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At least 577 records · Page 32
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Titanium Niobium Oxide: From Discovery to Application in Fast-Charging Lithium-Ion Batteries

Lithium-ion batteries are essential for portable technology and are now poised to disrupt a century of combustion-based transportation. The electrification revolution could eliminate our reliance on fossil fuels and enable a clean energy future; advanced batteries would facilitate this transition. However, owing to the demanding performance, cost, and safety requirements, it is challenging to translate new materials from laboratory prototypes to industrial-scale products. This Perspective describes that journey for a new lithium-ion battery anode material, TiNb 2 O 7 (TNO). TNO is intended as an alternative to graphite or Li 4 Ti 5 O 12 with better rate and safety characteristics than the former and higher energy density than the latter. The high capacity of TNO stems from the multielectron redox of Nb 5+ to Nb 3+ , its operating voltage window well above the Li + /Li reduction potential prevents lithium dendrite formation, and its open crystal structure leads to high-power performance. Nevertheless, the creation of a practical TNO anode was nonlinear and nontrivial. Its history is built on 30 years of fundamental science that preceded its application as a battery anode, and its battery development included a nearly 30-year gap. The insights and lessons contained in this Perspective, many of them acquired firsthand, serve two purposes: (i) to unite the disparate studies of TiNb 2 O 7 into a coherent modern understanding relevant to its application as a battery material and (ii) to highlight briefly some of the challenges faced when scaling up a new material that affect TiNb 2 O 7 as well as new electrode candidates more generally.

25 ENERGY STORAGE↗
NASA NTRS1985

The 371 deg C mechanical properties of graphite/polyimide composites

A series of condensation polyimides based on pyromellitic dianhydride is synthesized and evaluated for potential application at 371 C. Several three-and four-ring benzenoid diamine systems containing oxygen bridging groups are investigated. Thermomechanical analysis of neat resin specimens indicate that the polyimide prepared from the dimethyl ester of pyrometallitic acid (PMDE) and 2,2-bis4-(4'-aminophenoxy) phenyl]-1,1,1,3,3,3- hexafluoropropane (BDAF) is the only resin system which has a glass transition temperature (Tg) above 371 C. The Tg of the PMDE/BDAF polyimide is found to be 390 C after a postcure air at 371 C for 24 hr. Unidirectional composites are fabricated from the PMDE/BDAF system and unsized Celion 6000 graphite fibers. Final cure temperatures in the range of 371 to 427 C with an applied pressure of 10.34 to 13.78 MPa are investigated. The void content of the composites ranges from 4.6 to 8.6 percent. Composites cured at 399 C under a pressure of 10.34 MPa and postcured in air at 371 C for 24 hr exhibit the highest 371 C interlaminar shear strength (ILSS, 40.7 MPa) and flexural strength (758 MPa). The thermo-oxidative stability of the composites is determined by subjecting specimens to isothermal exposure at 371 C in air at atmospheric pressure, as well as a pressure of 0.52 MPa. Specimens exposed at atmospheric pressure exhibit a weight loss of 12 percent after 200 hr of exposure and 88 percent retention of its original 371 C ILSS. In contrast, the specimens exposed at 0.52 MPa pressure exhibit a comparable weight loss after only 72 hr, and a 71 percent retention of its original 371 C ILSS.

Delvigs, P.↗
NASA NTRS2004

Ultrasensitive Label-free Electronic Chip for DNA Analysis Using Carbon Nanotube Nanoelectrode Arrays

