General Synthetic Strategy to Ordered Mesoporous Carbon Catalysts with Single-Atom Metal Sites for E
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Luo, Zhicheng↗
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The diversity of aluminum-based drinking water treatment residuals for use in environmental remediation
Drinking water treatment residuals (DWTRs) are complex mixtures of organic and inorganic phases generally disposed of as waste materials. However, their strong sorptive properties could be further exploited to immobilize contaminants. To characterize these materials, we applied a range of analytical techniques to a set of aluminum-based DWTRs. Here we determined surface areas, elemental compositions using CHNS analysis and X-ray fluorescence (XRF), performed thermogravimetric analyses paired with mass spectrometry (TGA-MS), and used synchrotron-based methods: X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS). Elemental analyses and specific surface area measurements – that vary between 7.23 ± 0.03 and 197.6 ± 0.9 m 2 g –1 – indicate that non-coagulant additives must play an important role in controlling sorption. High resolution powder XRD reveals the presence of only a few crystalline minerals mostly derived from source waters or additives. Fe was detected by XRF in all samples, whereas Mn was present in significant levels in samples with potassium permanganate as additive. The chemical speciation of these elements was characterized by performing spectral decompositions of XAS spectra. The spectral features of Fe are consistent with iron(III) oxides/hydroxides and structural iron in clays. On the other hand, Mn is predominantly present under its reduced form, Mn(II).
54 ENVIRONMENTAL SCIENCES↗
Oxygen electrodes for rechargeable alkaline fuel cells
Electrocatalysts and supports for the positive electrode of moderate temperature single unit rechargeable alkaline fuel cells were investigated and developed. The electrocatalysts are defined as the material with a higher activity for the oxygen electrode reaction than the support. Advanced development will require that the materials be prepared in high surface area forms, and may also entail integration of various candidate materials. Eight candidate support materials and seven electrocatalysts were investigated. Of the 8 support, 3 materials meet the preliminary requirements in terms of electrical conductivity and stability. Emphasis is now on preparing in high surface area form and testing under more severe corrosion stress conditions. Of the 7 electrocatalysts prepared and evaluated, at least 5 materials remain as potential candidates. The major emphasis remains on preparation, physical characterization and electrochemical performance testing.
Swette, Larry↗
Changes in the distribution of plastids and endoplasmic reticulum during cellular differentiation in root caps of Zea mays
In calyptrogen cells of Zea mays, proplastids are distributed randomly throughout the cell, and the endoplasmic reticulum (ER) is distributed parallel to the cell walls. The differentiation of calyptrogen cells into columella statocytes is characterized by the following sequential events: (1) formation of ER complexes at the distal and proximal ends of the cell, (2) differentiation of proplastids into amyloplasts, (3) sedimentation of amyloplasts onto the distal ER complex, (4) breakdown of the distal ER complex and sedimentation of amyloplasts to the bottom of the cell, and (5) formation of sheets of ER parallel to the longitudinal cell walls. Columella statocytes located in the centre of the cap each possess 4530 +/- 780 micrometers2 of ER surface area, an increase of 670 per cent over that of calyptrogen cells. The differentiation of peripheral cells correlates positively with (1) the ER becoming arranged in concentric sheets, (2) amyloplasts and ER becoming randomly distributed, and (3) a 280 per cent increase in ER surface area over that of columella statocytes. These results are discussed relative to graviperception and mucilage secretion, which are functions of columella and peripheral cells, respectively.
NASA Discipline Number 40-10↗
Modeling the Exo-Brake and the Development of Strategies for De-Orbit Drag Modulation
The Exo-Brake is a simple, non-propulsive means of de-orbiting small payloads from orbital platforms such as the International Space Station (ISS). Two de-orbiting experiments with fixed surface area Exo-Brakes have been successfully conducted in the last two years on the TechEdSat-3 and -4 nano-satellite missions. The development of the free molecular flow aerodynamic data-base is presented in terms of angle of attack, projected front surface area variation, and altitude. Altitudes are considered ranging from the 400km ISS jettison altitude to 90km. Trajectory tools are then used to predict de-orbit/entry corridors with the inclusion of the key atmospheric and geomagnetic uncertainties. Control system strategies are discussed which will be applied to the next two planned TechEdSat-5 and -6 nano-satellite missions - thus increasing the targeting accuracy at the Von Karman altitude through the proposed drag modulation technique.
