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DOE OSTI2021

Effects of carbon treating on piperazine oxidation in pilot plant testing of PZAS™

From February to June 2019, a pilot plant campaign was run for 2100 h at the National Carbon Capture Center (NCCC) using moderately degraded 5 m PZ with simulated flue gas equivalent to a 0.64 MW natural gas combined cycle. Piperazine with the Advanced Stripper™ (PZAS™) and a baghouse were used, and N 2 sparging was applied at the bottom of the absorber. A carbon bed was activated and showed beneficial effects in removing degradation products and reducing the oxidation rate. The cumulative NH 3 production was 180 mmol/k, indicating a PZ oxidation rate of 0.07 mmol/kg/h (0.3 kg PZ/tonne of CO 2 ). The total formate before turning on the carbon bed was 41 mmol/kg, and the total Fe was 0.1 mmol/kg. Carbon treating reduced NH3 production from 0.1 mmol/kg/h to 0.056 mmol/kg/h after 400 h of operation, reduced the UV-Vis absorbance of the samples at 320 nm, and caused a decrease of dissolved Cr. Bench-scale experiments were performed using the NCCC solvent and the same type of carbon. In bench-scale experiments, the UV-Vis absorbance and the concentration of Fe, Mn, and Cr all decreased. Finally, a linear equilibrium relationship was observed between the UV-Vis absorbance and the carbon loading.

03 NATURAL GAS↗

NASA NTRS2007

Concurrent CO2 Control and O2 Generation for Advanced Life Support

The electrochemical reduction of carbon dioxide (CO2) using ceramic oxygen generators (COGs) is well known and widely studied, however, conventional devices using yttria-stabilized zirconia (YSZ) electrolytes operate at temperatures greater than 700 C. Operating at such high temperatures increases system mass compared to lower temperature systems because of increased energy overhead to get the COG up to operating temperature and the need for heavier insulation and/or heat exchangers to reduce the COG oxygen (O2) output temperature for comfortable inhalation. Recently, the University of Florida developed novel ceramic oxygen generators employing a bilayer electrolyte of gadolinia-doped ceria and erbia-stabilized bismuth for NASA's future exploration of Mars. To reduce landed mass and operation expenditures during the mission, in-situ resource utilization was proposed using these COGs to obtain both lifesupporting oxygen and oxidant/propellant fuel, by converting CO2 from the Mars atmosphere. The results showed that oxygen could be reliably produced from CO2 at temperatures as low as 400 C. These results indicate that this technology could be adapted to CO2 removal from a spacesuit and other applications in which CO2 removal was an issue. The strategy proposed for CO2 removal for advanced life support systems employs a catalytic layer combined with a COG so that it is reduced all the way to solid carbon and oxygen. Hence, a three-phased approach was used for the development of a viable low weight COG for CO2 removal. First, to reduce the COG operating temperature a high oxide ion conductivity electrolyte was developed. Second, to promote full CO2 reduction while avoiding the problem of carbon deposition on the COG cathode, novel cathodes and a removable catalytic carbon deposition layer were designed. Third, to improve efficiency, a pre-stage for CO2 absorption was used to concentrate CO2 from the exhalate before sending it to the COG. These subsystems were then integrated into a single CO2 removal system. This paper describes our progress to date on these tasks.

Paul, Heather L.↗

DOE OSTI2025

Magnetized, radiofrequency-driven hollow cathode chemical-vapor deposition of ultrathick hydrogenated amorphous carbon

Amorphous carbon is an attractive material for next-generation inertial confinement fusion (ICF) ablators due to its amorphous structure, tunable density, compatibility with dopants, chemical inertness, and mechanical robustness. Ablators are typically deposited as ultrathick (10–200 μm) coatings on removable spherical templates. The deposition of such thick amorphous carbon films is challenging due to high intrinsic compressive stress, which causes film buckling and delamination. Here, we study the deposition of amorphous carbon films by magnetized, radiofrequency-driven hollow cathode chemical vapor deposition with a custom-designed source in Ne plasmas. Emphasis is on the hollow-cathode source design and effects of the plasma discharge power and the precursor flow rate on film properties. We demonstrate deposition rates of >1 μm/h for films with hydrogen content of ∼40 at. %, densities of 1.1–1.7 g/cm 3 , and trace quantities of oxygen impurities. In conclusion, we also demonstrate the feasibility of depositing thick hydrogenated amorphous carbon films (∼30 μm) for ICF applications.

