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At least 559 records · Page 31

Image analysis of particle field by means of computed tomography

In order to visualize and investigate spray structures, computed tomography technique is applied to analyze droplet information. From the transmitted light intensity through the spray and/or the data of particle size distribution obtained from a Fraunhofer diffraction principle, the quantitative volume of spray droplet or local particle size was calculated and the reconstruction of spray structures was made. The background of computed tomography is described along with some experimental results of the structure of intermittent spray such as diesel spray.

Nakayama, Mitsushige↗

Larger-Stroke Piezoelectrically Actuated Microvalve

A proposed normally-closed microvalve would contain a piezoelectric bending actuator instead of a piezoelectric linear actuator like that of the microvalve described in the preceding article. Whereas the stroke of the linear actuator of the preceding article would be limited to approximately equal to 6 micrometers, the stroke of the proposed bending actuator would lie in the approximate range of 10 to 15 micrometers-large enough to enable the microvalve to handle a variety of liquids containing suspended particles having sizes up to 10 m. Such particulate-laden liquids occur in a variety of microfluidic systems, one example being a system that sorts cells or large biomolecules for analysis. In comparison with the linear actuator of the preceding article, the bending actuator would be smaller and less massive. The combination of increased stroke, smaller mass, and smaller volume would be obtained at the cost of decreased actuation force: The proposed actuator would generate a force in the approximate range of 1 to 4 N, the exact amount depending on operating conditions and details of design. This level of actuation force would be too low to enable the valve to handle a fluid at the high pressure level mentioned in the preceding article. The proposal encompasses two alternative designs one featuring a miniature piezoelectric bimorph actuator and one featuring a thick-film unimorph piezoelectric actuator (see figure). In either version, the valve would consume a power of only 0.01 W when actuated at a frequency of 100 Hz. Also, in either version, it would be necessary to attach a soft elastomeric sealing ring to the valve seat so that any particles that settle on the seat would be pushed deep into the elastomeric material to prevent or reduce leakage. The overall dimensions of the bimorph version would be 7 by 7 by 1 mm. The actuator in this version would generate a force of 1 N and a stroke of 10 m at an applied potential of 150 V. The actuation force would be sufficient to enable the valve to handle a fluid pressurized up to about 50 psi (approximately equal to 0.35 MPa). The overall dimensions of the unimorph version would be 2 by 2 by 0.5 mm. In this version, an electric field across the piezoelectric film on a diaphragm would cause the film to pull on, and thereby bend, the diaphragm. At an applied potential of 20 V, the actuator in this version would generate a stroke of 10 micrometers and a force of 0.01 N. This force level would be too low to enable handling of fluids at pressures comparable to those of the bimorph version. This version would be useful primarily in microfluidic and nanofluidic applications that involve extremely low differential pressures and in which there are requirements for extreme miniaturization of valves. Examples of such applications include liquid chromatography and sequencing of deoxyribonucleic acid.

Yang, Eui-Hyeok↗

Few‐Unit‐Cell MFI Zeolite Synthesized using a Simple Di‐quaternary Ammonium Structure‐Directing Agent

Abstract Synthesis of a pentasil‐type zeolite with ultra‐small few‐unit‐cell crystalline domains, which we call FDP (few‐unit‐cell crystalline domain pentasil), is reported. FDP is made using bis‐1,5(tributyl ammonium) pentamethylene cations as structure directing agent (SDA). This di‐quaternary ammonium SDA combines butyl ammonium, in place of the one commonly used for MFI synthesis, propyl ammonium, and a five‐carbon nitrogen‐connecting chain, in place of the six‐carbon connecting chain SDAs that are known to fit well within the MFI pores. X‐ray diffraction analysis and electron microscopy imaging of FDP indicate ca. 10 nm crystalline domains organized in hierarchical micro‐/meso‐porous aggregates exhibiting mesoscopic order with an aggregate particle size up to ca. 5 μm. Al and Sn can be incorporated into the FDP zeolite framework to produce active and selective methanol‐to‐hydrocarbon and glucose isomerization catalysts, respectively.