Exo-Brake↗
Synthesis of multicomponent oxygen evolution reaction coatings via block copolymer templating with vapor- and solution-phase precursors
Porous mixed transition metal oxide heterostructures are promising electrocatalysts due to their high surface area. However, achieving conformal multicomponent oxide coatings with controlled nanoscale architectures remains challenging. Here, we report a synthesis strategy that integrates solution-based swelling infiltration (SBI) with gas-phase sequential infiltration synthesis (SIS) in a block copolymer template to fabricate porous, high-surface-area, conformal mixed-oxide electrocatalytic coatings. In this approach, a PS75-P4VP25 block copolymer (BCP) film is first infiltrated with transition metal acetylacetonate precursors via SBI, followed by exposure to gas phase precursors of ZnO via SIS process. Thermal annealing of the infiltrated BCP films converts them into all-inorganic Fe–ZnO, Fe–Co–ZnO, and Fe–Ni–ZnO coatings. Electrochemical testing on 70 nm thick conformal coatings demonstrates promising oxygen evolution reaction (OER) activity in alkaline media, with mass-specific current densities up to 1.0 × 10 5 mA/g at an overpotential of 330 mV (vs. RHE) at ultralow loading (~0.005 g/cm 2 ). Among the compositions, Fe–Co–ZnO and amorphous Fe–Ni–ZnO show the best OER performance, delivering current densities of 2.00 and 3.04 mA/cm 2 , respectively, compared to 1.52 mA/cm 2 for Fe–ZnO.. This work establishes SBI–SIS as a versatile route for fabricating nm-thin, high-performance multicomponent oxide heterostructures on cost-efficient supports, enabling efficient catalyst utilization in electrochemical energy conversion application.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Understanding Pore Formation in ALD Alumina Overcoats
AlO X thin films deposited by atomic layer deposition (ALD) have previously been used to increase both stability and selectivity of supported palladium catalysts and are known to develop nanoscale porosity upon heating. Furthermore, understanding the factors that affect ALD thin film porosity would enable future design of layered catalytic structures with tunable nanoscale features on industrially relevant high surface area materials. In this study, porous and nonporous aluminum oxide supports with and without palladium nanoparticles were overcoated with thin films of 2 - 7 nm AlO X by ALD deposited at temperatures of 100 °C, 200 °C and 300 °C. Hydroxyl loss and changes in surface chemistry were observed upon heating the films, and changes in surface area and pore volume of the annealed films were correlated to AlO x deposition temperature and presence of Pd. Crystallization of the overcoat to γ-Al 2 O 3 is shown to occur separately from hydroxyl loss and pore formation. A mechanistic understanding of pore formation in AlO X ALD films is obtained by reference to studies of the structural transformations accompanying the formation of transition aluminas from hydroxide precursors. Additionally, a direct and tunable correlation is established between pore development and the overall hydroxyl content of AlO X ALD coatings.
36 MATERIALS SCIENCE↗
Performance of Several Method-of-Characteristics Exhaust Nozzles
Nozzle performance data were obtained with three "method-of-characteristics" nozzles and a 150 conical nozzle at pressure ratios up to 130. Each basic configuration was cut off and tested at expansion ratios of 25, 20, 15, and 10. Unheated dry air was used at nozzle inlet pressures up to 22,000 pounds per square foot absolute. Nozzle thrust data were extrapolated to infinite pressure ratio (zero discharge pressure). As much as 1-percent increase in thrust with no increase in nozzle surface area (weight), can be obtained by using a method-of-characteristics, nozzle instead of a 15 conical nozzle when operating with a nozzle expansion ratio of 25 and nozzle pressure ratios from 200 to infinity. Conversely, for the same thrust, reductions in nozzle divergent surface area in the order of 25 percent are possible. The thrust performance of the method-of-characteristics nozzle was not as good as that of the 150 conical nozzle when operating at pressure ratios considerably below design (below 100 for the expansion ratio 25 nozzles). Theoretical and measured nozzle momentum coefficients agreed within about 0.6 percent. This is the order of accuracy of both the measured and theoretical values.
