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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 1,279 records · Page 71
All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

The crystal facet-dependent electrochemical performance of TiO 2 nanocrystals for heavy metal detection: Theoretical prediction and experimental proof

Tailored design/fabrication of electroanalytical materials with highly-active exposed crystal planes is of great importance for the development of electrochemical sensing. In this work, combining experimental and theoretical efforts, we reported a facile strategy to fabricate TiO 2 nanocrystals with tunable electrochemical performance for heavy metal detection. Density functional theory (DFT) calculations indicated that TiO 2 (001) facet showed relative larger adsorption energy and lower diffusion energy barrier toward heavy metal ions, which is favorable for obtaining better electrochemical stripping behaviors. Based on this prediction, a series of TiO 2 nanocrystals with different ratios of exposed (001) and (101) facets were synthesized. Electrochemical stripping experiments further demonstrated that with the increase of the percentage of exposed (001) facet, the sensitivity toward Pb(II) and Cd(II) was increased accordingly. When the percentage of exposed (001) facet was increased from 7% to 80%, the sensitivity increased by 190% and 93% for Pb(II) and Cd(II), respectively. In conclusion, our work provides an effective route to construct advanced electroanalytical materials for sensing.

47 OTHER INSTRUMENTATION↗
DOE OSTI2020

Comparative study on the overall energy performance between photovoltaic and Low-E insulated glass units

In this report a novel semi-transparent building integrated photovoltaic (BIPV) laminate was developed and introduced in this paper. It was produced by cutting standard mono-crystalline silicon solar cells into small strips and then making electrical connections between each strip before laminating the cells between two layers of glass. The overall energy performance and energy saving potential of the BIPV insulated glass unit (IGU) under real world conditions were identified through a side by side comparative study. Compared to the reference IGU, the BIPV IGU had lower solar heat gain coefficient (SHGC) but much higher U-factor. The average HVAC electricity saving of the BIPV IGU was about 10% relative to the reference IGU. Daylighting measurement and analysis were carried out to evaluate the trade-offs associated with the BIPV IGU between daylight, glare, and lighting energy use. The results indicated that the BIPV IGU is better than the reference IGU in reducing discomfort glare. However, if the most conservative viewpoint near the window is used for the assessment, a lower transmittance BIPV IGU is required to bring the overall discomfort levels below the perceptible level. Lastly, the net energy saving potential associated with the novel BIPV IGU was identified based on the power, thermal and daylighting performance. On average, the BIPV IGU saved 16.8% of the total electricity use of the room. Further studies and improvement on the energy conversion efficiency of solar cells, the optimal transmittance as well as the thermal properties would make this technology more energy-efficient and affordable.

14 SOLAR ENERGY↗
DOE OSTI2014

Use of porcine vaginal tissue ex-vivo to model environmental effects on vaginal mucosa to toxic shock syndrome toxin-1

Menstrual toxic shock syndrome (mTSS) is a rare, recognizable, and treatable disease that has been associated with tampon use epidemiologically. It involves a confluence of microbial risk factors (Staphylococcus aureus strains that produce the superantigen—TSST-1), as well as environmental characteristics of the vaginal ecosystem during menstruation and host susceptibility factors. This paper describes a series of experiments using the well-characterized model of porcine vaginal mucosa ex-vivo to assess the effect of these factors associated with tampon use on the permeability of the mucosa. The flux of radiolabeled TSST-1 and tritiated water ({sup 3}H{sub 2}O) through porcine vaginal mucosa was determined at various temperatures, after mechanical disruption of the epithelial surface by tape stripping, after treatment with surfactants or other compounds, and in the presence of microbial virulence factors. Elevated temperatures (42, 47 and 52 °C) did not significantly increase flux of {sup 3}H{sub 2}O. Stripping of the epithelial layers significantly increased the flux of labeled toxin in a dose-dependent manner. Addition of benzalkonium chloride (0.1 and 0.5%) and glycerol (4%) significantly increased the flux of {sup 3}H{sub 2}O but sodium lauryl sulfate at any concentration tested did not. The flux of the labeled toxin was significantly increased in the presence of benzalkonium chloride but not Pluronic® L92 and Tween 20 and significantly increased with addition of α-hemolysin but not endotoxin. These results show that the permeability of porcine vagina ex-vivo to labeled toxin or water can be used to evaluate changes to the vaginal environment and modifications in tampon materials, and thus aid in risk assessment. - Highlights: • Model assessed local effects of tampon use on vaginal mucosa. • Risks were evaluated using two tracers to assess permeability in an ex vivo model. • Mechanical damage to the epithelial surface increased tracer penetration. • Surfactants increased penetration of tracers across vaginal mucosa. • Alpha-hemolysin increased the penetration of bacterial toxin across vaginal mucosa.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2015

