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DOE OSTI2020

Enhancing nanostructured nickel-rich lithium-ion battery cathodes via surface stabilization

Layered, nickel-rich lithium transition metal oxides have emerged as leading candidates for lithium-ion battery (LIB) cathode materials. High-performance applications for nickel-rich cathodes, such as electric vehicles and grid-level energy storage, demand electrodes that deliver high power without compromising cell lifetimes or impedance. Nanoparticle-based nickel-rich cathodes seemingly present a solution to this challenge due to shorter lithium-ion diffusion lengths compared to incumbent micrometer-scale active material particles. However, since smaller particle sizes imply that surface effects become increasingly important, particle surface chemistry must be well characterized and controlled to achieve robust electrochemical properties. Moreover, residual surface impurities can disrupt commonly used carbon coating schemes, which result in compromised cell performance. Using x-ray photoelectron spectroscopy, here we present a detailed characterization of the surface chemistry of LiNi0.8Al0.15Co0.05O2 (NCA) nanoparticles, ultimately identifying surface impurities that limit LIB performance. With this chemical insight, annealing procedures are developed that minimize these surface impurities, thus improving electrochemical properties and enabling conformal graphene coatings that reduce cell impedance, maximize electrode packing density, and enhance cell lifetime fourfold. Overall, this work demonstrates that controlling and stabilizing surface chemistry enables the full potential of nanostructured nickel-rich cathodes to be realized in high-performance LIB technology.

Lim, Jin-Myoung↗

DOE OSTI2021

Polysulfide-Permanganate Flow Battery Using Abundant Active Materials

A new flow battery is presented using the abundant and inexpensive active material pairs permanganate/manganate and disulfide/tetrasulfide. A wetted material set is identified for compatibility with the strongly oxidizing manganese couple at ambient and elevated temperatures. Both solutions allow high active material solubility, with cells tested at theoretical energy densities up to 43 Wh l −1 for the ∼1.2 V cell. Full cells built with nickel foam electrodes and sodium-exchanged Nafion 115 membranes deliver a baseline area-specific resistance of 2.7 Ω-cm 2 . Incorporation of high-surface-area cobalt-coated carbon paper and high-surface-area stainless steel mesh electrodes, and an expanded Nafion 115 membrane delivers cells with 44% lower resistance at 1.6 Ω-cm 2 . All cells show performance decay over the course of cycling. The Co-decorated carbon paper electrodes provide significant kinetic improvements, shifting electrode performance from non-linear with Ni-foam to linear with a volume-normalized exchange current density value of 3.2 A cm −3 . The expanded membrane provides increased conductivity over the 13 mS cm −1 conductivity observed in as-received, sodium-exchanged Nafion 115. Although boiled membranes provide improved conductivity, it is at the cost of decreased Coulombic efficiency and poorer manufacturability. Full cell models suggest that similar cell resistances (1.7 Ω-cm 2 ) should be feasible with as-received Nafion 115 and advanced electrodes.

25 ENERGY STORAGE↗

DOE OSTI2024

Bipolar Membrane Capacitive Deionization for the Selective Capture of Lithium Ions from Brines and Conversion to Lithium Hydroxide

Meeting the increasing demand for lithium in vehicle electrification and renewable energy storage requires innovations in lithium-ion (Li + ) separations. Traditional solar evaporation methods for lithium recovery are slow and consume tremendous volumes of water and secondary chemicals (acids and bases). This study introduces a bipolar membrane capacitive deionization (BPM-CDI) unit for direct lithium extraction and LiOH production without the external addition of acids and bases. Utilizing de-lithiated lithium-iron-phosphate (LFP) coated carbon cloth electrodes, the BPM-CDI unit demonstrates selective Li + capture over competing ions. Molecular dynamics simulations and H-cell experiments elucidate pH inversion mechanisms during Li + release, yielding LiOH. The BPM-CDI platform efficiently removes Li + from synthetic brines featuring 8x higher Mg 2+ concentrations (200 ppm Mg 2+ ) and 26x higher Na + concentrations (682 ppm Na + ), achieving a LiOH concentration of 124 ppm (36 ppm Li + ) after 8 cycles of recirculation. Post-mortem analysis confirms electrode integrity and stability. BPM-CDI integrated with selective electrodes is a promising electrochemical separation-reactor platform for lithium recovery while producing LiOH.