Carbon based materials↗

NASA NTRS2005

Growing Aligned Carbon Nanotubes for Interconnections in ICs

A process for growing multiwalled carbon nanotubes anchored at specified locations and aligned along specified directions has been invented. Typically, one would grow a number of the nanotubes oriented perpendicularly to a silicon integrated-circuit (IC) substrate, starting from (and anchored on) patterned catalytic spots on the substrate. Such arrays of perpendicular carbon nanotubes could be used as electrical interconnections between levels of multilevel ICs. The process (see Figure 1) begins with the formation of a layer, a few hundred nanometers thick, of a compatible electrically insulating material (e.g., SiO(x) or Si(y)N(z) on the silicon substrate. A patterned film of a suitable electrical conductor (Al, Mo, Cr, Ti, Ta, Pt, Ir, or doped Si), having a thickness between 1 nm and 2 m, is deposited on the insulating layer to form the IC conductor pattern. Next, a catalytic material (usually, Ni, Fe, or Co) is deposited to a thickness between 1 and 30 nm on the spots from which it is desired to grow carbon nanotubes. The carbon nanotubes are grown by plasma-enhanced chemical vapor deposition (PECVD). Unlike the matted and tangled carbon nanotubes grown by thermal CVD, the carbon nanotubes grown by PECVD are perpendicular and freestanding because an electric field perpendicular to the substrate is used in PECVD. Next, the free space between the carbon nanotubes is filled with SiO2 by means of CVD from tetraethylorthosilicate (TEOS), thereby forming an array of carbon nanotubes embedded in SiO2. Chemical mechanical polishing (CMP) is then performed to remove excess SiO2 and form a flat-top surface in which the outer ends of the carbon nanotubes are exposed. Optionally, depending on the application, metal lines to connect selected ends of carbon nanotubes may be deposited on the top surface. The top part of Figure 2 is a scanning electron micrograph (SEM) of carbon nanotubes grown, as described above, on catalytic spots of about 100 nm diameter patterned by electron-beam lithography. These and other nanotubes were found to have lengths ranging from 2 to 10 m and diameters ranging from 30 to 200 nm, the exact values of length depending on growth times and conditions and the exact values of diameter depending on the diameters and thicknesses of the catalyst spots. The bottom part of Figure 2 is an SEM of an embedded array of carbon nanotubes after CMP.

Li, Jun↗

DOE OSTI2022

Self-consistent description of the halo nature of 31 Ne with continuum and pairing correlations

Here a relativistic structure model has previously been used to predict a halo structure for 31 Ne, consistent with halo signatures from measured reaction cross sections of Ne isotopes bombarding Carbon targets. However, previous attempts to calculate those cross sections with reaction models were missing contributions from resonances and pairing correlations in their structure input. Use a reaction model with our relativistic fully microscopic structure model input to predict these cross sections and momentum distributions and analyze for possible halo signatures. Structure input for exotic Ne isotopes were obtained via the analytical continuation of the coupling constant (ACCC) method based on the relativistic mean field (RMF) theory with Bardeen - Cooper - Schrieffer (BCS) pairing approximation, the RAB approach. Total reaction cross sections, one-neutron removal cross sections, and momentum distributions of breakup reaction products were calculated with a Glauber model using our relativistic structure input. Our predictions of total reaction and one-neutron removal cross sections of 31 Ne on a Carbon target were significantly enhanced compared with those of neighboring Neon isotopes, agreeing with measurements at 240 MeV/nucleon and consistent with a single neutron halo. Furthermore, our calculations of the inclusive longitudinal momentum distribution of the 30 Ne and valence neutron residues from the 31 Ne breakup reaction indicate a dilute density distribution in coordinate space, another halo signature. We give a full description of the halo nature of 31 Ne that includes a self-consistent use of pairing and continuum contributions that makes predictions consistent with reaction cross section measurements. This approach can be utilized to determine the halo structure of other exotic nuclei.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