Lu, Peng↗

Few‐Unit‐Cell MFI Zeolite Synthesized using a Simple Di‐quaternary Ammonium Structure‐Directing Agent

Abstract Synthesis of a pentasil‐type zeolite with ultra‐small few‐unit‐cell crystalline domains, which we call FDP (few‐unit‐cell crystalline domain pentasil), is reported. FDP is made using bis‐1,5(tributyl ammonium) pentamethylene cations as structure directing agent (SDA). This di‐quaternary ammonium SDA combines butyl ammonium, in place of the one commonly used for MFI synthesis, propyl ammonium, and a five‐carbon nitrogen‐connecting chain, in place of the six‐carbon connecting chain SDAs that are known to fit well within the MFI pores. X‐ray diffraction analysis and electron microscopy imaging of FDP indicate ca. 10 nm crystalline domains organized in hierarchical micro‐/meso‐porous aggregates exhibiting mesoscopic order with an aggregate particle size up to ca. 5 μm. Al and Sn can be incorporated into the FDP zeolite framework to produce active and selective methanol‐to‐hydrocarbon and glucose isomerization catalysts, respectively.

36 MATERIALS SCIENCE↗

Aggregation-induced phosphorescence sensitization in two heptanuclear and decanuclear gold–silver sandwich clusters

The strategy of aggregation-induced emission enhancement (AIEE) has been proven to be efficient in wide areas and has recently been adopted in the field of metal nanoclusters. Furthermore, the relationship between atomically precise clusters and AIEE is still unclear. Herein, we have successfully obtained two few-atom heterometallic gold–silver hepta-/decanuclear clusters, denoted Au 6 Ag and Au 9 Ag, and determined their structures by X-ray diffraction and mass spectrometry. The nature of the AuI…AgI interactions thereof is demonstrated through energy decomposition analysis to be far-beyond typical closed-shell metal–metal interaction dominated by dispersion interaction. Furthermore, a positive correlation has been established between the particle size of the nanoaggregates and the photoluminescence quantum yield for Au 6 Ag, manifesting AIEE control upon varying the stoichiometric ratio of Au : Ag in atomically-precise clusters.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Assembly of small silica nanoparticles using lipid-tethered DNA ‘bonds’

Single-stranded DNA molecules modified with cholesterol functional groups are physically tethered to silica nanoparticles (diameter 25 nm) that are encapsulated in a lipid bilayer. Such tethering increases the azimuthal mobility of the DNA molecules across the nanoparticle surface and enables nonspecific bonding, eliminating the need for specialized surface chemistries (such as silane or thiol ligands). To induce assembly, double-stranded DNA ‘bridge’ molecules are then added with complementary nucleotides to the DNA ‘anchor’ molecules that are physically tethered to the lipids on the surface of the particles. Assembly is observed to occur at room temperature and without the need for temperature annealing. Using automated liquid handling tools, assemblies are created in high throughput and rapidly characterized using SAXS. It is determined that the relative concentration of DNA-to-silica and the ionic strength of the solution are important parameters that affect the resulting assembly. Analysis of SAXS data is performed using coarse-grained particle dynamics simulations. The results support the spontaneous formation of semi-crystalline particle assemblies by particle condensation, where the interparticle distance is tuned by the sequence of the DNA ‘bridge’ used to link the particles. Crystallinity analysis performed on the resulting simulations, optimized to match SAXS observations, suggest that particle clusters display increased crystallinity in the center of the clusters, but their maximum size remains relatively small (sub-micron) before settling occurs, which limits the extent of crystallization.

Chiang, Huat Thart [Univ. of Washington, Seattle, ↗

LIvermore SEM image Tools

Scanning Electron Microscopy (SEM) images provide a variety of structural and morphological information for the characterization of the nanomaterials. This code offers automatic recognition and quantitative analysis of SEM images in a high-throughput manner using computer vision and machine learning techniques. The main function of this application is to extract particle size and morphology information of overlapping nanoparticles and core-shell nanostructures in a user friendly interface. The code is written in C++ with QT environment, and has been tested on MacOSX.

KIM, HYOJIN↗

Diagnostics of wear in aeronautical systems

The use of appropriate diagnostic tools for aircraft oil wetted components is reviewed, noting that it can reduce direct operating costs through reduced unscheduled maintenance, particularly in helicopter engine and transmission systems where bearing failures are a significant cost factor. Engine and transmission wear modes are described, and diagnostic methods for oil and wet particle analysis, the spectrometric oil analysis program, chip detectors, ferrography, in-line oil monitor and radioactive isotope tagging are discussed, noting that they are effective over a limited range of particle sizes but compliment each other if used in parallel. Fine filtration can potentially increase time between overhauls, but reduces the effectiveness of conventional oil monitoring techniques so that alternative diagnostic techniques must be used. It is concluded that the development of a diagnostic system should be parallel and integral with the development of a mechanical system.