There is a strong need for faster, cheaper, and simpler methods for nucleic acid analysis in today s clinical tests. Nanotechnologies can potentially provide solutions to these requirements by integrating nanomaterials with biofunctionalities. Dramatic improvement in the sensitivity and multiplexing can be achieved through the high-degree miniaturization. Here, we present our study in the development of an ultrasensitive label-free electronic chip for DNA/RNA analysis based on carbon nanotube nanoelectrode arrays. A reliable nanoelectrode array based on vertically aligned multi-walled carbon nanotubes (MWNTs) embedded in a SiO2 matrix is fabricated using a bottom-up approach. Characteristic nanoelectrode behavior is observed with a low-density MWNT nanoelectrode array in measuring both the bulk and surface immobilized redox species. The open-end of MWNTs are found to present similar properties as graphite edge-plane electrodes, with a wide potential window, flexible chemical functionalities, and good biocompatibility. A BRCA1 related oligonucleotide probe with 18 bases is covalently functionalized at the open ends of the MWNTs and specifically hybridized with an oligonucleotide target as well as a PCR amplicon. The guanine bases in the target molecules are employed as the signal moieties for the electrochemical measurements. Ru(bpy)3(2+) mediator is used to further amplify the guanine oxidation signal. This technique has been employed for direct electrochemical detection of label-free PCR amplicon through specific hybridization with the BRCAl probe. The detection limit is estimated to be less than approximately 1000 DNA molecules, approaching the limit of the sensitivity by laser-based fluorescence techniques in DNA microarray. This system provides a general electronic platform for rapid molecular diagnostics in applications requiring ultrahigh sensitivity, high-degree of miniaturization, simple sample preparation, and low- cost operation.

Li, Jun↗
DOE OSTI2020

A Surface Se-Substituted LiCo[O 2-δ Se δ ] Cathode with Ultrastable High-Voltage Cycling in Pouch Full-Cells

Cycling LiCoO 2 to above 4.5 V for higher capacity is enticing; however, hybrid O anion- and Co cation-redox (HACR) at high voltages facilitates intrinsic O α - (α < 2) migration, causing oxygen loss, phase collapse, and electrolyte decomposition that severely degrade the battery cyclability. Hereby, commercial LiCoO 2 particles are operando treated with selenium, a well-known anti-aging element to capture oxygen-radicals in the human body, showing an “anti-aging” effect in high-voltage battery cycling and successfully stopping the escape of oxygen from LiCoO 2 even when the cathode is cycled to 4.62 V. Furthermore, ab initio calculation and soft X-ray absorption spectroscopy analysis suggest that during deep charging, the precoated Se will initially substitute some mobile O α - at the charged LiCoO 2 surface, transplanting the pumped charges from O α - and reducing it back to O 2- to stabilize the oxygen lattice in prolonged cycling. As a result, the material retains 80% and 77% of its capacity after 450 and 550 cycles under 100 mA g -1 in 4.57 V pouch full-cells matched with a graphite anode and an ultralean electrolyte (2 g Ah -1 ).

36 MATERIALS SCIENCE↗
DOE OSTI2025

Methodology of Atomic Force Microscopy Visualization of Electrode–Electrolyte Interfaces

Electrochemical atomic force microscopy (EC-AFM) provides unprecedented insights into the microstructure of electrode–electrolyte interfaces during electrochemical reactions. However, performing EC-AFM measurements has many challenges, for example, drift, contamination, and probe degradation. We present solutions to these experimental issues through electrochemical cell design and carefully chosen experimental parameters. The possibility that the probes can react with the interface during scanning, generating false-positive electrochemical dynamics, is discussed as an example of the challenge of high-fidelity EC-AFM measurement. Here, we demonstrate this effect in highly ordered pyrolytic graphite and show that we could use electrochemical control of the AFM probe to enable high-fidelity in situ AFM visualization of solid–liquid interfaces during electrochemical reactions.

Electrochemical cells↗
NASA NTRS1993

Solidification of eutectic system alloys in space (M-19)

