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DOE OSTI2020

Implications of Non-Bingham Rheology

One of the key challenges now facing the US Department of Energy (DOE) is the fate of radioactive waste remaining from World War II and the Cold War which is stored underground in tanks some 75 feet in diameter and over 30 feet tall. Over time, the waste has segmented into multiple layers with sludges and slurries at the bottom with salt crust layers often at the top and liquid in between. DOE’s current official baseline plans call for remaining sludges and slurries to be removed from the tanks and converted into a more stable glass waste form. Minimizing worker exposure to radiation drives DOE to use slurry processing techniques to suspend, mobilize, transport, mix, and process the waste. Therefore, a clear and quantitative understanding of Hanford waste rheology is essential for the success of the DOE mission. Historically much of the waste has been characterized using Eugene Bingham’s model more than a century old that provides a straight line fit to higher shear rate data with the intercept suggesting a yield stress and the slope providing the consistency. Yet, Bingham fits overestimate the shear stress at a given shear rate for low to intermediate shear rates, exactly the range of shear rates typically encountered in pipe flow, where shear rates peak along the pipe wall and vanish in the center. This model produces a fictitious yield stress for some of the wastes that do not exhibit yield phenomena. While over estimating the yield stress may be prudent, safe, and conservative for some applications (e.g., pump sizing to ensure that pumps can handle yield stresses), over estimating the rheology may be inaccurate and non-conservative for other applications (e.g., eroding settled particle beds). Therefore, this paper evaluates the slurry rheology of Hanford and Savannah River wastes using a more modern rheological model that fits the full range of experimental data. Although a bias has been recognized and alternative models proposed, the magnitude of this bias and the implications for tank waste have only been qualitatively suggested. The purpose of this paper is to evaluate quantitatively implications of the poor quality of fit between a Bingham model for rheology and experimental data at modest shear rates. We first demonstrate the magnitude of the bias between the data and the Bingham extrapolation. We then evaluate quantitatively the velocity profile under laminar conditions. This analysis shows that the bias may be large (hundreds of percent or more) at modest shear rates and that modest shear rates dominate pipe velocity profiles.

Rheology, Radioactive waste↗

DOE OSTI2023

Ice nucleation measurements from DRUM impactors during TRACER campaign in the Houston TX region from July to September 2022