Wedeven, L. D.↗

Collectors Of Airborne And Spaceborne Particles

Brushlike collectors capture samples of dust and other particles in space vacuum or air for optical, scanning-electron-microscope, and/or x-ray analysis. Gently decelerates particles without damaging them, minimizing tendency of some particles to rebound. Depending on design of specific collector of this type, it captures particles ranging upward in size from fractions of micrometer to few micrometers.

Frazer, Robert E.↗

Nanocrystalline Chalcopyrite Materials (CuInS2 and CuInSe2) via Low-Temperature Pyrolysis of Molecular Single-Source Precursors

Nanometer sized particles of the chalcopyrite compounds CuInS2 and CuInSe2 were synthesized by thermal decomposition of molecular single-source precursors (PPh3)2CuIn(SEt)4 and (PPh3)2CuIn(SePh)4, respectively, in the non-coordinating solvent dioctyl phthalate at temperatures between 200 and 300 C. The nanoparticles range in size from 3 - 30 nm and are aggregated to form roughly spherical clusters of about 500 nm in diameter. X-ray diffraction of the nanoparticle powders shows greatly broadened lines indicative of very small particle sizes, which is confirmed by TEM. Peaks present in the XRD can be indexed to reference patterns for the respective chalcopyrite compounds. Optical spectroscopy and elemental analysis by energy dispersive spectroscopy support the identification of the nanoparticles as chalcopyrites.

Castro, Stephanie L.↗

Xplo-SA9T: Optimization of Sorbent Technology With Existing and New Amine Variants for Carbon Dioxide Removal and Humidity Control

Scrubbing of the spacesuit air stream to control humidity and regulate carbon dioxide (CO 2 ) relies on amine-loaded resins, colloquially known as sorbents. The efficacy of Rapid Cycle Amine technology relies on the propensity of nitrogens toward adsorption of CO 2 while simultaneously offering regenerative properties under vacuum or positive pressure. The commonly utilized sorbent, SA9T, was recreated and evaluated further to increase stability and serve as a benchmark comparison for newly synthesized amine sorbent technologies. Ongoing storage studies with eight different environments will allow the development of applicable storage protocols and provide insight into possible ammonia generation pathways. Attempts to alleviate the known issues with SA9T included the alteration of the primary amine (tetraethylenepentamine), the choice of resin, and the particle size distribution. In-house CO 2 breakthrough experiments were conducted using a specialized apparatus that can simulate spacesuit conditions, offering high-quality triplicate capacity analysis affording direct comparison to known adsorbents in the literature. Thermo-Desorption Gas Chromatography Mass Spectrometry studies on the synthesized materials revealed any reagent or solvent offgassing while Nuclear Magnetic Resonance spectroscopy tracked the stability of the bound amine. Scanning Electron Microscope images of sieved materials provided a more accurate size interpretation facilitating synthetic design and pressure drop elimination. All efficient sorbents were synthesized to a commercial batch scale subsequent to evaluation including Xplo-SA9T.

John R Tidwell↗

Single-particle chemical analysis reveals organic-rich detonation soot products

The detonation of high explosives produces a wide variety of particulate matter (PM) with distinct properties, not all of which are traditionally studied for chemical composition, formation processes, and forensic applications. We report particle-resolved measurements of Composition B detonation soot using soot particle aerosol mass spectrometry (SP-AMS), identifying carbonaceous species and metals not previously characterized on a single-particle basis. Results are combined with scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDS) to enhance source-dependent signatures. Black carbon, including graphitic carbon and detonation nanodiamonds, contributed 50.5-71.4% of PM 2.5 mass, while 22.5-43.4% was non-refractory organic carbon, a previously overlooked component that exhibited a complex and varying composition. Detonations were performed with and without PMMA confinement and under steady and overdriven conditions. Distinct particles enriched with polycyclic aromatic hydrocarbons (PAHs) were observed in experiments utilizing confinement, with quantities dependent on manufacturing method. SEM-EDS validated SP-AMS findings of metals internally mixed with carbonaceous species and extended the particle size range to 100 µm. This work makes detecting non-refractory organics using single-particle techniques more feasible for detonation forensics and understanding high-energy soot formation. While this analysis uses offline sample collection, SP-AMS could be deployed for in-situ measurements of detonation PM 2.5 transported in the atmosphere.

