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All sourcesNASA NTRSDOE OSTI
NASA NTRS2014

Optoelectronic Tweezers for Microparticle and Cell Manipulation

An optical image-driven light induced dielectrophoresis (DEP) apparatus and method are described which provide for the manipulation of particles or cells with a diameter on the order of 100 micromillimeters or less. The apparatus is referred to as optoelectric tweezers (OET) and provides a number of advantages over conventional optical tweezers, in particular the ability to perform operations in parallel and over a large area without damage to living cells. The OET device generally comprises a planar liquid-filled structure having one or more portions which are photoconductive to convert incoming light to a change in the electric field pattern. The light patterns are dynamically generated to provide a number of manipulation structures that can manipulate single particles and cells or group of particles/cells. The OET preferably includes a microscopic imaging means to provide feedback for the optical manipulation, such as detecting position and characteristics wherein the light patterns are modulated accordingly.

Wu, Ming Chiang↗
NASA NTRS2018

Method of Making Dye-Doped Polystyre Microparticles

Various embodiments provide dye-doped polystyrene microspheres generated using dispersion polymerization. Polystyrene microspheres may be doped with fluorescent dyes, such as xanthene derivatives including kiton red 620 (KR620), using dispersion polymerization. Certain functionalities, such as sodium styrene sulfonate, may be used to shift the equilibrium distribution of dye molecules to favor incorporation of the dye into the particles. Polyelectrolyte materials, such as poly(diallyldimethyl ammonium chloride), PolyDADMAC, may be used to electrostatically trap and bind dye molecules within the particles. A buffer may be used to stabilize the pH change of the solution during dye-doped polystyrene microsphere generation and the buffer may be selected depending on the pKa of the dye being incorporated. The various embodiments may provide dye-doped polystyrene microspheres, such as KR620-doped polystyrene microspheres that are non-toxic and non-carcinogenic. These non-toxic and non-carcinogenic dye-doped polystyrene microspheres may be suitable for use in wind tunnel testing.

Wohl, Jr., Christopher J.↗
DOE OSTI2025

High‐Concentration Antibody Formulation via Solvent‐Based Dehydration

Abstract Although subcutaneous (SC) delivery is the preferred administration route for immunotherapies and other biologics for improved patient compliance and lower healthcare costs, it necessitates high‐concentration antibody formulations. However, high‐concentration antibody solutions face significant instabilities and prohibitively high viscosities. Other approaches for high‐concentration formulations have been developed, including non‐aqueous solutions, which can be irritating or painful, and antibody‐laden hydrogel microparticles, which require centrifugation and are limited to concentrations <300 mg mL −1 . This work presents a new formulation process wherein the antibody is concentrated and encapsulated into hydrogel microparticles via solvent‐based dehydration. The final dosage form is an aqueous particle suspension with a formulation concentration of 360 mg mL −1 . In this process, microparticles are synthesized continuously, and antibody precipitation is realized simultaneously to dehydration, which allows for higher antibody concentrations. Antibody phase behavior and precipitation–dehydration kinetics are analyzed. The antibody is structurally and functionally stable in the microparticle post‐processing and after 4 months. Injectability of the suspension meets clinical standards with glide force <20 N. For the first time, an aqueous antibody formulation at high concentrations comparable to non‐aqueous formulations is presented, ideal for subcutaneous administration. The process is envisioned to be generalizable as a platform for SC delivery in multiple clinical applications.

Zheng, Talia [Department of Chemical Engineering M↗
NASA NTRS2015

Characterization of Encapsulated Corrosion Inhibitors for Environmentally Friendly Smart Coatings

The NASA Kennedy Space Center's Corrosion Technology Lab at the Kennedy Space Center in Florida, U.S.A. has been developing multifunctional smart coatings based on the microencapsulation of environmentally friendly corrosion indicators, inhibitors and self-healing agents. This allows the incorporation of autonomous corrosion control functionalities, such as corrosion detection and inhibition as well as the self-healing of mechanical damage, into coatings. This paper presents technical details on the characterization of inhibitor-containing particles and their corrosion inhibitive effects using electrochemical and mass loss methods. Three organic environmentally friendly corrosion inhibitors were encapsulated in organic microparticles that are compatible with desired coatings. The release of the inhibitors from the microparticles in basic solution was studied. Fast release, for immediate corrosion protection, as well as long-term release for continued protection, was observed. The inhibition efficacy of the inhibitors, incorporated directly and in microparticles, on carbon steel was evaluated. Polarization curves and mass loss measurements showed that, in the case of 2MBT, its corrosion inhibition effectiveness was greater when it was delivered from microparticles.