During TRACER, three Davis Rotating Uniform size-cut Monitors (DRUM; DRUMAir 4-DRUM) were used to collect aerosols for ice nucleation measurements in the Brooks laboratory at Texas A&M University. The three instruments were located at AMF1 in La Porte, Ancillary site in Guy (ANC), and onboard the Texas A&M Rapid Onsite Atmospheric Measurements Van (ROAM-V). ROAM-V was deployed to capture airmasses behind (maritime) and ahead (continental) of the passage of the sea-breeze front through Houston. On select sampling days, ROAM-V sampled in the morning/mid-day on the coast and then transited to a second inland site for the afternoon/evening. The suite of instruments deployed on ROAM-V included a Condensation Particle Counter (CPC; GRIMM Model 5.403 CPC), Scanning Mobility Particle Sizer (SMPS; TSI 3750 detector, TSI 3082 classifier, TSI 3088 neutralizer, TSI 3081A Differential Mobility Analyzer), Cloud Condensation Nuclei counter (Droplet Measurement Technologies CCN Counter), micro pulse lidar (Droplet Measurement Technologies Micro Pulse LiDAR (miniMPL)), and one of the Davis Rotating Uniform size-cut Monitors (DRUM; DRUMAir 4-DRUM). Before sampling at each location, the latitude and longitude were recorded using the GPS on the phone application “My Altitude”. Each DRUM sampler was operated at a flow rate of 23 LPM. Each DRUM has four stages where the aerodynamic diameter size cuts are as follows: stage 1 larger than 3 μm, stage 2 from 3 to 1.2 μm, stage 3 from 1.2 to 0.34 μm, and stage 4 from 0.34 to 0.15 μm. Pretreated aluminum foil was used as a substrate on all stages. At AMF1 and ANC sites, the DRUMs were operated on the shared aerosol inlet, with generous support of the DOE ARM site staff. These instruments rotated 24 mm per day and only contained aluminum foil substrates. Substrates were changed weekly and transported to Texas A&M for storage in -80C freezer until analysis. The DRUM onboard ROAM-V was operated at a faster rotation rate of 150 mm per day to clearly separate the multiple deployment locations for ROAM-V. For the ROAM-V DRUM, substrates were changed every deployment and transported to Texas A&M for storage in -80C freezer until analysis. At Texas A&M, ice nucleation experiments were conducted to measure the ice nucleation temperature of the ambient aerosol samples collected from the three DRUMs using our previously established procedures (Alsante et al., 2023; Fornea et al., 2009; Matthews et al., 2023). For ice nucleation, only samples collected on stage 3 were analyzed, given that these are the most relevant size (1.2 to 0.34 μm diameter) for potential ice nucleating particles. For the AMF1 and ANC sites, we cut and analyzed 2 mm (2-hour) samples. We analyzed the time periods of the AMF1 site instrument when the ROAM-V was deployed. A 72-hour period from July 11th at 23:49 through July 15th at 1:49 was analyzed from the ANC site instrument. For the ROAM-V instrument, we separated the daily samples by site location. Between 1- and 6-hour independent samples were analyzed at each location. We also cut the ROAM-V samples in half to allow for compositional analysis of the aerosol on the other half of the substrate. All viable samples from the ROAM-V were analyzed. Analysis was done using a custom-built ice nucleation apparatus, recently updated to include an array of 16 individual samples (Matthews et al., 2023). On our experimental setup, we used 100 μL of Ultra-High-Performance Liquid Chromatography (UHPLC) water (Sigma Aldrich, >99.9% purity) to wash off the aerosol from the DRUM substrate. Then, we micropipetted 2 μL droplet samples into each of the 16 wells of the array, using hydrophobically coated microscope slides. Experiments would cycle 28 times from 10 C to -40C over a 20-hour period. During analysis of the TRACER samples, nine experiments were conducted with UHPLC water process blanks that followed an identical preparation procedure. The average freezing temperature and standard deviation for these process blanks is -27.7±2.4 C. This data was collected for ARM Field Campaign AFC07023 and supported by DOE ASR grant DE-SC0021047. For any further questions, please feel free to contact the instrument PI, Sarah D. Brooks, sbrooks@tamu.edu. Alsante, A. N., Thornton, D. C., & Brooks, S. D. (2023). Ice nucleation catalyzed by the photosynthesis enzyme RuBisCO and other abundant biomolecules. Communications Earth & Environment, 4(1), 51. Fornea, A. P., Brooks, S. D., Dooley, J. B., & Saha, A. (2009). Heterogeneous freezing of ice on atmospheric aerosols containing ash, soot, and soil. Journal of Geophysical Research: Atmospheres, 114(D13). DOI:10.1029/2009JD011958 Matthews, B. H., Alsante, A. N., & Brooks, S. D. (2023). Pollen Emissions of Subpollen Particles and Ice Nucleating Particles. ACS Earth and Space Chemistry.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS2018

Nanomanufacturing of Graphene Nanosheets Through Hole Engineering

Facile and scalable fabrication of highly dense and high quality graphene films and articles is extremely attractive for a range of electronic and mechanical applications. Pristine, high quality graphene with its inherent impermeability poses challenges in fabricating dense films and thick parts with high electrical conductivity due to the difficulty in removing trapped air and/or solvents used in various fabrication methods. To overcome this deficiency, nano-holes were intentionally created in pristine graphene (“holey graphene”) with an average diameter of approximately 15 nm. The holes serve as pathways for the rapid removal of gases or liquids and enable the fabrication of dense holey graphene nanostructures. Subsequently, a high temperature process is applied to effectively repair the nano-holes and recover the high quality graphene conjugated network. Through the creation and repair of the nano-holes, dense graphene articles were created that exhibited an ultrahigh conductivity of 2209 S/cm and a high carrier mobility of 673 cm2V-1s-1. This unique processing methodology enables the facile and scalable fabrication of high quality graphene constructs for a variety of applications.