Kulkarni, Tanmay↗

NASA NTRS1971

Development of a collapsible reinforced cylindrical space observation window

Existing material technology was applied to the development of a collapsible transparent window suitable for manned spacecraft structures. The effort reported encompasses the evaluation of flame retardants intended for use in the window matrix polymer, evaluation of reinforcement angle which would allow for a twisting pantographing motion as the cylindrical window is mechanically collapsed upon itself, and evaluation of several reinforcement embedment methods. A fabrication technique was developed to produce a reinforced cylindrical space window of 45.7 cm diameter and 61.0 cm length. The basic technique involved the application of a clear film on a male-section mold; winding axial and girth reinforcements and vacuum casting the outer layer. The high-strength transparent window composite consisted of a polyether urethane matrix reinforced with an orthogonal pattern of black-coated carbon steel wire cable. A thin film of RTV silicone rubber was applied to both surfaces of the urethane. The flexibility, retraction system, and installation system are described.

Khan, A. Q.↗

NASA NTRS1977

Residual stresses in boron/tungsten and boron/carbon fibers

Longitudinal residual stress distribution is determined for 102-micron diam B/W and B/C fibers. The 102-micron diam B/W fibers are deposited on a 12.7-micron diam tungsten wire resistively heated in a BCl3-H2 reactor. The 102-micron diam B/C fibers are made by deposition of boron on a pyrolytic graphite-coated carbon fiber. The longitudinal residual stress distribution is calculated from measurements of the change in length of the fiber produced by removal of the surface through electropolishing. It is found that for both types of fibers, the residual stress vary from a compressive stress at the surface to a tensile stress in the boron near the core. Closer to the core and in the core, significant differences in the residual stresses are observed for the B/W and B/C fibers.

Behrendt, D. R.↗

NASA NTRS1985

Processing of Complex Compound Semiconductors in Space

The purpose of this first year ground based research effort was to develop growth and characterization facilities for bulk single crystals of compound semiconductor alloys. As a system of 2-6 alloy crystal growth, C sub x Mn sub (1-x)Te was chosen since it has a relatively narrow solidus-liquidus separation serving as a suitable first model for zone melting and solution growth. Also, it allows, in principle, perfect lattice matching to Cd sub x Hg sub(1-x)Te that needs to be studied as a model for the investigation of heteroepitaxial growth from Te-solutions. A vertical zone melting furnace was built and used in the synthesis of Cd sub x Mn sub(1-x)Te from the elements and crystal growth in carbon coated fused silica crucibles of Bridgman growth geometry. Photoluminescence spectra of the crystals reveal band to band recombination at energies that agree with the reported literature data. In addition, deep luminescence is present at energies corresponding to proportional shifts from the 1.4 eV deep emission observed for bulk single crystals of CdTe.

Bachmann, K.↗

NASA NTRS1986

Characterization of NTD germanium and ion-implanted Si bolometers at 0.3K and 0.1K

Bolometer elements were built and tested using NTD germanium and ion-implanted Si thermometer elements. The thermal links were made using aluminum wires and NbC(x)N(y) coated carbon fibers. The temperature dependence of the detector resistance, lead thermal conductivity, and heat capacity were measured. The dependence of the detector resistance on applied electric field was also measured. This, combined with the current-voltage curve for the detector, allowed the calculation of the detector responsivity. Known amounts of energy were deposited into the detector by allowing X-rays from the decay of Fe-55 to be thermalized in the detector. In the best-measured case, the predicted pulse height/measured height was 1.04 + or - .05. The noise at frequencies above 25 Hz in the NTD Ge was near that predicted by thermodynamics. The noise below 25 Hz has a 1/f character and may be in the carbon fiber/bolometer junction. The implanted detectors show some 1/f noise which depends on the total thermometer volume. Comparison between noise measurements and theory will be presented.

Moseley, H.↗

NASA NTRS1987

Traveling-wave-tube efficiency improvement by a low-cost technique for deposition of carbon on multistage depressed collector

A simple method of improving the traveling-wave-tube (TWT) and multistage depressed collector (MDC) efficiency has been demonstrated. The efficiency improvement was produced by the application of a thin layer of carbon to the copper electrodes of the MDC by means of a rapid, low-cost technique involving the pyrolysis of hydrocarbon oil in electric arc discharges. Experimental results with a representative TWT and MDC showed an 11 percent improvement in both the TWT and MDC efficiencies as compared to those of the same TWT and MDC efficiencies with bare copper electrode surfaces. An extended test with a 500-W, continuous wave (CW) TWT and small-sized MDC indicated good stability of the carbon coated electrode surfaces after a relatively small initial degradation in TWT overall and apparent MDC efficiencies.