NASA NTRS2006

Method for manufacturing high quality carbon nanotubes

A non-catalytic process for the production of carbon nanotubes includes supplying an electric current to a carbon anode and a carbon cathode which have been securely positioned in the open atmosphere with a gap between them. The electric current creates an electric arc between the carbon anode and the carbon cathode, which causes carbon to be vaporized from the carbon anode and a carbonaceous residue to be deposited on the carbon cathode. Inert gas is pumped into the gap to flush out oxygen, thereby preventing interference with the vaporization of carbon from the anode and preventing oxidation of the carbonaceous residue being deposited on the cathode. The anode and cathode are cooled while electric current is being supplied thereto. When the supply of electric current is terminated, the carbonaceous residue is removed from the cathode and is purified to yield carbon nanotubes.

Benavides, Jeanette M.↗

NASA NTRSDate not supplied

Meteorite Sample Section Repair at NASA Johnson Space Center

Introduction: Meteorite thin and thick sections are routinely shipped from NASA Johnson Space Center to fulfill sample allocation requests from principle investigators around the world. Sections are also re-turned to JSC when researchers are finished studying them since, in most cases, they can be reused for other studies. The sections are very fragile unfortunately, and sometimes return to us needing repairs. The fol-lowing should give you an idea of how we repair sections here in the very lab where they were created. NOTE: Please do not attempt to repair ANSMET meteorite sections that are in your possession. We will perform the repairs for you at NASA JSC if you send the section back to us. Section Delamination: The majority of the meteorite sections that we produce here are secured to the glass slide using a high quality, two-part epoxy. Occasionally, we are asked to use superglue if the researcher wishes to dismount the section from the slide. Both epoxy and superglue are excellent adhesives, but they both tend to embrittle with time which results in delamination from the slide. Exposure to vacuum can also degrade the adhesion between the sample section and the glass slide. Repeated handling of the slide edges can accelerate delamination and, as a preventive measure, the outer 1-2 mm of epoxy is trimmed from newly created sections at JSC. If conductive tapes (copper, carbon, etc.) are used on the section during analysis, great care must be taken in removing the tape so that the epoxy is not pulled up with it. If in doubt, the tape can be left on the section when it is returned to JSC. Before we perform any repairs to sample sections, carbon, gold, or other coatings are removed. We accomplish this using a slurry of 0.05 micron alumina and 190 proof ethyl alcohol applied to a felt polishing pad fitted to a rotating lap wheel. Coatings are re-moved in this manner from all sections that are re-turned to JSC. The extent of the delamination determines how we proceed with the section repair. If the meteorite sample area of the section is not disturbed, then we carefully remove the delaminated epoxy. This is done using a binocular microscope with a 6X zoom, cut-proof gloves, and a very sharp, single edged razor blade. We cut the delaminated epoxy with the blade angled away from the sample area and using very light pressure. The trimmed section is then cleaned in an ultrasonic bath of 200 proof ethyl alcohol for no more than 10 seconds and carefully dried using a lint-free clean room wipe. The section is then placed into a lab oven at 110o F in preparation for epoxy. We mix the resin and hardener components of the low viscosity epoxy and very small amounts are applied to the cut edges of the section using a needle probe and the binocular microscope. Warming the epoxy helps secure the existing section by filling any voids between the glass slide and the section. After the new epoxy cures, we give the section a light polish on a lap wheel fitted with cotton polishing paper that is charged with 1 micron diamond paste. If the section has delaminated to the point of sample area being lifted from the glass, then it may be irreparable. We employ the above technique along with clamping the section in a Teflon pad arrangement in order to flatten the sample while the epoxy cures. Otherwise, the sample will tend to curl. This works to some degree, but once the sample area curls, it seldom re-turns to the original flatness without cracking or bending. Canada Balsam and Crystalbond: We repair damaged sections that had originally been prepared using Canada Balsam or Crystalbond adhesives through the gradual application of heat. We take great care with these samples since these bonding materials tend to get brittle with age. The section is heated in gradual steps (40-50o F per hour) to the melting point of the adhesive. We repair the sample while the adhesive is fluid and then the section is cooled in the same gradual manner in which it was heated. Slide Cracks and Breaks: Accidents happen. Especially with something as small and fragile as a thin/thick section. We all know someone who has driven a microscope objective into a section. As bad as the damage may look, the section can be repaired in most instances. NOTE: Please do not try to tape or glue section pieces back together prior to returning the dam-aged section. This practice usually renders the section irreparable. If the glass slide is cracked but the section is still in one piece, we repair it by infilling the crack with the low viscosity epoxy mentioned earlier. If the slide is in pieces, we can reassemble it with epoxy on a new backer slide. This is a tricky task as the pieces need to be in the correct plane with respect to each other, especially if the sample area is split among several pieces.

