be spaced apart by lightweight, low-thermal-conductance netting made from polyethylene terephthalate.

Willen, G. Scott↗

DOE OSTI2024

In-situ electrochemical optical techniques in the investigation of lithium interfacial phenomena with a liquid and a solid-state electrolyte

An in-situ electrochemical optical diagnosis is the key to the investigation of electrode interface during a redox reaction. Because the morphology changes particularly, dendrite formation, dendrite shapes, solid electrolyte interface formation and gas generation can be revealed visually. The challenge of ensuring uniform current density on a flat Li anode in a liquid electrolyte was addressed and uniform Li plating was demonstrated. The dendrite shape change under different reduction current density was discussed. Here the Li dendrite shape change and the performance of Li anodes with a surface lamination of graphite and red phosphate were used as examples to demonstrate the capability of the in-situ optical cell. An in-situ electrochemical optical cell used in the investigation of the increasingly popular solid-state Li batteries has its own challenges. Due to the untransparent nature of a solid-state electrolyte, an optical investigation on a solid-state electrolyte Li battery needs to be done by exposing the cross-section of the cell. In addition, it is very difficult to assemble an optical cell with a brittle and fragile solid-state electrolyte in a glove box. A set of formation and transfer dies, and an optical cell were introduced. The Li dendrite growth at the interface can be observed in a solid-state Li cell.

25 ENERGY STORAGE↗

NASA NTRS1995

Advanced Life Systems for Extreme Environments: An Arctic Application

The problems of obtaining adequate pure drinking water and disposing of liquid and solid waste in the U.S. Arctic, a region where virtually all water is frozen solid for much of the year, has led to unsanitary solutions (U.S. Arctic Research Commission). These solutions are also damaging to the environment. Sanitation and a safe water supply are particularly problems in rural villages. About one-fourth of Alaska's 86.000 Native residents live in these communities. They are without running water and use plastic buckets for toilets. The outbreak of diseases is believed to be partially attributable to exposure to human waste. Villages with the most frequent outbreaks of disease are those in which running water is difficult to obtain (Office of Technology Assessment, 1994). Waste is emptied into open lagoons, rivers, or onto the sea coast. It does not degrade rapidly and in addition to affecting human health, can be harmful to the fragile ecology of the Arctic and the indigenous wildlife and fish populations. Advanced Life Systems for Extreme Environments (ALSEE) provides a solution to sanitation and safe water problems. The system uses an advanced integrated technology developed for Antarctic and space applications. ALSEE uses the systems approach to address more than waste and water problems. By incorporating hydroponic horticulture and aquaculture into the waste treatment system, ALSEE addresses the quality and quantity of fresh foods available to Arctic residents. A temperate climate is required for year-round plant growth. ALSEE facilities can be designed to include a climate controlled area within the structure. This type of environment is a change from the long periods of darkness and cold found in the Arctic and can help alleviate stress so often associated with these extremes. While the overall concept of ALSEE projects is advanced, system facilities can be operated by village residents with appropriate training. ALSEE provides continuing training and education as a part of the project. Not only is this desirable but necessary. There is ample evidence in "gravoyard" throughout rural Alaska of technologies which failed not because they were not applic4tble, but because they were not integrated and could not be operated or repaired by village residents. Waste streams in villages will vary depending on the human diet and the non-food waste stream. ALSEE units can be adapted to different village situations once the content of the waste stream is known. Units located in population hubs can serve as research, education. and demonstration centers. Appropriate modifications can be determined at these centers to transfer technology to more remote locations where waste stream conditions may differ.

Lewis, Carol E.↗

DOE OSTI2024

Theory of Ion-Mediated Segmental Localization, Activated Structural Relaxation, and the Glass Transition in Polymerized Ionic Liquids

Here we combine polymer integral equation theory for structural correlations with a force-level theory for activated segmental relaxation to construct a microscopic theory for how ions modify the onset of segmental localization, the polymer alpha relaxation time, and glass transition temperature, T g , in dry polymerized ionic liquids (PolyILs). Our most important findings concerning the behavior of T g are (i) a weak dependence on anion–cation Coulomb attraction strength due to strong decoupling of ion and segmental dynamics, (ii) strong reduction with increasing mobile ion size due to both plasticization effects and weakening of ion-modified monomer caging, and (iii) increase with backbone rigidity and intrachain dynamic cooperativity. We quantitatively estimate T g variations as ion size and polymer static and dynamic rigidity are widely varied. The experimental data of 19 PolyILs are organized into a specific pattern consistent with the theoretical predictions with glass transition temperatures varying over a very wide range (~250 K) as observed experimentally. Based on the theoretical results, suggestions are made concerning the search for high conductivity Li- or Na-based PolyILs based on further lowering of T g via new polymer synthesis. Calculations of the alpha time as a function of packing fraction reveal the dynamic fragility increases for larger mobile ions, a more flexible backbone, and/or a smaller degree of intrachain dynamic cooperativity, as a consequence of the increasing importance of collective elasticity in determining the activation barrier. An analysis of transient segmental localization and a crossover to activated dynamics reveals similar, but not identical, trends as predicted at the laboratory vitrification timescale.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