Corrosion↗
NASA NTRS2015

Release Properties and Electrochemical Characterization of Encapsulated Corrosion Inhibitors for Environmentally Friendly Smart Coatings

The NASA Kennedy Space Center's Corrosion Technology Lab at the Kennedy Space Center in Florida, U.S.A. has been developing multifunctional smart coatings based on the microencapsulation of environmentally friendly corrosion indicators, inhibitors and self-healing agents. This allows for the incorporation of autonomous corrosion control functionalities, such as corrosion detection and inhibition as well as the self-healing of mechanical damage, into coatings. This paper presents technical details on the characterization of inhibitor-containing particles and their corrosion inhibitive effects using electrochemical and mass loss methods. Three organic environmentally friendly corrosion inhibitors were encapsulated in organic microparticles that are compatible with desired coatings. The total inhibitor content and the release of one of the inhibitors from the microparticles in basic solution was measured. Particles with inhibitor contents of up 60 wt% were synthesized. Fast release, for immediate corrosion protection, as well as long-term release for continued protection, was observed. The inhibition efficacy of the inhibitors, both as the pure materials and in microparticles, on carbon steel was evaluated. Polarization curves and mass loss measurements showed that, in the case of 2MBT, its corrosion inhibition effectiveness was greater when it was delivered from microparticles.

Coatings↗
NASA NTRS2016

Corrosion-Activated Micro-Containers for Environmentally Friendly Corrosion Protective Coatings

This work concerns the development of environmentally friendly encapsulation technology, specifically designed to incorporate corrosion indicators, inhibitors, and self-healing agents into a coating, in such a way that the delivery of the indicators and inhibitors is triggered by the corrosion process, and the delivery of self-healing agents is triggered by mechanical damage to the coating. Encapsulation of the active corrosion control ingredients allows the incorporation of desired autonomous corrosion control functions such as: early corrosion detection, hidden corrosion detection, corrosion inhibition, and self-healing of mechanical damage into a coating. The technology offers the versatility needed to include one or several corrosion control functions into the same coating.The development of the encapsulation technology has progressed from the initial proof-of-concept work, in which a corrosion indicator was encapsulated into an oil-core (hydrophobic) microcapsule and shown to be delivered autonomously, under simulated corrosion conditions, to a sophisticated portfolio of micro carriers (organic, inorganic, and hybrid) that can be used to deliver a wide range of active corrosion ingredients at a rate that can be adjusted to offer immediate as well as long-term corrosion control. The micro carriers have been incorporated into different coating formulas to test and optimize the autonomous corrosion detection, inhibition, and self-healing functions of the coatings. This paper provides an overview of progress made to date and highlights recent technical developments, such as improved corrosion detection sensitivity, inhibitor test results in various types of coatings, and highly effective self-healing coatings based on green chemistry. The NASA Kennedy Space Centers Corrosion Technology Lab at the Kennedy Space Center in Florida, U.S.A. has been developing multifunctional smart coatings based on the microencapsulation of environmentally friendly corrosion indicators, inhibitors and self-healing agents. This allows the incorporation of autonomous corrosion control functionalities, such as corrosion detection and inhibition as well as the self-healing of mechanical damage, into coatings. This paper presents technical details on the characterization of inhibitor-containing particles and their corrosion inhibitive effects using electrochemical and mass loss methods.Three organic environmentally friendly corrosion inhibitors were encapsulated in organic microparticles that are compatible with desired coatings. The release of the inhibitors from the microparticles in basic solution was studied. Fast release, for immediate corrosion protection, as well as long-term release for continued protection, was observed.The inhibition efficacy of the inhibitors, incorporated directly and in microparticles, on carbon steel was evaluated. Polarization curves and mass loss measurements showed that, in the case of 2MBT, its corrosion inhibition effectiveness was greater when it was delivered from microparticles.