Meteorite↗

DOE OSTI2021

Energy Evaluation of Electron Beam Treatment of Perfluoroalkyl Substances in Water: A Critical Review

Due to their recalcitrant nature and ubiquitous use, per- and polyfluoroalkyl substances (PFAS) will continue to be major water treatment hurdles. Although effective water treatment technologies exist for physical removal of many PFAS from water (e.g., activated carbon and ion-exchange resin), a PFAS-concentrated waste stream is generated as an end product that can potentially reintroduce PFAS back into the environment. Thus, there is an increased interest in developing destructive technologies to decompose and mineralize PFAS directly in water or in these waste streams. High energy electron beam (e-beam) accelerators have been used for water treatment to degrade a wide range of recalcitrant contaminants, including PFAS, since the 1960s. However, large-scale applications of e-beam for water treatment are restricted due to its high energy consumption and inability to treat large flow rates. Considering there are very few available technologies for destructive removal of PFAS, this study provides a critical review on the treatment of PFAS by direct irradiation of contaminated water by e-beam from an energy consumption point of view. To date, very limited studies have been conducted to investigate the success of this technology to treat PFAS. Results from the limited studies were not directly comparable due to the variation in operating conditions and water quality parameters used in the studies. Here, for the first time, we develop and apply the concept of electrical energy per order (EE/O) to assess the performance of e-beam for PFAS treatment. Results show that EE/O is a better performance parameter than the G value of e-beam for interstudy comparisons and to evaluate the effects of water quality and operating parameters on e-beam performance. We additionally developed a kinetic scheme to predict the performance of e-beam to treat PFAS and revealed that the competition between species to react with aqueous electrons is the determinant factor influencing PFAS degradation efficiency. Comparison of EE/O values of e-beam (range: 31–176 kWh m –3 order –1 ) with other destructive technologies (range: 5–9595 kWh m –3 order –1 ) suggest that e-beam, for PFAS treatment, is a promising approach under favorable conditions. Furthermore, this review further elucidates the feasibility and limitations of e-beam technology that could be improved upon to potentially make e-beam viable for large-scale water treatment applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Polymer Waste Valorization into Advanced Carbon Nanomaterials for Potential Energy and Environment Applications

The rise in universal population and accompanying demands have directed toward an exponential surge in the generation of polymeric waste. The estimate predicts that world-wide plastic production will rise to ≈590 million metric tons by 2050, whereas 5000 million more tires will be routinely abandoned by 2030. Handling this waste and its detrimental consequences on the Earth's ecosystem and human health presents a significant challenge. Converting the wastes into carbon-based functional materials viz. activated carbon, graphene, and nanotubes is considered the most scientific and adaptable method. Herein, this world provides an overview of the various sources of polymeric wastes, modes of build-up, impact on the environment, and management approaches. Update on advances and novel modifications made in methodologies for converting diverse types of polymeric wastes into carbon nanomaterials over the last 5 years are given. A remarkable focus is made to comprehend the applications of polymeric waste-derived carbon nanomaterials (PWDCNMs) in the CO 2 capture, removal of heavy metal ions, supercapacitor-based energy storage and water splitting with an emphasis on the correlation between PWDCNMs' properties and their performances. In conclusion, this review offers insights into emerging developments in the upcycling of polymeric wastes and their applications in environment and energy.