It is well known that in the liquid state eutectic alloys are theoretically homogeneous under 1 g conditions. However, the homogeneous solidified structure of this alloy is not obtained because thermal convection and non-equilibrium solidification occur. The present investigators have clarified the solidification mechanisms of the eutectic system alloys under 1 g conditions by using the in situ observation method; in particular, the primary crystals of the eutectic system alloys never nucleated in the liquid, but instead did so on the mold wall, and the crystals separated from the mold wall by fluid motion caused by thermal convection. They also found that the equiaxed eutectic grains (eutectic cells) are formed on the primary crystals. In this case, the leading phase of the eutectic must agree with the phase of the primary crystals. In space, no thermal convection occurs so that primary crystals should not move from the mold wall and should not appear inside the solidified structure. Therefore no equiaxed eutectic grains will be formed under microgravity conditions. Past space experiments concerning eutectic alloys were classified into two types of experiments: one with respect to the solidification mechanisms of the eutectic alloys and the other to the unidirectional solidification of this alloy. The former type of experiment has the problem that the solidified structures between microgravity and 1 g conditions show little difference. This is why the flight samples were prepared by the ordinary cast techniques on Earth. Therefore it is impossible to ascertain whether or not the nucleation and growth of primary crystals in the melt occur and if primary crystals influence the formation of the equiaxed eutectic grains. In this experiment, hypo- and hyper-eutectic aluminum copper alloys which are near eutectic point are used. The chemical compositions of the samples are Al-32.4mass%Cu (Hypo-eutectic) and Al-33.5mass%Cu (hyper-eutectic). Long rods for the samples are cast by the Ohno Continuous Casting Process and they show the unidirectionally solidified structure. Each flight and ground sample was made of these same rods. The dimensions of all samples are 4.5 mm in diameter and 23.5 mm in length. Each sample is put in a graphite capsule and then vacuum sealed in a double silica ampoule. Then the ampoule is put in the tantalum cartridge and sealed by electron beam welding. For onbard experiments, a Continuous Heating Furnance (CHF) will be used for melting and solidifying samples under microgravity conditions. Six flight samples will be used. Four samples are hypo-eutectic and two are hyper-eutectic alloys. The surface of the two hypo-eutectic alloy samples are covered with aluminum oxide film to prevent Marangoni convection expected under microgravity conditions. Each sample will be heated to 700 C and held at that temperature for 5 min. After that the samples will be allowed to cool to 500 C in the furnace and they will be taken out of the furnace for He gas cooling. The heating and cooling diagrams for the flight experiments are shown. After collecting the flight samples, the solidified structures of the samples will be examined and the mechanisms of eutectic solidification under microgravity conditions will be determined. It is likely that successful flight experiment results will lead to production of high quality eutectic alloys and eutectic composite materials in space.

Ohno, Atsumi↗
NASA NTRS1995

Magnetic properties of iron-bearing graphite fibers

Carbon fibers containing ferromagnetically-ordered iron or other transition metals could be used in a variety of lightweight magnetic composites. Intercalation of bulk graphite with CoCl2 or FeCl3, followed by reduction with butyl lithium, did indeed produce magnetic samples; however, the observed room temperature permeabilities (mu) were less than 2 G/Oe. Magnetic data are presented on carbon fibers containing large amounts of elemental iron, which were prepared by a new method. In this method Amoco P-75 fibers were intercalated with Br2 and I2 followed by fluorination, forming CF(0.75). This product was then intercalated with FeCl3. Subsequent heat treatments in oxidizing and reducing atmospheres converted most of the iron to the pure alpha phase. Room temperature permeabilities as large as 40 G/Oe are observed.

Ferrante, R.↗
DOE OSTI2022

A Low-Voltage Layered Na 2 TiGeO 5 Anode for Lithium-Ion Battery

Titanium-based anode materials have achieved much progress with the wide studies in lithium-ion batteries. However, these known materials usually possess high discharge voltage platforms and limited energy densities. In this work, a titanium-based oxide of Na 2 TiGeO 5 with layered structure, two-dimensional lamellar frame and exposed highly active (001) facet, exhibiting good electrochemical performance in terms of high capacity (410 mAh g –1 with a current density of 50 mA g –1 ), excellent rate capability and cycling stability with no obvious capacity attenuation after 4000 cycles, is reported. The appropriate discharge voltage plateau at around 0.2 V endows the Na 2 TiGeO 5 anode material high security compared with graphite and high energy density compared with spinel Li 4 Ti 5 O 12 . Combining the electrochemical tests and the density functional theory calculations, the Li + storage mechanism of Na 2 TiGeO 5 is elucidated and the conversion reaction process is revealed. More importantly, this study provides a way to develop low-voltage and high-capacity titanium-based anode materials for efficient energy storage.

25 ENERGY STORAGE↗
DOE OSTI2022

Atomic-scale mechanism of carbon nucleation from a deep crustal fluid by replica exchange reactive molecular dynamics simulation