Yanan Chen↗

NASA NTRS2003

Small, Untethered, Mobile Robots for Inspecting Gas Pipes

Small, untethered mobile robots denoted gas-pipe explorers (GPEXs) have been proposed for inspecting the interiors of pipes used in the local distribution natural gas. The United States has network of gas-distribution pipes with a total length of approximately 109 m. These pipes are often made of iron and steel and some are more than 100 years old. As this network ages, there is a need to locate weaknesses that necessitate repair and/or preventive maintenance. The most common weaknesses are leaks and reductions in thickness, which are caused mostly by chemical reactions between the iron in the pipes and various substances in soil and groundwater. At present, mobile robots called pigs are used to inspect and clean the interiors of gas-transmission pipelines. Some carry magnetic-flux-leakage (MFL) sensors for measuring average wall thicknesses, some capture images, and some measure sizes and physical conditions. The operating ranges of pigs are limited to fairly straight sections of wide transmission- type (as distinguished from distribution- type) pipes: pigs are too large to negotiate such obstacles as bends with radii comparable to or smaller than pipe diameters, intrusions of other pipes at branch connections, and reductions in diameter at valves and meters. The GPEXs would be smaller and would be able to negotiate sharp bends and other obstacles that typically occur in gas-distribution pipes.

Wilcox, Brian↗

DOE OSTI2023

SMPS data from TAMU TRACER campaign in the Houston TX region from July to September 2022

During TRACER, the Texas A&M Rapid Onsite Atmospheric Measurements Van (ROAM-V) was deployed to capture airmasses behind (maritime) and ahead (continental) of the passage of the sea-breeze front through Houston. On select sampling days, ROAM-V sampled in the morning/mid-day on the coast and then transited to a second inland site for the afternoon/evening. The suite of instruments deployed on ROAM-V included a Condensation Particle Counter (CPC; GRIMM Model 5.403 CPC), Scanning Mobility Particle Sizer (SMPS; TSI 3750 detector, TSI 3082 classifier, TSI 3088 neutralizer, TSI 3081A Differential Mobility Analyzer), Cloud Condensation Nuclei counter (Droplet Measurement Technologies CCN Counter), micro pulse lidar (Droplet Measurement Technologies Micro Pulse LiDAR (miniMPL)), and a Davis Rotating Uniform size-cut Monitor (DRUM; DRUMAir 4-DRUM). Before sampling at each location, the latitude and longitude were recorded using the GPS on the phone application “My Altitude”. Onboard the ROAM-V, aerosol samples are drawn through a shared isokinetic inlet at a flow rate ranging from 3.5 to 7.0 LPM. A portion of this flow, 1.0 LPM, is directed through TSI's 0.071 cm impactor attached to the classifier of the SMPS setup. The SMPS’s DMA and CPC are connected through a 20.3 cm length of 0.48 cm diameter tubing. Measured SMPS size distributions were used to calculate size-dependent particle losses for each SMPS scan. Particle losses from diffusion (based on Kesten, 1991 and Gormley, 1949) and inertial impaction in 90-degree bends (based on Aerosol Measurement, 2011 and Crane, 1977) were included in the loss calculation. This data was collected for ARM Field Campaign AFC07055 and supported by DOE ASR grant DE-SC0021047. For any further questions, please feel free to contact the instrument PI, Sarah D. Brooks, sbrooks@tamu.edu. Kesten et. al. Calibration of a TSI Model 3025 Ultrafine Condensation Particle Counter. Aerosol Science and Technology, 15:2, 107-111, 1991. Gormley et. al. Diffusion from a Stream Flowing through a Cylindrical Tube. Proceedings of the Royal Irish Academy, Vol 52, 163-169, 1948. Aerosol Measurement: Principles, Techniques, and Applications, Third Edition. John Wiley & Sons, Inc, 2011. Crane et. al. Inertial Deposition of Particles in a Bent Pipe. Journal of Aerosol Science, Vol 8, 161-170, 1977.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2023