36 MATERIALS SCIENCE↗

Using CubeSats to Monitor Debris Flux

Recent updates to NASA's Orbital Debris Engineering Model (ORDEM 3.0) include a population of small particles (1-2 mm in size) composed of high-density materials (e.g., steel) that drive much of the predicted risk for satellites in the 700-1000 km altitude regime. This modeled population was based on the analysis of returned surfaces of the Shuttle, which flew below 600 km altitude. The cessation of Shuttle missions, plus the lack of in situ data above 600 km means that a data source is being sought to either confirm or modify this high-density population. One possible data source would be a database of anomalous sporadic changes in spacecraft orbit/orientation that might be due to momentum transfer from small particles too small to seriously damage the spacecraft. Because the momentum imparted from an impact would be tiny, it would most likely show up in the orbital behavior of cubesats and other small satellites. While such small satellites were few in number, this was not a particularly attractive option, but now with the proliferation of cubesats in multiple orbit planes and altitudes, the possible collecting area has increased significantly. This presentation will discuss the physics of momentum-transferring impacts from hypervelocity collisions, and make predictions about rates, directions, and locations of such impacts. In addition, it will include recommendations for satellite users on what kind of data might be worth archiving and investigating.

Matney, Mark↗

DED Additively Manufactured HEAs Optimized via Parametric Study of Functionally Graded Materials

Complex concentrated alloys (CCAs) are a system of alloys composition of nearly equiatomic elements, creating a state of high configurational entropy in the material. These alloys are of interest for various industrial applications due to their high strength and hardness, wide operational temperature range, creep and diffusion resistance, and radiation resistance. In the current work CoCrFeNi-base CCAs are synthesize by combining three commonly industrial alloys: IN718, SS316L, and 70Co30Cr (commercially known as Stellite 21), in-situ utilizing directed energy deposition (DED) additive manufacturing (AM). One bulk specimen is fabricated with a 1:1:1 ratio of IN718, SS316L, and 70Co30Cr where IN718 is a source of nickel and chrome, SS316 is a source of iron and chrome, and 70Co30Cr is a source of cobalt and supplemental chrome. Additionally, a functionally graded material (FGM) of the identified CCA system from SS316 was fabricated with 10 layers, where the initial five layers are the base material of SS316L and graded by steps of 20% to transition to the CCA system. Overall build quality, microstructure, compositional distribution, phases analysis, and microhardness were studied by laser optical microscopy, scanning election microscopy (SEM), energy dispersive spectroscopy (EDS), X-ray diffraction analysis (XRD), and Vickers microhardness techniques. Overall build quality showed a successful bulk build with acceptable density, however unmelted particles are observed in the as-built alloy. Compositional results show that the system meets the Boltzmann’s hypothesis definition of an HEA, and that an FCC CCA was produced with increased hardness, small grain size, and superior hardness properties to the SS316L substrate. While initial XRD results show predominately FCC structure, EDS analysis of interdendritic regions show the existence of Laves phases in the material. The fabrication of an FGM CCA allowed for potential screening of additional alloy mixes which may be of interest to explore in future research, and the resulting composition is compared to predicted values. This novel method of CCA fabrication results in substantial cost savings of these CCA systems over traditional methods.

36 MATERIALS SCIENCE↗

Orion Artemis I As Flown MMOD Analysis

Introduction The Lockheed Martin Orion spacecraft conducted the Artemis I flight around the Moon from November 16 through December 11, 2022. After the flight, an engineer from the NASA Johnson Space Center (JSC) Hypervelocity Impact Technology (HVIT) Group performed a Micrometeoroid and Orbital Debris MMOD analysis using the Bumper 3 risk assessment tool to predict the number of small impacts that would likely have occurred during the mission. Separately, a team from the same group inspected the Orion capsule for hypervelocity impact damage features. The results of the inspection were compared to those of the analysis to aid in improving the analysis, including the environment models. Scope of Work The spacecraft geometry model was created by Lockheed Martin during construction of the Artemis I Orion vehicle based on Computer Aided Design (CAD) models of the vehicle. New hypervelocity impact testing was performed to verify Ballistic Limit Equations (BLEs) used in the analysis to link impactor size and damage to the Thermal Protection System (TPS). The exact trajectory flown was recorded during the flight, including vehicle attitude. This data was used in conjunction with the ORDEM 3.2 and MEM 3 environment modeling tools to create models of particle flux impacting the spacecraft throughout the mission. Meteoroid shower forecast information was also included to account for additional particle flux associated with meteoroid showers. Inspection of the Orion capsule included the Backshell thermal tiles and the tape covering it, windows, fabric thermal materials, and small areas of other materials. Potential MMOD damage found was characterized using various techniques, including optical microscopy, computed tomography scanning, and X-ray spectroscopy. Findings The number of craters found in the Backshell tile, and their size distribution, matches well with the Bumper analysis prediction. Tape, window, and other material impacts recorded similarly align to Bumper analysis predictions. Conclusions and Recommendations This comparison of analysis with inspection of the hardware provides valuable insight into the MMOD environment and how accurately analysis tools assess the impact risk to spacecraft. As this was the first large, non-ablative returned surface from a lunar mission, this analysis extends the MMOD community’s insight beyond low Earth orbit into cis-lunar space.