Corrosion Control↗
NASA NTRS1995

LDEF Interplanetary Dust Experiment (IDE) results

The Interplanetary Dust Experiment (IDE) provided high time resolution detection of microparticle impacts on the Long Duration Exposure Facility satellite. Particles, in the diameter range from 0.2 microns to several hundred microns, were detected impacting on six orthogonal surfaces of the gravity-gradient stabilized LDEF spacecraft. The total sensitive surface area was about one square meter, distributed between LDEF rows 3 (Wake or West), 6 (South), 9 (Ram or East), 12 (North), as well as the Space and Earth ends of LDEF. The time of each impact is known to an accuracy that corresponds to better than one degree in orbital longitude. Because LDEF was gravity-gradient stabilized and magnetically damped, the direction of the normal to each detector panel is precisely known for each impact. The 11 1/2 month tape-recorded data set represents the most extensive record gathered of the number, orbital location, and incidence direction for microparticle impacts in low Earth orbit. Perhaps the most striking result from IDE was the discovery that microparticle impacts, especially on the Ram, South, and North surfaces, were highly episodic. Most such impacts occurred in localized regions of the orbit for dozens or even hundreds of orbits in what we have termed Multiple Orbit Event Sequences (MOES). In addition, more than a dozen intense and short-lived 'spikes' were seen in which impact fluxes exceeded the background by several orders of magnitude. These events were distributed in a highly non-uniform fashion in time and terrestrial longitude and latitude.

Oliver, John P.↗
NASA NTRS2014

Ambulation Increases Decompression Sickness in Altitude Exposure

INTRODUCTION - Exercise accelerates inert gas elimination during oxygen breathing prior to decompression (prebreathe), but may also promote bubble formation and increase the risk of decompression sickness (DCS). The timing, pattern and intensity of exercise are likely critical to the net effect. The NASA Prebreathe Reduction Program (PRP) combined oxygen prebreathe and exercise preceding a 4.3 psi exposure in non-ambulatory subjects (a microgravity analog) to produce two protocols now used by astronauts preparing for extravehicular activity (CEVIS and ISLE). Additional work is required to investigate whether exercise normal to 1 G environments increases the risk of DCS over microgravity simulation. METHODS - The CEVIS protocol was replicated with one exception. Our subjects completed controlled ambulation (walking in place with fixed cadence and step height) during both preflight and at 4.3 psi instead of remaining non-ambulatory throughout. Decompression stress was graded with aural Doppler (Spencer 0-IV scale). Two-dimensional echocardiographic imaging was used to look for left heart gas emboli (the presence of which prompted test termination). Venous blood was collected at three points to correlate Doppler measures of decompression stress with microparticle (cell fragment) accumulation. Fisher Exact Tests compared test and control groups. Trial suspension would occur when DCS risk >15% or grade IV venous gas emboli (VGE) risk >20% (at 70% confidence). RESULTS - Eleven person-trials were completed (9 male, 2 female) when DCS prompted suspension. DCS was greater than in CEVIS trials (3/11 [27%] vs. 0/45 [0%], respectively, p=0.03). Statistical significance was not reached for peak grade IV VGE (2/11 [18%] vs. 3/45 [7%], p=0.149) or cumulative grade IV VGE observations per subject-trial (8/128 [6%] vs. 26/630 [4%], p=0.151). Microparticle data were collected for 5/11 trials (3 with DCS outcomes), with widely varying patterns that could not be resolved statistically. CONCLUSION - We did find that that ambulation increases decompression stress. Additional trials would improve the statistical power to assess differences in VGE and to evaluate the relationship between decompression stress and microparticles.

Conkin, Johnny↗
DOE OSTI2025

Microextraction-Single Particle-Inductively Coupled Plasma-Mass Spectrometry for the Direct Analysis of Nanoparticles on Surfaces