Enabling Structure/Interface Regulation for High Performance Ni-Rich Cathodes

Here, further commercialization of Ni-rich layered cathodes is hindered by severe structure/interface degradation and kinetic hindrance that occur during electrochemical operation, which leads to safety risks and reduced range in electric vehicles (EVs). Herein, by selecting elements with different solubility properties, a multifunctional strategy that synchronously fabricates perovskite-type SrZrO 3 coating and Sr/Zr co-doping is employed to strengthen the structure/interface stability and the Li + transport mobility of LiNi 0.85 Co 0.10 Mn 0.05 O 2 (NCM). Perovskite-type SrZrO 3 protective layers formed on the particle surface can substantially mitigate the unexpected interfacial side reactions and surface phase transitions. In addition, a robust crystal framework is constructed by optimizing local O coordination through the introduction of strong Zr-O bonds. Notably, Li + diffusion kinetics is effectively improved due to expanded cell parameters and O-Li-O slab spacing with the incorporation of large-diameter Sr pillar ions, as revealed by X-ray diffraction. As a result, the Sr/Zr-modified NCM achieves a remarkable capacity retention of 99.4% after 200 cycles at 1 C, and a high rate capacity of 168.9 mAh g -1 at 10 C. This work opens new avenues to develop high-performance NCM cathodes with high energy and high power for EVs with long calendar life.

25 ENERGY STORAGE↗

NASA NTRS2002

WOBBLE: A Proposed Mission to Characterize Past and Present Water on Mars

WOBBLE ("Water Observations from a Balloon Borne Light Explorer") is a mission concept study for a small robotic probe to explore Mars and to accomplish a scientific mission compatible with the goals of the NASA Code S enterprise. The detection of past or present water is a crucial goal for Mars exploration, representing a cross-cutting science theme relevant to past or extant life, climate history, sample return missions and eventual human exploration. The WOBBLE mission concept was developed to study evidence of water using in-situ detection methods. The features on Mars most suited to this investigation are the gullies identified by Malin and Edgett as evidence for recent, near-surface runoff of liquid water. These features are typically located on the inside face of crater rims, where the local slope angle is at or near the angle of repose. This makes the terrain difficult or impossible to access with conventional wheeled rover technology. Combined with the small size of the gullies in relation to a standard landing error ellipse, scientific investigation of these features requires a new approach to surface mobility. WOBBLE uses a low-altitude balloon-borne platform to traverse the surface from the landing site, to the investigation site, and then rise up the slope to investigate the regions of interest at close range. Of the mobility technologies available for near-term Mars exploration, only a balloon platform is capable of a well targeted, detailed sampling of the gully regions over periods of days or more. The science approach embodied in WOBBLE is two-pronged, designed to investigate both the historical evidence of liquid water utilizing high-resolution geomorphology and the characterization of mineral deposits, and present subsurface liquid water using radar sounding techniques. The WOBBLE balloon is a high-pressure hydrogen gas design, 24 meters in diameter and lifting a total payload of 130 kg, including a high-resolution camera/IR imager, Raman spectrometer, and a ground penetrating radar (GPR) sounder. The stowed balloon and payload are designed to fit within the current airbag delivery system being built for the Mars Exploration Rovers. Characterization of local meteorological conditions and wind is made over the initial sols following landing and before balloon inflation. Following balloon inflation and launch, a controlled, targeted approach toward the identified regions of interest is made in a series of several low-altitude "hops," with the balloon tethered to the ground between the hop intervals. A "snake" system is used to control the altitude to a few tens of meters above the local ground level. Enroute to the target gully, GPR soundings and Raman spectroscopy measurements study past or present water, while continued camera bearings and meteorological measurements refine the next "hop" trajectory. Once at the gully/outflow region, GPR and Raman soundings continue while the camera obtains detailed, approx. 0.5 cm images for geomorphology studies. The WOBBLE concept is applicable to Mars Scout, Mars Surveyor, or Discovery class missions.