Ebihara, Ben T.↗

NASA NTRS1987

TWT efficiency improvement by a low-cost technique for deposition of carbon on MDC electrodes

A simple method of improving the TWT and multistage depressed collector (MDC) efficiency has been demonstrated. The efficiency improvement was produced by the application of a thin layer of carbon to the copper electrodes of the MDC by means of a rapid low-cost technique involving the pyrolysis of hydrocarbon oil in electric arc discharges. Experimental results with a representative TWT and MDC showed an 11 percent improvement in both the TWT and MDC efficiencies as compared to those of the same TWT and MDC with machined copper electrode surfaces. An extended test with a 550-W CW TWT indicated good durability of the carbon-coated electrode surfaces.

Ebihara, Ben T.↗

NASA NTRS1988

Antarctic polar stratospheric aerosols: The roles of nitrates, chlorides and sulfates

Nitric and hydrochloric acids have been postulated to condense in the winter polar stratosphere to become an important component of polar stratospheric clouds. One implication is that the removal of NO(y) from the gas phase by this mechanism allows high Cl(x) concentrations to react with O3, because the formation of ClNO3 is inhibited. Contributions of NO3 and Cl to the stratospheric aerosol were determined during the 1987 Airborne Antarctic Ozone Experiment by testing for the presence of nitrates and chlorides in the condensed phase. Aerosol particles were collected on four 500 micron diameter gold wires, each pretreated differently to give results that were specific to certain physical and chemical aerosol properties. One wire was carbon-coated for concentration and size analyses by scanning electron microscopy; X-ray energy dispersive analyses permitted the detection of S and Cl in individual particles. Three more wires were coated with Nitron, barium chloride and silver nitrate, respectively, to detect nitrate, sulfate and chloride in aerosol particles. All three ions, viz., sulfates, nitrates and chlorides were detected in the Antarctic stratospheric aerosol. In terms of number concentrations, the aerosol was dominated by sulfates, followed by chlorides and nitrates. An inverse linear regression can be established between nitrate concentrations and ozone mixing ratio, and between temperature and nitrates.

Pueschel, R. F.↗

NASA NTRS1989

Fatigue crack growth study of SCS6/Ti-15-3 composite

A study was performed to determine the fatigue crack growth (FCG) behavior and the associated fatigue damage processes in a (0)(8) and (90)(8) oriented SCS(6)/Ti-15-3 composite. Companion testing (CT) was also done on identically processed Ti-15-3 unreinforced material. The active fatigue crack growth failure processes were very similar for both composite orientations tested. For both orientations, fatigue crack growth was along the fiber direction. It was found that the composite constituent most susceptible to fatigue damage was the interface region and in particular the carbon coating surrounding the fiber. The failure of the interface region lead to crack initiation and also strongly influenced the FCG behavior in this composite. The failure of the interface region was apparently driven by normal stresses perpendicular to the fiber direction. The FCG rates were considerably higher for the (90)(8) oriented CT specimens in comparison to the unreinforced material. This is consistent with the scenario in which the interface has lower fatigue resistance than the matrix, causing lower composite fatigue resistance. The FCG rates of the (0)(8) composite could not be directly compared to the (90)(8) composite but were shown to increase with an increase in the crack length.

Kantzos, Peter↗

NASA NTRS1989

Fatigue crack growth in a unidirectional SCS-6/Ti-15-3 composite

An investigation was conducted to characterize and model the fatigue crack growth (FCG) behavior of a SCS-6/Ti-15-3 metal matrix composite. Part of the study was conducted using a fatigue loading stage mounted inside a scanning electron microscope (SEM). This unique facility allowed high magnification viewing of the composite fatigue processes and measurement of the near crack tip displacements. The unidirectional composite was tested in the (0)8 (i.e., longitudinal) and (90)8 (i.e., transverse) orientations. For comparison purposes unreinforced matrix material produced by the identical process as the reinforced material was also tested. The results of the study reveal that the fatigue crack growth behavior of the composite is a function of specimen geometry, fiber orientation and the interaction of local stress fields with the highly anisotropic composite. In the case of (0)8 oriented single edge notch (SEN) specimens and (90)8 oriented compact tension (CT) specimens, the crack growth was normal to the loading direction. However, for the (0)8 CT specimens the crack grew mostly parallel to the loading and the fiber direction. The unusual fatigue behavior of the (0)8 CT specimens was attributed to the specimen geometry and the associated high tensile bending stresses perpendicular to the fiber direction. These stresses resulted in preferential cracking in the weak interface region perpendicular to the fiber direction. The interface region, and in particular the carbon coating surrounding the fiber proved to be the composites weakest link. In the (0)8 SEN the crack growth was confined to the matrix leaving behind unbroken fibers which bridged the cracked surfaces. As the crack grew longer, more fibers bridged the crack resulting in a progressive decrease in the crack growth rates and eventual crack arrest. The actual near crack tip displacement measurements were used in a proposed formulation for a bridging-corrected effective crack driving force, delta K(sub eff). This parameter was able to account for most of the experienced bridging and correlated the (0)8 SEN fatigue crack growth data reasonably well.