A novel employment of single particle-inductively coupled plasma-mass spectrometry (SP-ICP-MS) was developed, where a microextraction (ME) probe is used to sample nanoparticles from a surface and analyze them in a single analytical step. The effects of several parameters on the performance of ME-SP-ICP-MS were investigated, including the flow rate, choice of carrier solution, particle size, and the design of the microextraction probe head itself. The optimized ME-SP-ICP-MS technique was used to compare the extraction efficiency (EE, defined as the ratio of particles measured to particles deposited on the surface) of the commercial probe head to a newly designed SP polyether ether ketone (PEEK) probe head. The SP PEEK probe head was found to have increased EE compared to the commercial probe head (8.5 ± 3% vs 3.9 ± 3%, respectively). Increasing the carrier solution flow rate was found to decrease the total analysis time at the cost of decreasing EE. Extraction efficiencies for ME-SP-ICP-MS were typically 4–10%, which is similar to transport efficiencies (1–10%) for conventional SP-ICP-MS. Lastly, ME-SP-ICP-MS was employed for the analysis of nano- and microparticles. The sizes of gold nanoparticles, 30 ± 3 and 51 ± 1.9 nm (certified sizes), and iron-based microparticles, 1000 ± 50 nm (certified size), were accurately determined to be 32.2 ± 2.5, 50.8 ± 3.4, and 1030 ± 57 nm, respectively, by ME-SP-ICP-MS. Further, this work demonstrates the potential of ME-SP-ICP-MS for the direct analysis of particles on common collection surfaces (GSR tabs, carbon planchettes, etc.) while retaining spatial information on particle distribution across the surface.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Towards an understanding of particle-scale flaws and microstructure evolution in cold spray via accumulation of single particle impacts

Cold spray coatings are the sum of countless individual bonding events between single particles impacting on top of one another at high velocities. Thus, the collective behavior of microparticles must be considered to elucidate the origins of coating flaws at the scale of the particles and larger, or the dynamic evolution of the overall coating microstructure. Laser-induced particle impact testing (LIPIT) has been extensively used to study single-particle impacts, and in this work is adapted to study the accumulation of numerous particles with knowledge of each individual particle's impact parameters (particle size, velocity). The method reproducibly deposits stacks of gold particles (>20 particles) with different characteristic spectra of impact velocity. The observation of impact-induced erosion lets us define a critical velocity for material-build-up that is higher than that for single-particle bonding. The quantitative single-particle data are analyzed in a correlative manner to the structure and flaws in the resulting stacks, providing some first statistical connections between, e.g., strain and recrystallization, or aberrant particle characteristics and defects. The results highlight opportunities for the study of many-particle phenomena in microparticle impact—from interaction of particles in cold spray to multi-step erosion processes—with a quantitative view of the behavior of single particles.

Erosion↗
DOE OSTI2025

Operando X-ray imaging reveals size-dependent evolution of cobalt oxide thermochemical material during thermal redox cycles

Multivalent metal oxides are promising thermochemical materials (TCMs) for energy storage and conversion owing to their high energy density, air compatibility, and high-temperature stability. Co 3 O 4 serves as a model system for examining particle-size- and structure-dependent redox behavior. While particle size and porosity are known to affect performance, their interplay and the kinetics of pore formation during cycling remain unclear. Here we show the chemical and 3D morphological evolution of Co 3 O 4 micro- and nanoparticles during redox cycles at 800–900 °C using thermal analysis, in-situ synchrotron transmission X-ray microscopy (TXM), and scanning electron microscopy. Thermal analysis shows that nanoparticles re-oxidize more rapidly than microparticles at 800 °C. In-situ nanotomography and chemical imaging reveals that nanoparticles undergo redox conversion without forming internal pores, whereas microparticles develop isolated porosity during reduction. These pores persist through re-oxidation, correlating to a lower conversion rate in subsequent cycles. Our results demonstrate distinct degradation kinetics in Co 3 O 4 micro- and nanoparticles, underscoring the critical role of particle size and porosity in redox performance and informing strategies to enhance the long-term efficiency of metal oxide TCMs.

25 ENERGY STORAGE↗
DOE OSTI2026

Studies of laser stimulated photodetachment from nanoparticles for particle charge measurements