Udrea, Bogdan↗

NASA NTRS1980

Topographic domes on Ganymede - Ice vulcanism or isostatic upwarping

Two formation processes are considered for two gently sloping domeshaped features on the surface of Ganymede, lying on grooved terrain and having diameters of roughly 250 km: (1) water vulcanism, triggered by a major impact, and (2) the isostatic upwarping of a crater formed in a thin crust. Numerical simulations show the volume of the domes to be consistent with eruption through fractures created by an impact that excavates partly through a thin crust. Isostatic upwarp rates calculated as a function of effective crustal temperature indicate that upwarping could also create such a dome if the impact excavated to a depth where the crust was sufficiently warm and mobile. Morphologic evidence suggests that both processes may have been important and, if either of the proposed models is correct, it is strongly implied that grooved terrain formation occurred prior to the thickening and stiffening of Ganymede's crust.

Squyres, S. W.↗

DOE OSTI2020

Chain flexibility and glass transition temperatures of poly(n-alkyl (meth)acrylate)s: Implications of tacticity and chain dynamics

The relationship between chain microstructure and glass transition temperature (T g ) is complicated for poly(alkyl methacrylate)s and poly(alkyl acrylate)s. Despite intensive studies, relationships between the structures of these polymers and their properties, including solution characteristics and T g , are still controversial. Solution properties, chain conformations, including Flory's characteristic ratio (C ∞ ), persistence length (l p ), and chain diameters, and T g are reported for series of poly(n-alkyl acrylate)s and poly(n-alkyl methacrylate)s having alkyl side chain lengths (n) ranging from 1 to 10 carbons in length, with uniform and well-characterized tacticities. Chain flexibilities of both series of polymers decrease as n increases, reflecting increased hindrances to rotation about backbone bonds as side chains become longer. Conversely, the T g s for both series of polymers decrease substantially as n increases, reflecting the greater side chain mobilities of long alkyl substituents. For shorter alkyl chain lengths, T g s for the poly(n-alkyl acrylate)s are much lower than for the corresponding poly(n-alkyl methacrylate)s, a difference which has been attributed in the past to the presumed reduced chain flexibility of polymethacrylates due to the presence of the α-methyl substituent. However, contrary to such expectations, C ∞ and l p values for these two series of polymers are nearly identical at a given n value, except for the longest n-alkyl substituents. Instead, the differences in T g may be attributed to the differences in tacticity of the two series – almost ideally atactic for the poly(n-alkyl acrylate)s but high in syndiotacticity for the poly(n-alkyl methacrylate)s. The T g s for the two series of polymers approach that of polyethylene at longer alkyl chain lengths. In addition, the effects of tacticity and chain dynamics on C ∞ , l p , and T g of poly(methyl methacrylate) is discussed.

36 MATERIALS SCIENCE↗

NASA NTRS2012

Demonstrations of Gravity-Independent Mobility and Drilling on Natural Rock using Microspines

The video presents microspine-based anchors be ing developed for gripping rocks on the surfaces of comets and asteroids, or for use on cliff faces and lava tubes on Mars. Two types of anchor prototypes are shown on supporting forces in all directions away from the rock; >160 N tangent, >150 N at 45?, and >180 N normal to the surface of the rock. A compliant robotic ankle with two active degrees of freedom interfaces these anchors to the Lemur IIB robot for future climbing trials. Finally, a rotary percussive drill is shown coring into rock regardless of gravitational orientation. As a harder- than-zero-g proof of concept, inverted drilling was performed creating 20mm diameter boreholes 83 mm deep in vesicular basalt samples while retaining 12 mm diameter rock cores in 3-6 pieces.