Here we present a mechanistic model of carbon nucleation and growth from a fluid at elevated temperature (T) and pressure conditions, typical of those found in the shallow Earth’s lithosphere. Our model uses a replica exchange reactive molecular dynamics framework in which molecular configurations are swapped between adjacent T replica at regular intervals according to underlying statistical mechanics. This framework allows predicting complex molecular structures and thermodynamics while remaining computationally efficient. Here we simulate the reactivity of an unstable mixture of CO 2 and CH 4 at 1000 K and 1 GPa. We find that the path to thermodynamic equilibrium is initially entropy-driven, producing a diversity of short-lived species, including various alcohols with intermediate carbon oxidation states. Cyclic and polycyclic radicals that are sometimes resonance-stabilized form next and set the stage for carbon nucleation. The carbon exsolution process releases abundant water, is exothermic and starts with the nucleation of a large aggregate of hydrogenated graphene flakes from covalently bonded polycyclic units. The carbon backbone of this nucleus subsequently grows into a hydrogen-depleted fullerene-like structure, before evolving toward a partially bilayered graphene layer. Overall, our results show that the mechanism of graphitic C formation is certainly not bimolecular, and that it may involve a combination of key condensation and radical chain reactions. This will help understand the isotopic, and reactive characteristics of carbon-bearing fluids during their upward transit through the Earth’s mantle and crust. Moreover, the mechanistic insights outlined here present intriguing similarities with the process of soot and interstellar dust formation, which suggests that the widespread distribution of abiotic polyaromatic and graphitic material on Earth and beyond may reflect the prevalence of a fundamental chemical pathway.

58 GEOSCIENCES↗
NASA NTRS1994

Ferric chloride graphite intercalation compounds prepared from graphite fluoride

The reaction between graphite fluoride and ferric chloride was observed in the temperature range of 300 to 400 C. The graphite fluorides used for this reaction have an sp3 electronic structure and are electrical insulators. They can be made by fluorinating either carbon fibers or powder having various degrees of graphitization. Reaction is fast and spontaneous and can occur in the presence of air. The ferric chloride does not have to be predried. The products have an sp2 electronic structure and are electrical conductors. They contain first stage FeCl3 intercalated graphite. Some of the products contain FeCl2*2H2O, others contain FeF3 in concentrations that depend on the intercalation condition. The graphite intercalated compounds (GIC) deintercalated slowly in air at room temperature, but deintercalated quickly and completely at 370 C. Deintercalation is accompanied by the disappearing of iron halides and the formation of rust (hematite) distributed unevenly on the fiber surface. When heated to 400 C in pure N2 (99.99 vol %), this new GIC deintercalates without losing its molecular structure. However, when the compounds are heated to 800 C in quartz tube, they lost most of its halogen atoms and formed iron oxides (other than hematite), distributed evenly in or on the fiber. This iron-oxide-covered fiber may be useful in making carbon-fiber/ceramic-matrix composites with strong bonding at the fiber-ceramic interface.

Hung, Ching-Cheh↗
NASA NTRS1973

Ablation of ATJ Graphite at High Temperatures

Results of an extensive experimental program on the ablation of ATJ graphite in air at surface pressures of 0.3 to 4.4 atm and surface temperatures of 2570 to 4030 K are presented. The measured mass-loss rates are correlated with surface temperature, pressure, and effective nose radius. The results are compared with several equilibrium thermochemical ablation theories which differ basically in the chemical species that are considered and in the thermodynamic properties assigned to these species. All the theories predict about the same mass-loss rate in the diffusion-controlled oxidation regime and are in good agreement with the experimental results. At higher temperatures, however, the experimental and theoretical results do not agree. At temperatures above 3700 K, the experimental mass-loss rate becomes independent of pressure and an exponential function of temperature. A comparison of the high-temperature results with the theories indicates that all the theories, except the one based on the thermodynamic properties from the JANAF tables, are invalid because they overpredict the mass-loss rate. On the other hand, the theory based on the JANAF properties underpredicts the measured mass-loss rate by a factor of three at 4000 K. At least a portion of this difference between experiment and theory is attributed to particulate mass loss which is visually observed.

Thermochemical ablation↗
NASA NTRS1981

Absorption of visible radiation in atmosphere containing mixtures of absorbing and nonabsorbing particles

The presence of a strongly absorbing material, tentatively identified as graphitic carbon, or 'soot', is indicated by measurements of single-scattering albedo of tropospheric aerosols. Although theoretical calculations based on models of the ways in which soot may mix with other aerosol materials yield the single-scattering albedo values of 0.6, accounted for by a minimum 20% soot by volume, in urban regions and 0.8, yielded by 1-5% soot by volume, in rural settings, it is found that these same values can be produced by similar amounts of the iron oxide magnetite. Magnetite is shown to be indistinguishable from soot by optical measurements performed on bulk samples, and calculation of various mixtures of soot indicate the difficulty of determining aerosol composition by optical scattering techniques.