Farley, John M.↗
Optimizing Surfactant Templating of Yttria-stabilized Zirconia Aerogels for High-temperature Applications: Effect of Anionic & Nonionic Surfactant
Aerogels are useful thermal insulators due to low density, low thermal conductivity, and a tortuous path for solid conduction. However, the formulation must be optimized to increase thermal stability as drastic densification and surface area decrease is often exhibited after high-temperature exposure. Current research investigates yttria-stabilized zirconia (YSZ) aerogels for expected use between 600°C and 1000°C. We anticipate that new sol-gel chemistries will yield YSZ aerogels with retained mesoporous structure, increased surface area, and minimized shrinkage upon high-temperature exposure. This work investigates the anionic surfactant, sodium dodecyl sulfate (SDS), and the nonionic surfactant, Pluronic® P-123, as templating agents to prevent the collapse of the aerogel pore structure upon gelation and drying. To determine the effect of surfactant, characterization techniques such as nitrogen physisorption, x-ray diffraction, and scanning electron microscopy are used. By optimizing surfactant concentration, the thermal stability of YSZ aerogels can be enhanced, producing more efficient thermal insulators.
Rebecca C. Walker↗
Polymer Aerogels for Lunar Survivability (PALS)
As the Space Community endeavors to reach new heights of exploration, materials for extreme environment are on the forefront of research. One such material would include polymer aerogels; lightweight solids with nano-scale pore size (10-20 nm), high internal surface area (500-850 m2/g), low thermal conductivity (~20 mW/K), low density ( 0.15-0.05 g/cm3) and extremely high porosities (>95%). Due to these interesting properties, aerogels are ideal as thermal insulators and are by no means limited to this application. The high porosity combined with high surface area, make aerogels an ideal host system for particle incorporation for applications such as IR filtration, sensor platforms, as well as vibro-acoustic, dust, and radiation mitigation materials.
Stephanie Vivod↗
Stimulated geologic hydrogen: from mechanistic control to engineered rock transformation
Geologic hydrogen (GeoH 2 ) generated from subsurface iron-rich rock–water reaction (i.e., serpentinization) is emerging as a promising candidate for the next primary energy source. Yet, accelerating GeoH 2 production from geological to human timescales via enhanced serpentinization remains a formidable scientific and technical challenge. Here, in this Review, we decipher the mechanistic control and explore strategies for accelerating in situ, engineered iron-rich rock transformation into carbon-free GeoH 2 by orders of magnitude. Serpentinization rate is hindered by low porosity and permeability of source rocks, suboptimal temperatures, unfavorable water chemistry, inefficient Fe 2+ -to-Fe 3+ conversion, thermodynamic constraints, and low reactive surface area. While closed-system experiments provide valuable mechanistic insights, open-system conditions with fluid circulation are more crucial for economically viable GeoH 2 production. We assess stimulation techniques from enhanced hydrocarbon and geothermal recovery as tools to be adopted or adapted for increasing reactive surface areas for stimulated GeoH2 production. We estimate that 7.40 × 10 5 to 1.73 × 10 6 million metric tons (Mt) of hydrogen could be engineered over 20 to 50 years from about 10% iron-rich rocks within 10 km depth of continental crust. Enabling GeoH 2 as a viable energy source requires not only advancing scientific frontiers but also forming a global GeoH 2 research network and innovation ecosystem to address the critical scientific, technical, societal, economic, and policy challenges.
08 HYDROGEN↗
Balloon-borne measurements of ClO, NO, and O3 in a volcanic cloud: An analysis of heterogeneous chemistry between 20 and 30 km
Balloon profiles of chlorine monoxide (ClO), nitric oxide (NO), and ozone (O3) were measured on March 11, 1992 from 100 to 10 mb over Greenland (67.0 deg N, 50.6 deg W). Measurements from SAGE II indicate that the aerosol surface area in the region was enhanced by sulfur from the eruption of Mt. Pinatubo, reaching 50 times background near 20 km. Concentrations of ClO were enhanced and concentrations of NO were suppressed relative to low aerosol conditions consistent with the effects of hydrolysis of N2O5 on the surface of sulfuric acid aerosols. The data are consistent with a value of 2 x 10(exp -4) for the reaction probability of the heterogeneous hydrolysis of ClONO2, indicating a minor role for this reaction at as temperature of 220 K. At these temperatures, we find no evidence for the catastrophic loss of ozone predicted to occur under conditions of enhanced aerosol surface area.