Arrhenian to non-Arrhenian crossover in glass melt viscosity

The activation energy for glass melt viscosity is a function of temperature, i.e., non-Arrhenian, within a middle range of viscosity values (typically, between 10 2 and 10 10 Pa s) and constant, i.e., Arrhenian, outside this range. At the low-viscosity end, the Arrhenian to non-Arrhenian transition (termed the crossover) falls within the glass processing range: glass melting and fining occur within the Arrhenian range while glass forming occurs within the non-Arrhenian range. By the Adam-Gibbs equation, the configuration entropy is nearly constant at high temperatures (low viscosities), where the glass melt turns into a simple liquid, and decreases with decreasing temperature (increasing viscosity) as the glass is increasingly polymerized. In the present study, the power-law function and hyperbolic tangent function are used to express the configuration entropy as a function of temperature. The viscosity crossover is defined as the point at which onset of structural grouping is causing the configuration entropy to deviate from its high-temperature value. In conclusion, it appears that the limited range of the configuration entropy of the fully depolymerized melt imposes a restriction on the crossover viscosity; for well-defined glass families, such as float glasses or nuclear waste glasses, the crossover point can be defined using a fixed, i.e., composition-independent, viscosity value.

36 MATERIALS SCIENCE↗

NASA NTRS2012

Focal Plane Alignment Utilizing Optical CMM

In many applications, an optical detector has to be located relative to mechanical reference points. One solution is to specify stringent requirements on (1) mounting the optical detector relative to the chip carrier, (2) soldering the chip carrier onto the printed circuit board (PCB), and (3) installing the PCB to the mechanical structure of the subsystem. Figure 1 shows a sketch of an optical detector mounted relative to mechanical reference with high positional accuracy. The optical detector is typically a fragile wafer that cannot be physically touched by any measurement tool. An optical coordinate measuring machine (CMM) can be used to position optical detectors relative to mechanical reference points. This approach will eliminate all requirements on positional tolerances. The only requirement is that the PCB is manufactured with oversized holes. An exaggerated sketch of this situation is shown in Figure 2. The sketch shows very loose tolerances on mounting the optical detector in the chip carrier, loose tolerance on soldering the chip carrier to the PCB, and finally large tolerance on where the mounting screws are located. The PCB is held with large screws and oversized holes. The PCB is mounted loosely so it can move freely around. The optical CMM measures the mechanical reference points. Based on these measurements, the required positions of the optical detector corners can be calculated. The optical CMM is commanded to go to the position where one detector corner is supposed to be. This is indicated with the cross-hairs in Figure 2(a). This figure is representative of the image of the optical CMM monitor. Using a suitable tapping tool, the PCB is manually tapped around until the corner of the optical detector is at the crosshairs of the optical CMM. The CMM is commanded to another corner, and the process is repeated a number of times until all corners of the optical detector are within a distance of 10 to 30 microns of the required position. The situation is sketched in Figure 2(b) (the figure also shows the tapping tool and where to tap). At this point the fasteners for the PCB are torqued slightly so the PCB can still move. The PCB location is adjusted again with the tapping tool. This process is repeated 3 to 4 times until the final torque is achieved. The oversized mounting holes are then filled with a liquid bonding agent to secure the board in position (not shown in the sketch). A 10- to 30-micron mounting accuracy has been achieved utilizing this method..