Kantzos, Peter↗

NASA NTRS1990

Role of the interfacial thermal barrier in the effective thermal diffusivity/conductivity of SiC-fiber-reinforced reaction-bonded silicon nitride

Experimental thermal diffusivity data transverse to the fiber direction for composites composed of a reaction bonded silicon nitride matrix reinforced with uniaxially aligned carbon-coated silicon carbide fibers indicate the existence of a significant thermal barrier at the matrix-fiber interface. Calculations of the interfacial thermal conductances indicate that at 300 C and 1-atm N2, more than 90 percent of the heat conduction across the interface occurs by gaseous conduction. Good agreement is obtained between thermal conductance values for the oxidized composite at 1 atm calculated from the thermal conductivity of the N2 gas and those inferred from the data for the effective composite thermal conductivity.

Bhatt, Hemanshu↗

NASA NTRS1989

Grain growth, optical polarisation, and extinction in interstellar clouds

Increases in the wavelength of maximum polarization and the ratio of total to selective extinction are generally assumed to be the result of grain growth in interstellar clouds. Using a grain model in which the interstellar extinction is explained by amorphous carbon (a-C) and hydrogenated amorphous carbon (a-C:H) mantles on silicate cores the effects of these absorbing carbonaceous mantles on the polarizing properties of large (500 to 2500 A radius) silicate grains were theoretically studied. The polarization model of Mathis was adopted and it was shown that carbon-coated silicate grains can explain the relationship between the wavelength of maximum polarization and R observed toward dark clouds.

Jones, A. P.↗

NASA NTRS1991

Polymeric routes to silicon carbide and silicon oxycarbide CMC

An overview of two approaches to the formation of ceramic composite matrices from polymeric precursors is presented. Copolymerization of alkyl- and alkenylsilanes (RSiH3) represents a new precursor system for the production of Beta-SiC on pyrolysis, with copolymer composition controlling polymer structure, char yield, and ceramic stoichiometry and morphology. Polysilsesquioxanes which are synthesized readily and can be handled in air serve as precursors to Si-C-O ceramics. Copolymers of phenyl and methyl silsesquioxanes display rheological properties favorable for composite fabrication; these can be tailored by control of pH, water/methoxy ratio and copolymer composition. Composites obtained from these utilize a carbon coated, eight harness satin weave Nicalon cloth reinforcement. The material exhibits nonlinear stress-strain behavior in tension.

Hurwitz, Frances I.↗

NASA NTRS1990

Fatigue crack growth study of SCS6/Ti-15-3 composite

A study was performed to determine the fatigue crack growth (FCG) behavior and the associated fatigue damage processes in a (0)8- and (90)8-oriented SCS6/Ti-15-3 composite. Companion testing was also done on identically processed Ti-15-3 unreinforced material. The active fatigue crack growth failure processes were very similar for both composite orientations tested. For both orientations, fatigue crack growth was along the fiber direction. It was found that the composite constituent most susceptible to fatigue damage was the interface region and, in particular, the carbon coating surrounding the fiber. The failure of the interface region led to crack initiation and also strongly influenced the FCG behavior in this composite. The failure of the interface region was apparently driven by normal stresses perpendicular to the fiber direction. The FCG rates were considerably higher for the (90)8-oriented CT specimens in comparison to the unreinforced material.

Kantzos, P.↗

NASA NTRS1991

Polymeric routes to silicon carbide and silicon oxycarbide CMC

Hurwitz, Frances I.↗

NASA NTRS1989

NASA technology applications team: Applications of aerospace technology

Two critical aspects of the Applications Engineering Program were especially successful: commercializing products of Application Projects; and leveraging NASA funds for projects by developing cofunding from industry and other agencies. Results are presented in the following areas: the excimer laser was commercialized for clearing plaque in the arteries of patients with coronary artery disease; the ultrasound burn depth analysis technology is to be licensed and commercialized; a phased commercialization plan was submitted to NASA for the intracranial pressure monitor; the Flexible Agricultural Robotics Manipulator System (FARMS) is making progress in the development of sensors and a customized end effector for a roboticized greenhouse operation; a dual robot are controller was improved; a multisensor urodynamic pressure catherer was successful in clinical tests; commercial applications were examined for diamond like carbon coatings; further work was done on the multichannel flow cytometer; progress on the liquid airpack for fire fighters; a wind energy conversion device was tested in a low speed wind tunnel; and the Space Shuttle Thermal Protection System was reviewed.

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