microspine anchors↗

NASA NTRS2005

A New Vehicle for Planetary Surface Exploration: The Mars Tumbleweed

The surface of Mars is currently being explored with a combination of orbiting spacecraft, stationary landers and wheeled rovers. However, only a small portion of the Martian surface has undergone in-situ examination. Landing sites must be chosen to insure the safety of the vehicles (and human explorers) and provide the greatest opportunity for mission success. While wheeled rovers provide the ability to move beyond the landing sites, they are also limited in their ability to traverse rough terrain; therefore, many scientifically interesting sites are inaccessible by current vehicles. In order to access these sites, a capability is needed that can transport scientific instruments across varied Martian terrain. A new "rover" concept for exploring the Martian surface, known as the Mars Tumbleweed, will derive mobility through use of the surface winds on Mars, much like the Tumbleweed plant does here on Earth. Using the winds on Mars, a Tumbleweed rover could conceivably travel great distances and cover broad areas of the planetary surface. Tumbleweed vehicles would be designed to withstand repeated bouncing and rolling on the rock covered Martian surface and may be durable enough to explore areas on Mars such as gullies and canyons that are currently inaccessible by conventional rovers. Achieving Mars wind-driven mobility; however, is not a minor task. The density of the atmosphere on Mars is approximately 60-80 times less than that on Earth and wind speeds are typically around 2-5 m/s during the day, with periodic winds of 10 m/s to 20 m/s (in excess of 25 m/s during seasonal dust storms). However, because of the Martian atmosphere#s low density, even the strongest winds on Mars equate to only a gentle breeze on Earth. Tumbleweed rovers therefore need to be relatively large (4-6 m in diameter), very lightweight (10-20 kg), and equipped with lightweight, low-power instruments. This paper provides an overview of the Tumbleweed concept, presents several notional design concepts, mission scenarios, and highlights recent tests and analyses of Tumbleweed prototypes.

Antol, Jeffrey↗

NASA NTRS2005

Mars Orbiter Sample Return Power Design

Mars has greatly intrigued scientists and the general public for many years because, of all the planets, its environment is most like Earth's. Many scientists believe that Mars once had running water, although surface water is gone today. The planet is very cold with a very thin atmosphere consisting mainly of CO2. Mariner 4, 6, and 7 explored the planet in flybys in the 1960s and by the orbiting Mariner 9 in 1971. NASA then mounted the ambitious Viking mission, which launched two orbiters and two landers to the planet in 1975. The landers found ambiguous evidence of life. Mars Pathfinder landed on the planet on July 4, 1997, delivering a mobile robot rover that demonstrated exploration of the local surface environment. Mars Global Surveyor is creating a highest-resolution map of the planet's surface. These prior and current missions to Mars have paved the way for a complex Mars Sample Return mission planned for 2003 and 2005. Returning surface samples from Mars will necessitate retrieval of material from Mars orbit. Sample mass and orbit are restricted to the launch capability of the Mars Ascent Vehicle. A small sample canister having a mass less than 4 kg and diameter of less than 16 cm will spend from three to seven years in a 600 km orbit waiting for retrieval by a second spacecraft consisting of an orbiter equipped with a sample canister retrieval system, and a Earth Entry Vehicle. To allow rapid detection of the on-orbit canister, rendezvous, and collection of the samples, the canister will have a tracking beacon powered by a surface mounted solar array. The canister must communicate using RF transmission with the recovery vehicle that will be coming in 2006 or 2009 to retrieve the canister. This paper considers the aspect and conclusion that went into the design of the power system that achieves the maximum power with the minimum risk. The power output for the spherical orbiting canister was modeled and plotted in various views of the orbit by the Satellite Orbit Analysis Program (SOAP).

Mardesich, N.↗

NASA NTRS1993

Magnetite-sulfide chondrules and nodules in CK carbonaceous chondrites - Implications for the timing of CK oxidation

CK carbonaceous chondrites contain rare (about 0.1 vol pct) magnetite-sulfide chondrules that range from about 240 to 500 microns in apparent diameter and have ellipsoidal to spheroidal morphologies, granular textures, and concentric layering. They resemble the magnetite-sulfide nodules occurring inside mafic silicate chondrules in CK chondrites. It seems likely that the magnetite-sulfide chondrules constitute the subset of magnetite-sulfide nodules that escaped as immiscible droplets from their molten silicate chondrule hosts during chondrule formation. The intactness of the magnetite-sulfide chondrules and nodules implies that oxidation of CK metal occurred before agglomeration. Hence, the pervasive silicate darkening of CK chondrites was caused by the shock mobilization of magnetite and sulfide, not metallic Fe-Ni and sulfide as in shock-darkened ordinary chondrites.