36 MATERIALS SCIENCE↗

NASA NTRS2003

A Carbon Arc Apparatus For Production Of Nanotubes In Microgravity

Although many methods are available for production of single-walled carbon nanotubes (SWNTs), the conventional carbon arc process remains the most popular due to its simplicity and large production rate. However, high temperatures inside the carbon arc generate strong buoyancy driven convection, and it is hypothesized that the non-uniform environment created by this flow will have large effects on the growth and morphology of SWNTs produced by the arc process. Indeed, using normal gravity experiments, Marin et al. have demonstrated that changes in the buoyant convection plume produced by altering the arc electrode orientation can be used to change the diameter distribution of the SWNTs produced; an effect they attribute to changes in the temperature of the local nanotube growth environment. While these experiments present convincing evidence that buoyant convection has a strong effect on nanotube growth, normal gravity experiments are severely limited in scope. The ideal way to study the effect of buoyancy on SWNT production is to remove it completely. Toward this goal, a microgravity carbon arc reactor has been designed for use in the NASA Glenn 2.2 and 5 second drop towers. Although simple in principle, conventional carbon arc machines, which generally employ large reaction chambers and require heavy duty welding power supplies capable of supplying kilowatts of power, are not suitable for microgravity experiments. Here we describe a miniature carbon arc machine for SWNT production that fits into a conventional drop rig for use on the NASA Glenn 2.2 and 5 second drop towers, but that has a performance (production rate) that is better than most large ground-based machines.

Alford, J. M.↗

DOE OSTI2026

Arctic Black Carbon Aerosol Deposition Study North Slope of Alaska 2020- ACSM Measurements

Particles are removed from the atmosphere through both wet and dry deposition. These processes are poorly understood, though they constitute important uncertainties in climate and air quality models. This project aims to use observational constraints on particle fluxes to improve model representations of dry deposition. In support of black carbon (SP2) and particles (UHSAS) flux measurements at the meteorological tower, we measured non-refractory chemically-speciated aerosol composition with an Aerosol Chemical Speciation Monitor at the the NSA Central Facility (C1). ACSM measurements were made between 9 Sept and 26 Oct 2021. This site is a coastal tundra location, and received snow during the project.

Chl_ACSM↗

DOE OSTI2026

Arctic Black Carbon Aerosol Deposition Study North Slope of Alaska 2020- ACSM Measurements

Aerosol Chemical Speciation Monitor↗

NASA NTRS2022

Skillful Seasonal Forecasts of Land Carbon Uptake in Northern Mid- and High Latitudes

Here we present a first look at the Gross Primary Production (GPP) forecast skill levels achievable with a state-of-the-art subseasonal-to-seasonal (S2S) forecast system. Using NASA’s retrospective S2S ensemble forecast in conjunction with a terrestrial biosphere model, and using an independent, remote sensing-based dataset for validation, we demonstrate an ability to accurately forecast spring-summer carbon uptake at multi-month leads. Averaged across mid-and high latitudes of the Northern Hemisphere land, the GPP forecast initialized on January 1 produces statistically significant skill through summer. The skill achieved, however, is spatially variable, with some regions appearing to extract skill from accurate forecasts of snowpack removal and others extracting skill from the initialization of carbon and nitrogen states. Our results reveal some heretofore unexplored facets of climate predictability and provide a look at what might be possible with future S2S forecast systems that are fully integrated with biogeochemical cycles.

Eunjee Lee↗

NASA NTRS2015

Bulk Preparation of Holey Graphene via Controlled Catalytic Oxidation

A scalable method allows preparation of bulk quantities of holey carbon allotropes with holes ranging from a few to over 100 nm in diameter. Carbon oxidation catalyst nanoparticles are first deposited onto a carbon allotrope surface in a facile, controllable, and solvent-free process. The catalyst-loaded carbons are then subjected to thermal treatment in air. The carbons in contact with the carbon oxidation catalyst nanoparticles are selectively oxidized into gaseous byproducts such as CO or CO.sub.2, leaving the surface with holes. The catalyst is then removed via refluxing in diluted nitric acid to obtain the final holey carbon allotropes. The average size of the holes correlates strongly with the size of the catalyst nanoparticles and is controlled by adjusting the catalyst precursor concentration. The temperature and time of the air oxidation step, and the catalyst removal treatment conditions, strongly affect the morphology of the holes.