Ackerman, T. P.↗
NASA NTRS1995

Ferrix Chloride-Graphite Intercalation Compounds Prepared From Graphite Flouride

The reaction between graphite fluoride and ferric chloride was observed in the temperature range of 300 to 400 C. The graphite fluorides used for this reaction have an sp(sup 3) electronic structure and are electrical insulators. They can be made by fluorinating either carbon fibers or powder having various degrees of graphitization. Reaction is fast and spontaneous and can occur in the presence of air. The ferric chloride does not have to be predried. The products have an sp(sup 2) electronic structure and are electrical conductors. They contain first-stage FeCl3 intercalated graphite. Some of the products contain FeCl2 (center dot) 2H2O, others contain FeF3, in concentrations that depend on the intercalation condition. The graphite intercalated compounds (GIC) deintercalated slowly in air at room temperature, but deintercalated quickly and completely at 370 C. Deintercalation is accompanied by the disappearance of iron halides and the formation of rust (hematite) distributed unevenly on the fiber surface. When heated to 400 C in pure N2 (99.99 vol%), this new GIC deintercalates without losing its molecular structure. However, when the compounds are exposed to 800 C N2, in a quartz tube, they lost most of their halogen atoms and formed iron oxides (other than hematite), distributed evenly in or on the fiber.

Hung, Ching-Cheh↗
DOE OSTI2020

Magnetite nanoparticle anchored graphene cathode enhances microbial electrosynthesis of polyhydroxybutyrate by Rhodopseudomonas palustris TIE-1

Microbial electrosynthesis (MES) is an emerging technology that can convert carbon dioxide (CO 2 ) into value-added organic carbon compounds using electrons supplied from a cathode. However, MES is affected by low product formation due to limited extracellular electron uptake by microbes. Herein, a novel cathode was developed from chemically synthesized magnetite nanoparticles and reduced graphene oxide nanocomposite (rGO-MNPs). This nanocomposite was electrochemically deposited on carbon felt (CF/rGO-MNPs), and the modified material was used as a cathode for MES production. The bioplastic, polyhydroxybutyrate (PHB) produced by Rhodopseudomonas palustris TIE-1 (TIE-1), was measured from reactors with modified and unmodified cathodes. Results demonstrate that the magnetite nanoparticle anchored graphene cathode (CF/rGO-MNPs) exhibited higher PHB production (91.31 ± 0.9 mg l -1 ). This is ~4.2 times higher than unmodified carbon felt (CF), and 20 times higher than previously reported using graphite. This modified cathode enhanced electron uptake to -11.7 ± 0.1 μ A cm -2 , ~5 times higher than CF cathode (-2.3 ± 0.08 μ A cm -2 ). The faradaic efficiency of the modified cathode was ~2 times higher than the unmodified cathode. Electrochemical analysis and scanning electron microscopy suggest that rGO-MNPs facilitated electron uptake and improved PHB production by TIE-1. Overall, the nanocomposite (rGO-MNPs) cathode modification enhances MES efficiency.

Materials Science↗
DOE OSTI2023

Characterization of Annealing-Induced Phase Segregation in Composite Silicon Anodes for Li-ion Batteries

Silicon (Si) anodes present a promising alternative to graphite anodes for lithium-ion batteries (LIBs), as Si has a greater specific capacity. However, one major constraint is the volumetric change of Si during lithiation that results in an unstable solid-electrolyte interphase (SEI), so Si-containing electrodes require the use of various strategies to mitigate these effects and improve performance. One such solution is the use of Si nanoparticles (NPs) that maximize the surface area to volume ratio. Here, we discuss electrodes made with Si NPs treated with polyethylene oxide (PEO) (for improving dispersion during processing), conductive carbon NPs, and P84 polyimide binder which shows significant impacts of annealing treatment on improvements of active material utilization, first cycle efficiency, and capacity retention with extensive cycling . We used air-free argon ion polishing to create electrode cross sections and imaged through the electrode thickness using atomic force microscopy (AFM)-based nano-electrical characterization of scanning spreading resistance microscopy (SSRM), nano-mechanical characterizations of contact resonance and force volume (CR-FV), and scanning electron microscopy-based energy dispersive x-ray spectroscopy (SEM-EDS). Results show that the Si and conductive carbon segregate into phases with a distinctive carbon-rich banded morphology that surrounds the Si-rich phase during annealing. In pristine electrodes, the carbon- and SEI-rich bands exhibit a higher electronic conductivity and a lower elastic modulus than the Si active material phase. These structures, as well as distinct electronic and mechanical properties, remain during cycling, suggesting an improvement of electrical conduction pathways and a mechanical strain buffer for active Si material expansion during cycling. This phase separation may be a major factor in the improvement seen in electrochemical performance due to annealing. Additionally, our nm-scale and multi-mode characterizations provide a novel route for understanding and improving energy storage devices, which is advantageous due to the highly inhomogeneous of composite electrodes in nm-mm scales.