Rubin, Alan E.↗

NASA NTRS1993

Lunar surface operations. Volume 1: Lunar surface emergency shelter

The lunar surface emergency shelter (LSES) is designed to provide survival-level accommodations for up to four astronauts for a maximum of five days. It would be used by astronauts who were caught out in the open during a large solar event. The habitable section consists of an aluminum pressure shell with an inner diameter of 6 ft. and a length of 12.2 ft. Access is through a 4 in. thick aluminum airlock door mounted at the rear of the shelter. Shielding is provided by a 14.9 in. thick layer of lunar regolith contained within a second, outer aluminum shell. This provides protection against a 200 MeV event, based on a 15 REM maximum dose. The shelter is self-contained with a maximum range of 1000 km. Power is supplied by a primary fuel cell which occupies 70.7 cu ft. of the interior volume. Mobility is achieved by towing the shelter behind existing lunar vehicles. It was assumed that a fully operational, independent lunar base was available to provide communication support and tools for set-up and maintenance. Transportation to the moon would be provided by the proposed heavy lift launch vehicle. Major design considerations for the LSES were safety, reliability, and minimal use of earth materials.

Shields, William↗

DOE OSTI2021

Material migration in W and Mo during bubble growth and fuzz formation

Growth of helium (He) induced bubbles and fuzz in tungsten (W) and molybdenum (Mo) is investigated using samples of W films on Mo substrates and Mo films on W substrates exposed to He-containing plasma in the temperature range of 340 to 1075 K, fluence range of 1.0–14 × 10 25 He·m -2 , and incident ion energy of <50 eV. No fuzz (only up to 2 nm diameter bubbles) and no material transport occur in W films at ≤750 K, while precursors-of or fully-developed fuzz and material mixing occur in W and Mo films at ≥800 K. This suggests that fuzz forms in multi-material systems as long as one material meets the conditions for fuzz formation, namely T s / T m ~ 0.27–0.5 where T s and T m are the sample exposure and material melting temperatures, respectively. Larger He bubbles, more material mixing, and further-developed fuzz occur at higher temperature due to increased mobility of He atoms and small He clusters. Accumulation of substrate material at the surface of fuzzy W and Mo thin-film (<80 nm) samples suggests fuzz growth by material transport from the bubble layer in the bulk up to the fiber tip, likely by a two-step process: (i) diffusion of punched dislocation loops in the bulk toward the fuzz base and (ii) diffusion of adatoms along the fuzz base and fiber surface (with effective transport of adatoms upwards due to trapping of adatoms at curved surfaces of fiber tips and/or due to the continuous generation of adatoms at the fuzz base). While the bubble size and fuzz thickness increase with reduced W concentration in Mo thin-film samples at 838 K likely due to an increase in trap mutation and dislocation loop punching in Mo compared to W, the fuzz thickness decreases with reduced W concentration at 1075 K despite an increase in the bubble size likely due to slower diffusion of interstitial loops in Mo.

Physics↗

NASA NTRS1985

Synthesis of ceramic powders and surface films from laser heated gases

Two new processes have been developed that are based on laser-heated gases. Both permit unusually precise levels of process control and, thereby, materials having superior properties. The power process yields Si, Si3N4 and SiC powders that are uniform in size, nonagglomerated, small diameter, spherically shaped and high purity. Manufacturing cost analyses show that submicron powders can be made with an energy cost of approximately 2 kWhr/kg and a dollar cost of 2-3.30 $/kg, exclusive of the costs of feed materials. The laser-induced chemical vapor deposition process (LICVD) causes reactant gases to be heated by absorbing IR light from a laser beam that passes parallel to the substrate surface. Laser heating permits independent control of gas and substrate temperatures while operating in a conventional, thermally activated chemical vapor deposition mode. Spin density, hydrogen content, electrical conductivity and mobility gap properties show the LICVD process capable of producing very high quality films.