Watson, Kent↗

DOE OSTI2026

Seismic Elastic Double-Beam Characterization of Faults and Fractures for CO₂ Storage Site Selection

Site characterization for underground injection and storage of gigatonne-scale CO₂ requires reliable and cost-effective methods to detect and characterize faults and fractures and to assess their stress state and fault activation potential. This is critical, as wastewater injection and disposal have been shown to activate faults and induce earthquakes, and CO₂ leakage remains a key concern for long-term storage. In this project, we developed seismic methods to detect and characterize large-scale sedimentary and crystalline basement faults and associated small-scale fractures below conventional seismic imaging resolution using multicomponent (9C) surface seismic data. Machine learning was used to automatically interpret large-scale faults, providing key information for estimating the maximum magnitude of potential induced earthquakes. High-fidelity imaging was achieved by exploiting redundancy across multiple elastic wave modes, where independent images from different modes and frequencies cross-validate each other. We also used our nonlinear signal comparison (NLSC) method for ground roll removal, improving data quality in complex near-surface conditions. The methods were validated using field data acquired in central Montana. Results show that basement faults extend into the sedimentary section and that small-scale fractures are widespread above the basement. The inferred stress orientation is consistent with regional stress data, and the estimated maximum induced earthquake magnitude is small (Mw ~2.3). The developed workflow provides a practical approach for fault and fracture characterization and for assessing induced seismicity and leakage risk. It is directly applicable to CO₂ storage site selection and to other subsurface systems.

02 PETROLEUM↗

DOE OSTI2025

Arctic Black Carbon Aerosol Deposition Study North Slope of Alaska 2020- SP2 Measurements

Particles are removed from the atmosphere through both wet and dry deposition. These processes are poorly understood, though they constitute important uncertainties in climate and air quality models. This project aims to use observational constraints on particle fluxes to improve model representations of dry deposition. Within this data set, we measured refractory black carbon with a single particle soot photometer (SP2) at the ARM facility’s North Slope of Alaska site. Measurements were made at the meteorological tower between 9 Sept and 27 Oct 2021. This site is a coastal tundra location, and received snow during the project.

Black carbon mass concentration↗

NASA NTRS2005

Control of Effluent Gases from Solid Waste Processing using Impregnated Carbon Nanotubes

One of the major problems associated with solid waste processing technologies is effluent contaminants that are released in gaseous forms from the processes. This is a concern in both biological as well as physicochemical solid waste processing. Carbon dioxide (CO2), the major gas released, does not present a serious problem and there are currently in place a number of flight-qualified technologies for CO2 removal. However, a number of other gases, in particular NOx, SO2, NH3, and various hydrocarbons (e.g. CH4) do present health hazards to the crew members in space habitats. In the present configuration of solid waste processing in the International Space Station (ISS), some of these gases are removed by the Trace Contaminant Control System (TCCS), demands a major resupply. Reduction of the resupply can be effective by using catalyst impregnated carbon nanotubes. For example, NO decomposition to N2 and O2 is thermodynamically favored. Data showing decomposition of NO on metal impregnated carbon nanotubes is presented. Comparisons are made of the existing TCCS systems with the carbon nanotube based technology for removing NOx based on mass/energy penalties.

Li, Jing↗

DOE OSTI2021

System and method for removing water and hydrogen from anode exhaust

A fuel cell system includes an anode configured to output an anode exhaust stream comprising hydrogen, carbon dioxide, and water; and a membrane dryer configured to receive the anode exhaust stream, remove water from the anode exhaust stream, and output a membrane dryer outlet stream. The membrane dryer includes a first chamber configured to receive the anode exhaust stream; a second chamber configured to receive a purge gas; and a semi-permeable membrane separating the first chamber and the second chamber. The semi-permeable membrane is configured to allow water to diffuse therethrough, thereby removing water from the anode exhaust stream. The membrane dryer may further be configured to remove hydrogen from the anode exhaust stream.

Jolly, Stephen↗