Determining nanoparticle charge is more challenging than that for microparticles due to change in the particle size during the synthesis substantial plasma property variations, and difficulties in visualizing individual particles, rendering conventional microparticle charge diagnostics ineffective in dusty plasma. In this work, we utilized laser-stimulated photodetachment (LSPD) to deduce the mean charge of nanoparticles. Nanoparticles were grown in an Ar/C 2 H 2 mixture using a capacitively coupled RF discharge and the LSPD induced changes in the electron current monitored by a cylindrical Langmuir probe. LSPD signals were obtained and analyzed across different dust growth phases. The prolonged decay of electron current pulses was attributed to the presence of residual negative ions, caused by the effective electrostatic trapping of these ions and the potential post—LSPD re-formation of new ones. The particle charge was estimated by combining the laser-stimulated photodetachment signal from the probe with the dust density obtained from laser-light extinction using the measured nanoparticle size distribution. For a nanoparticles size range of approximately 100–250 nm and mean diameter of $d$ p ∼154.37 nm, the effective mean charge was estimated to be $\langle$$Q$$\rangle$ d $≈$ 37 elementary charge units. The measured charge values are lower than those predicted by orbital motion limited theory, which may be attributed to significant electron depletion in the nanodusty plasma. LSPD results in Ar/C 2 H 2 nano-dusty plasma confirm the applicability of this method for estimating individual nanoparticle charges. However, it has also been demonstrated that electron detachment from residual background negative ions can influence the detachment current decay and must be carefully considered.

dust particle charge↗
NASA NTRS1974

Physics of sub-micron cosmic dust particles

Laboratory tests with simulated micrometeoroids to measure the heat transfer coefficient are discussed. Equations for ablation path length for electrically accelerated micrometeoroids entering a gas target are developed which yield guidelines for the laboratory measurement of the heat transfer coefficient. Test results are presented for lanthanum hexaboride (LaB sub 6) microparticles in air, argon, and oxygen targets. The tests indicate the heat transfer coefficient has a value of approximately 0.9 at 30 km/sec, and that it increases to approximately unity at 50 km/sec and above. Test results extend to over 100 km/sec. Results are also given for two types of small particle detectors. A solid state capacitor type detector was tested from 0.61 km/sec to 50 km/sec. An impact ionization type detector was tested from 1.0 to 150 km/sec using LaB sub 6 microparticles.

Roy, N. L.↗
NASA NTRS1975

Research investigation of the physical interactions and phenomena associated with hypervelocity sub-micron particles

Signals from impact ionization plasmas were studied as a means of performing microparticle composition analysis. Impact ionization signal response was measured in a time-of-flight (TOF) system for lanthanum hexaboride, carbonyl iron, and aluminum microparticle impacts on a tantalum target, primarily in the 1 - 8 km/s velocity range. Oscilloscope photographs of representative ion TOF signal response are given for each material studied. Graphs and histograms are presented of the total charge collected as well as the charge collected in each observed ion mass group. Data show that ion signals consist primarily of the lower ionization potential elements over the 1 - 8 km/s range.

Roy, N. L.↗
NASA NTRS1981

A model for protocellular coordination of nucleic acid and protein syntheses

The proteinoid model for the coordination of protein synthesis with nucleic acid coding within the evolving protocell is discussed. Evidence for the self-ordering of amino acid chains, which would enhance the catalytic activity of a lysine-rich proteinoid, is presented, along with that for the preferential formation of microparticles, particularly proteinoid microparticles, in various solutions. Demonstrations of the catalytic activity of lysine-rich proteinoids in the synthesis of peptide and internucleotide bonds are pointed out. The view of evolution as a two stage sequence in which the geological synthesis of peptides evolved to the protocellular synthesis of peptides and oligonucleotides is discussed, and contrasted with the alternative view, in accord with the central dogma, that nucleic acids arose first then governed the production of proteins and protocells.

Fox, S. W.↗
NASA NTRS1982

Heterogeneous atmospheric chemistry

The present conference on heterogeneous atmospheric chemistry considers such topics concerning clusters, particles and microparticles as common problems in nucleation and growth, chemical kinetics, and catalysis, chemical reactions with aerosols, electron beam studies of natural and anthropogenic microparticles, and structural studies employing molecular beam techniques, as well as such gas-solid interaction topics as photoassisted reactions, catalyzed photolysis, and heterogeneous catalysis. Also discussed are sulfur dioxide absorption, oxidation, and oxidation inhibition in falling drops, sulfur dioxide/water equilibria, the evidence for heterogeneous catalysis in the atmosphere, the importance of heterogeneous processes to tropospheric chemistry, soot-catalyzed atmospheric reactions, and the concentrations and mechanisms of formation of sulfate in the atmospheric boundary layer.

Schryer, D. R.↗