Haggerty, J. S.↗

NASA NTRS1999

MRI Measurements and Granular Dynamics Simulation of Segregation of Granular Mixture

A counter intuitive axial segregation phenomenon in a rotating horizontal cylinder has recently captured attention of many researchers in different disciplines. There is a growing consensus that the interplay between the particle dynamics and the evolution of the internal structure during the segregation process must be carefully investigated. Magnetic resonance imaging (MRI) has been used to non-invasively obtain much needed dynamic/static information such as velocity and concentration profiles, and it has proven to be capable of depicting the evolution of segregation processes. Segregation in a rotating cylinder involves two processes: the first is to transport small particles in the radial direction to form a radial core, and the second is to transform the radial core into axially segregated bands. Percolation and/or "stopping" have been proposed as mechanisms for the radial segregation. As to mechanisms for axial band formation, much less is known. The difference in the dynamic angle of repose has been proposed to segregate different components in the axial direction. Recently, Hill and Kakalios have reported that particles mix or demix depending upon the competition between diffusion and preferential drift whose order can be determined by the dynamic angle of repose through the adjustment of the rotation rate. We claim that the dynamic angle of repose could be one of the causes, however, it fails to offer reasonable explanations for certain aspects of the axial migration. For example, we always observe that the radial segregation precedes the axial segregation and small particles migrate in the radial direction to form an axially extended radial core. It then transforms into axially segregated bands. By definition, the effects of the dynamic angle of repose are restricted near the free surface where the flowing layer is present. However, during the process of transforming from the radially segregated core to axially segregated bands, small particles located in the deep core region, which is untouched by the flowing layer, also completely disappear. Usually, the dynamics angle of repose are uniquely defined for individual species to characterize particle properties, and the dynamic angle of repose thus defined provides little information for the dynamic angle of repose of the mixture since the concentration ratio and the internal packing structure do not remain the same during the segregation processes. Under microgravity environment, the dynamics angle of repose argument does not hold since there is simply no flowing layer to influence/determine the preferred directions of segregation. We have thus designed an experiment so that the effects of the dynamic angle of repose can be minimized by filling the cylinder almost completely full. Small particles still formed a radial core and also migrated to form axial bands. As ground based experiments we have designed and conducted both 2D and 3D segregation experiments. The 2D experiments are performed using a thin cylinder (the gap between two end caps is about 5 mm) filled with different combinations of particles. The 3D experiments are conducted with a long cylinder of its length and diameter of 27cm and 7cm, respectively. Results of 2D experiments indicate that different mechanisms govern particle motion in regions near and far from the axis of rotation. Results of 3D experiments indicate that a series of collapses of microstructures of particle packing (micro-collapses) may be responsible for the creation of voids for small particles to migrate through in the axial direction. We have successfully eliminated the dynamic angle of repose as a cause for segregation, however, by almost completely filling the cylinder with the particles, we have lost an opportunity to investigate a possibility of particle "mobility" being a cause for segregation which requires a flowing surface but not the difference in the angle of repose. This is currently being investigated.

Nakagawa, M.↗

DOE OSTI2020

A micromirror array with annular partitioning for high-speed random-access axial focusing

Dynamic axial focusing functionality has recently experienced widespread incorporation in microscopy, augmented/virtual reality (AR/VR), adaptive optics and material processing. However, the limitations of existing varifocal tools continue to beset the performance capabilities and operating overhead of the optical systems that mobilize such functionality. The varifocal tools that are the least burdensome to operate (e.g. liquid crystal, elastomeric or optofluidic lenses) suffer from low (≈100 Hz) refresh rates. Conversely, the fastest devices sacrifice either critical capabilities such as their dwelling capacity (e.g. acoustic gradient lenses or monolithic micromechanical mirrors) or low operating overhead (e.g. deformable mirrors). Here, we present a general-purpose random-access axial focusing device that bridges these previously conflicting features of high speed, dwelling capacity and lightweight drive by employing low-rigidity micromirrors that exploit the robustness of defocusing phase profiles. Geometrically, the device consists of an 8.2 mm diameter array of piston-motion and 48-μm-pitch micromirror pixels that provide 2π phase shifting for wavelengths shorter than 1100 nm with 10–90% settling in 64.8 μs (i.e., 15.44 kHz refresh rate). The pixels are electrically partitioned into 32 rings for a driving scheme that enables phase-wrapped operation with circular symmetry and requires <30 V per channel. Optical experiments demonstrated the array’s wide focusing range with a measured ability to target 29 distinct resolvable depth planes. Overall, the features of the proposed array offer the potential for compact, straightforward methods of tackling bottlenecked applications, including high-throughput single-cell targeting in neurobiology and the delivery of dense 3D visual information in AR/VR.

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