Liebe, Carl Christian↗

DOE OSTI2023

Accelerating Biomimetic Solar - Energy Harvesting: Mapping the Interaction Landscape of Plasmonic-Excitonic Hybrid Nanosystems (Final Report)

In general, excitonic and plasmonic nanoscale materials in close proximity show high potential for significant breakthroughs in energy related materials research. The interactions between these two kinds of materials result in coupled optical transitions (plexcitons), distinct from those of both the individual exciton and plasmon as well as from those of the sum of their constituents (synergistic effects). By linking together materials-research and physical-research approaches, this project contributes to a concerted approach on nanomaterials energy research. The project’s overall goal is to accelerate the development of well-defined plexcitonic model systems consisting of carefully engineered plasmonic and excitonic nanomaterial— essential for both gaining a fundamental understanding of plexcitonic nanomaterials and the development of novel design principles for biomimetic solar energy harvesting. During the 3-year project period and the terminal renewal with limited support for a 12-month period, we successfully synthesized and characterized (1) a robust excitonic nanomaterial and (2) a library of plasmonic nanoparticles as well as developed (3) a microfluidic platform for homogenous nanosynthesis as summarized below: (1) Robust Excitonic Nanomaterial. Supramolecular assemblies are Nature’s most successful material system for solar energy harvesting. However, photovoltaic devices based on artificial supramolecular assemblies continue to be stymied by disappointing efficiencies and poor stability. The conceptual failure may lie in current solar cell architectures, which rely on solidifying supramolecular assemblies as an ensemble into a solid matrix, neglecting the intrinsic fragility of the assemblies’ internal structure, thus disrupting or even destroying their delicate optoelectronic properties, that is, delicate Frenkel excitonic properties. Supramolecular assemblies may finally serve as usable light harvesting material systems for solar energy conversion technologies, only if they meet the following criteria: (a) Stability, that is, the fragile structure including its delicate Frenkel excitonic character needs to be stable, (b) Robustness, that is, resistant against elevated and fluctuating temperatures, and (c) Viability for device integration, that is, capable of being immobilized onto solid substrates. Here, by developing a nanocomposite via a tunable, cage-like scaffold design, we successfully provided stable supramolecular nanocomposites, that inhabit robust Frenkel excitons despite harming environmental conditions such as extreme heat stress. (2) Library of Plasmonic Nanoparticles. Naturally, current models describing plasmonic hybrid quantum states—plasmonic hybridizations—parallel those developed for molecular orbitals, equating individual plasmonic nanostructures with “atoms” and the plasmonic nanoassemblies with “molecules.” In analogy to organic synthesis, a suitably robust fabrication method would allow for “atom-like” manipulation of “molecule-like” plasmonic nanoassemblies; of high value for next-generation energy nanotechnologies. Despite this frequent comparison, current plasmonic nanoassembly fabrication methods favor top-down templating over wet-chemical synthesis, however, achieving precise control over nanostructure’s geometry and surface characteristics remain an art and a scientific challenge. The conceptual failure may lie in the current wet-chemical synthesis paradigm, as it relies on the accessibility of a multi-dimensional synthesis parameter space through limited, rather one-dimensional synthesis procedures by employing step-by-step approaches. Solution-based nanoarchitectonics for rational design of precisely built plasmonic nanoassemblies via solution-based fabrication may finally be possible only if multi-dimensional syntheses approaches are available that allow for comprehensive control over the plasmonic nanomaterials’ (a) Structural Properties and (b) Surface Properties. Here, by developing an innovative multidimensional 1,3-propanediol based polyol synthesis, we successfully provided control over the plasmonic building-block’s geometry (size and shape) together with its surface characteristics. Our results present a critical step toward the vision of a “periodic table-like” system for plasmonic materials based on straightforward wet-chemical syntheses for energy nanotechnologies. Developing deliberate modifications on this synthesis, we generated a library of plasmonic nanostructures covering the vast parameter space—opening the door for fundamental investigation of plexcitonic model systems. (3) Microfluidic Platform for Homogenous Nanosynthesis. Control over structural properties of plexcitonic nanocomposites remains a challenge due to current limitations in nanosynthesis techniques. Slight variations in nanostructure’s geometry impact their optoelectronic properties, demanding precise synthesis beyond the capabilities of solution-based (batch) synthesis processes. In contrast, the small, confined liquid volumes used in microfluidics—a reaction technique where the manipulation of fluids takes place in channels with dimensions of tens of micrometers—allows for homogenous synthesis conditions, providing excellent control of the reaction and, as a result, of the materials’ geopmetry and composition. However, thus far, the majority of plexcitonic systems has been developed via batch synthesis. Here, by successfully developing a two-channel microreactor, our microfluidic-supported synthesis approach combines the advantages of both microfluidics and batch platforms, allowing for precise spatio-temporal control over all synthesis parameters opening the possibility for homogenous nanosythnesis of well-defined plexcitonic model systems.

14 SOLAR ENERGY↗