Dessler, A. E.↗
Balloon-Borne Measurements of CLO, NO and O3 in a Volcanic Cloud: An Analysis of Heterogeneous Chemistry between 20 and 30 KM
Balloon profiles of chlorine monoxide (ClO), nitric oxide (NO), and ozone (O3) were measured on March 11, 1992 from 100 to 10 mb over Greenland (67.0 deg N, 50.6 deg W). Measurements from SAGE II indicate that the aerosol surface area in the region was enhanced by sulfur from the eruption of Mt. Pinatubo, reaching 50 times background near 20 km. Concentrations of ClO were enhanced and concentrations of NO were suppressed relative to low aerosol conditions consistent with the effects of hydrolysis of N2O5 on the surface of sulfuric acid aerosols. The data are consistent with a value of 2 x 10(exp -4) for the reaction probability of the heterogeneous hydrolysis of ClONO2, indicating a minor role for this reaction at a temperature of 220 K. At these temperatures, we find no evidence for the catastrophic loss of ozone predicted to occur under conditions of enhanced aerosol surface area.
Dessler, A. E.↗
A Study of Stratospheric Aerosols and Their Effect on Inorganic Chlorine Partitioning Using Balloon, In Situ, and Satellite Observations
Heterogeneous reactions on the surface of aerosols lead to a decrease in the concentration of nitrogen radicals and an increase in the concentration of chlorine and hydrogen radical species. As a consequence, enhanced sulfate aerosol levels in the lower stratosphere resulting from volcanic eruptions lead to lower concentrations of ozone due to more rapid loss by chlorine and hydrogen radicals. This study focuses on continuing the effort to quantify the effect of sulfate aerosols on the partitioning of inorganic chlorine species at midlatitudes. The study begins with an examination of balloon-borne measurements of key chlorine species obtained by the JPL MkIV interferometer for different aerosol loading conditions. A detailed comparison of the response of HCl to variations in aerosol surface area observed by MkIV, ER-2 instruments, HALOE, and ATMOS is carried out by examining HCl vs CH4 correlation diagrams, since CH4 is the only tracer measured on each platform. Finally, the consistency between theory and observed changes in ClO and HCl due to variations in aerosol surface area is examined.
Osterman, G. B.↗
A physics-driven Σ-Y atomization model for heavy-duty engine simulations
The atomization of a liquid jet is a multi-scale and multi-physics problem of interest for many engineering applications. Particularly, it drives the fuel-oxidizer mixing and dictates the efficiency of combustion engines. High-fidelity multi-phase simulations remain challenging due to the excessive computational cost required to capture all the atomization scales. Thus, atomization models are necessary to represent sub-grid liquid structures. Here, in this work, a modified Σ-Y model in the context of Eulerian-Lagrangian Spray Atomization (ELSA) is used to transport the surface area density of the spray. The model's predictive performance is assessed under various operating conditions relevant to heavy-duty engines using the Engine Combustion Network (ECN) Spray C and Spray D research-grade injectors. The classic droplet collision formulation of the Σ-Y model alone does not replicate the response of the measured spray surface area to changes in injector, ambient pressure, and injection pressure, requiring individual tuning of the model's parameters. Instead, a transition between dense and dilute spray breakup mechanisms is proposed in terms of the average droplet spacing. The collision breakup mechanism represents the dilute spray, whereas the droplet size in the dense spray is driven by a competition between the integral scale of turbulence and the balance between the turbulent kinetic energy and the surface energy of the droplets. Such an approach minimizes the requirements for model tuning. Moreover, the role of the constants of a compressible standard k-ε RANS model is assessed in the injector's internal flow and external spray simulation framework, and an updated set is proposed. The results are validated against x-ray radiography and Ultra-Small Angle X-ray Scattering (USAXS) data and highlight the predictive capabilities of the proposed physics-driven Σ-Y model, which is compatible with engine simulation turnaround times.