ENERGY STORAGE↗
DOE OSTI2026

Techno-Economic Analysis of Recycling Strategies for Catalyst and Acid During Catalytic Graphitization

With the aim of meeting the urgent demand for active anode materials (AAM) in energy storage systems, bio-based graphite (biographite) emerges as an affordable solution to de-risk the turbulent supply chain of critical minerals. Anode grade biographite requires high crystallinity and purity, which can be achieved by catalytic graphitization with iron, followed by acid washing. Therefore, a well-conceived process integration that recycles catalyst can be the starting point to commercialization. This study evaluates closed-loop catalyst recovery, and byproducts valorization scenarios through a technoeconomic framework to help understand the scale-up potential of biographite. For the acid washing, three reactors in series meet the required biographite purity at 99.95%. Iron and acid recovery can reduce material consumption and waste generation by ~95%, albeit at the expense of ~80% increase in capital costs. Recovery scenarios present similar capital and operational expenses, yielding minimum selling prices (MSP) near $6 kg-1 of biographite. Monte Carlo methodology reveals that feedstock price accounts for ~60% of MSP variance, followed by plant capacity ~20%. The likelihood of reaching a competitive profit margin of 30% in the U.S. AAM market sits at 85% average for recovery scenarios, and 103% when iron oxide is sold as byproduct. Additionally, an IRR >= 15% can be achieved for half of Monte Carlo simulations, representing promising early-stage results. Biographite production offers a strategic pathway to stabilize the anode market beyond China by integrating established technologies for a scalable, economically viable, and sustainable process. The role of catalyst recovery and byproducts utilization is critical for advancing the biomaterials industry.

97 MATHEMATICS AND COMPUTING↗
NASA NTRS1976

Effects of atomic oxygen on graphite ablation

It is shown that a previously derived semiempirical equation for describing observed ablation rates of isotropic graphites cannot be applied to low-density flows containing dissociated oxygen. Experimentally determined reaction probabilities of isotropic graphites to molecular and atomic oxygen are used to calculate heat-transfer rates and stagnation-point ablation rates for typical conditions. Integrated mass losses are computed for a group of flight trajectories which start from geosynchronous orbit and enter earth's atmosphere in a skipping motion following near-elliptic decaying orbits. A comparison of the results with those obtained by the equation under question shows excellent agreement for steep trajectories, but large discrepancies for shallow trajectories. The differences are attributed to surface oxidation by atomic oxygen.

Park, C.↗
NASA NTRS2011

Online Oxide Contamination Measurement and Purification Demonstration

Liquid metal sodium-potassium (NaK) has advantageous thermodynamic properties indicating its use as a fission reactor coolant for a surface (lunar, martian) power system. A major area of concern for fission reactor cooling systems is system corrosion due to oxygen contaminants at the high operating temperatures experienced. A small-scale, approximately 4-L capacity, simulated fission reactor cooling system employing NaK as a coolant was fabricated and tested with the goal of demonstrating a noninvasive oxygen detection and purification system. In order to generate prototypical conditions in the simulated cooling system, several system components were designed, fabricated, and tested. These major components were a fully-sealed, magnetically-coupled mechanical NaK pump, a graphite element heated reservoir, a plugging indicator system, and a cold trap. All system components were successfully demonstrated at a maximum system flow rate of approximately 150 cc/s at temperatures up to 550 C. Coolant purification was accomplished using a cold trap before and after plugging operations which showed a relative reduction in oxygen content.

Bradley, D. E.↗