MMOD↗

Orion Artemis I As Flown MMOD Analysis

Introduction The Lockheed Martin Orion spacecraft conducted the Artemis I flight around the Moon from November 16 through December 11, 2022. After the flight, an engineer from the NASA Johnson Space Center (JSC) Hypervelocity Impact Technology (HVIT) Group performed a Micrometeoroid and Orbital Debris MMOD analysis using the Bumper 3 risk assessment tool to predict the number of small impacts that would likely have occurred during the mission. Separately, a team from the same group inspected the Orion capsule for hypervelocity impact damage features. The results of the inspection were compared to those of the analysis to aid in improving the analysis, including the environment models. Scope of Work The spacecraft geometry model was created by Lockheed Martin during construction of the Artemis I Orion vehicle based on Computer Aided Design (CAD) models of the vehicle. New hypervelocity impact testing was performed to verify Ballistic Limit Equations (BLEs) used in the analysis to link impactor size and damage to the Thermal Protection System (TPS). The exact trajectory flown was recorded during the flight, including vehicle attitude. This data was used in conjunction with the ORDEM 3.2 and MEM 3 environment modeling tools to create models of particle flux impacting the spacecraft throughout the mission. Meteoroid shower forecast information was also included to account for additional particle flux associated with meteoroid showers. Inspection of the Orion capsule included the Backshell thermal tiles and the tape covering it, windows, fabric thermal materials, and small areas of other materials. Potential MMOD damage found was characterized using various techniques, including optical microscopy, computed tomography scanning, and X-ray spectroscopy. Findings The number of craters found in the Backshell tile, and their size distribution, matches well with the Bumper analysis prediction. Tape, window, and other material impacts recorded similarly align to Bumper analysis predictions. Conclusions and Recommendations This comparison of analysis with inspection of the hardware provides valuable insight into the MMOD environment and how accurately analysis tools assess the impact risk to spacecraft. As this was the first large, non-ablative returned surface from a lunar mission, this analysis extends the MMOD community’s insight beyond low Earth orbit into cis-lunar space.

MMOD↗

Liquid crystalline behavior and photoluminescence of lanthanide decanoate nanoparticles synthesized by microwave radiation

Luminescent lanthanide decanoate nanoparticles (LnC 10 NPs; Ln = Pr, Nd, Sm, Eu, Gd, Er) with spherical morphology (<100 nm) have been synthesized via a facile microwave (MWV) method using Ln(NO 3 ) 3 ·xH 2 O, ethanol/water, and decanoic acid. These hybrid nanomaterials adopt a lamellar structure consisting of inorganic Ln 3+ layers separated by a decanoate anion bilayer and exhibit liquid crystalline (LC) phases during melting. The particle size, crystalline structure, and LC behavior were characterized using transmission electron microscopy (TEM), differential scanning calorimetry (DSC), and powder X-ray diffraction (ambient and heated). Thermal analysis indicated the formation of Smectic A LC phases by LnC 10 nanoparticles, with the smaller lanthanides (Ln = Sm, Gd, Er) displaying additional solid intermediate and Smectic C phases. The formation of LC phases by the smaller Ln 3+ suggests that these nanoscale materials have vastly different thermal properties than their bulk counterparts, which do not exhibit LC behavior. In this work, photoluminescence spectroscopy revealed the LnC 10 NPs to be highly optically active, producing strong visible emissions that corresponded to expected electronic transitions by the various Ln 3+ ions. Under long-wave UV irradiation (λ = 365 nm), bright visible luminescence was observed for colloidal suspensions of Nd, Sm, Eu, Gd, and ErC 10 NPs. To the best of the authors’ knowledge, this is the first reported synthesis of nanoscale metal alkanoates, the first report of liquid crystalline behavior by any decanoate of lanthanides smaller than Nd, and the first observation of strong visible luminescence by non-vitrified lanthanide alkanoates.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