42 ENGINEERING↗
Upcycling linear low-density polyethylene waste to turbostratic graphene for high mass loading supercapacitors
Linear low-density polyethylene (LLDPE) waste is difficult to upcycle into more valuable carbon materials because it tends to completely decompose into small molecules during thermal processing. In this work, LLDPE is upcycled into a high quality turbostratic graphene using a pre-treatment step to oxidatively crosslink the polymer with the assistance of solid additives (KCl and K 2 CO 3 ) that improve crosslinking by increasing the effective surface area of the polymer melt during processing. After this pretreatment step, the crosslinked polymer could then be carbonized and catalytically graphenized between 400–950°C without decomposition of the polymer feedstock. The LLDPE derived graphene (LLDPE-G) obtained from this process has a Brunauer–Emmett–Teller (BET) specific surface area, up to 1800m 2 g -1 and average Raman I D /I G and I 2D /I G ratios of 0.85 and 0.57, respectively, indicating high quality graphene. When used as an electrode material in symmetric supercapacitors, LLDPE-G possesses a specific capacitance up to 175Fg -1 at a mass loading of 20mgcm -2 , which is two times the commercial requirement, yielding an areal capacitance of 3.5 Fcm -2 . Moreover, LLDPE-G exhibits exceptional cycling stability with a capacitance retention of 95.8 % after 100,000 cycles at a current density of 4.0 Ag -1 . Additionally, the KCl and K 2 CO 3 solids are recycled and reused over 3 complete reaction cycles to make new LLDPE-G with the material quality and electrocapacitive performance retained and verified after each cycle. Our approach creates new opportunities for upcycling waste LLDPE and other varieties of polyethylene into a higher value graphene used for electrochemical energy storage applications.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Upcycling Low Linear Density Polyethylene Waste into Turbostratic Graphene for High Mass Loading Supercapacitors
In this work, LLDPE was upcycled into a high quality turbostratic graphene using a pre-treatment step to oxidatively crosslink the polymer with the assistance of solid additives (KCl and K2CO3) that improve crosslinking by increasing the effective surface area of the polymer melt during processing. After this pretreatment step, the crosslinked polymer could then be carbonized and catalytically graphenized between 400-950 °C without complete decomposition of the material. The LLDPE derived graphene (LLDPE-G) obtained from this process has a Brunauer–Emmett–Teller (BET) specific surface area, up to 1800 m2g-1 and average Raman ID/IG and I2D/IG ratios of 0.85 and 0.57, respectively, indicating high quality graphene. When used as an electrode material in symmetric supercapacitors, LLDPE-G possesses an outstanding specific capacitance up to 175 Fg-1 at a mass loading of 20 mgcm-2, which is two times the commercial requirement, yielding an excellent areal capacitance of 3.5 Fcm-2. Moreover, LLDPE-G exhibits exceptional cycling stability with a capacitance retention of 95.8% after 100,000 cycles at a current density of 4.0 Ag-1. Additionally, the KCl and K2CO3 were recycled and reused over 3 complete cycles to make new LLDPE-G with the material quality and electrocapacitive performance retained and verified after each cycle. Our approach creates new opportunities for upcycling not only waste LLDPE but also other varieties of PE to high value graphene materials.
Gao, Yuan [NETL Site Support Contractor, National ↗
Condensed Water in Tropical Cyclone "Oliver", 8 February 1993
On February 8, 1993, the NASA DC-8 aircraft profiled from 10,000 to 37,000 feet (3.1-11.3 km) pressure altitude in a stratified section of tropical cyclone "Oliver" over the Coral Sea northeast of Australia. Size, shape and phase of cloud and precipitation particles were measured with a 2-D Greyscale probe. Cloud/precipitation particles changed from liquid to ice as soon as the freezing level was reached near 17,000 feet (5.2 km) pressure altitude. The cloud was completely glaciated at -5 C. There was no correlation between ice particle habit and ambient temperature. In the liquid phase, the precipitation-cloud drop concentration was 4.0 x 10(exp 3)/cu m, the geometric mean diameter D(sub g) = 0.5-0.7 mm, and the liquid water content 0.7-1.9 g m(exp-3). The largest particles anywhere in the cloud, dominated by fused dendrites at concentrations similar to that of raindrops (2.5 x 10(exp 3) m(exp -3)) but a higher condensed water content(5.4 g/cu m estimated) were found in the mixed phase; condensed water is removed very effectively from the mixed layer due to high settling velocities of the large mixed particles. The highest number concentration (4.9 x 10(exp 4)/cu m, smallest size (D(sub g) = 0.3-0.4 mm), largest surface area (up to 2.6 x 10 (exp 2) sq cm/cu m at 0.4- 1.0 g/cu m of condensate) existed in the ice phase at the coldest temperature (- 40 C) at 35,000 feet ( 10.7 km). Each cloud contained aerosol (haze particles) in addition to cloud particles. The aerosol total surface area exceeded that of the cirrus particles at the coldest temperature. Thus, aerosols must play a significant role in the upscattering of solar radiation. Light extinction (6.2/km) and backscatter (0.8/sr/km) was highest in the coldest portion of the cirrus cloud at the highest altitude.
Pueschel, R. F.↗