The adverse effects of aldrin and dieldrin on both myometrial contractions and the secretory functions of bovine ovaries and uterus in vitro

Aldrin and dieldrin are chloroorganic insecticides which are recognised as endocrine disruptors. The aim of the study was to investigate their effect on the secretory functions of the uterus and ovary and on myometrial contractions. Myometrial strips and uterine and ovarian cells from nonpregnant cows were incubated with the xenobiotics (0.1, 1 or 10 ng/ml) for 24 or 72 h. Next, their effect on viability of myometrial, endometrial, granulosa and luteal cells, myometrial strip contractions, the synthesis and secretion of prostaglandins (PGs: PGF2α and PGE2) from uterine cells, the secretion of oestradiol (E2), testosterone (T) and oxytocin (OT) from granulosa cells and the secretion of progesterone (P4) and OT from luteal cells were determined. Neither of the xenobiotics (10 ng/ml) affected (P > 0.05) the viability of the ovarian and uterine cells, while both (0.1–10 ng/ml) decreased (P < 0.05) the basal and OT-stimulated myometrial contractions. In spite of these effects, neither of the insecticides affected (P > 0.05) the synthesis and the secretion of PGs from the myometrial cells. Although they also did not impair the secretion of the PGs from the endometrial cells, they abolished (P < 0.05) the stimulatory effect of OT (P < 0.05) on the secretion of the PGs and stimulated (P < 0.05) the secretion of OT from the granulosa and luteal cells. Moreover, aldrin and dieldrin stimulated secretion of E2 and T from the granulosa cells, while only dieldrin increased (P < 0.05) the secretion of P4 from luteal cells. The data show that aldrin and dieldrin stimulated the secretory function of the cultured granulosa and luteal cells and inhibited the myometrial contractions of cows in vitro, which may affect on natural parturition. - Highlights: • Aldrin and dieldrin inhibited bovine myometrial contractions. • The studied xenobiotics stimulated steroids and oxytocin secretion from ovaries. • Prostaglandins are not involved in adverse effect of the xenobiotics on uterine contractions. • On this basis, we believe that aldrin and dieldrin can hinder the course and onset of parturition.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2017

Lithium recycling and cathode material regeneration from acid leach liquor of spent lithium-ion battery via facile co-extraction and co-precipitation processes

Highlights: • A novel process for combining Li and cathode material recycling is developed. • Ni, Co and Mn are co-extracted and separated with Li. • Li recovered as Li{sub 2}CO{sub 3} with the purity of 99.2% is achieved. • The spherical cathode material LiNi{sub 1/3}Co{sub 1/3}Mn{sub 1/3}O{sub 2} is directly regenerated. - Abstract: A novel process for extracting transition metals, recovering lithium and regenerating cathode materials based on facile co-extraction and co-precipitation processes has been developed. 100% manganese, 99% cobalt and 85% nickel are co-extracted and separated from lithium by D2EHPA in kerosene. Then, Li is recovered from the raffinate as Li{sub 2}CO{sub 3} with the purity of 99.2% by precipitation method. Finally, organic load phase is stripped with 0.5 M H{sub 2}SO{sub 4}, and the cathode material LiNi{sub 1/3}Co{sub 1/3}Mn{sub 1/3}O{sub 2} is directly regenerated from stripping liquor without separating metal individually by co-precipitation method. The regenerative cathode material LiNi{sub 1/3}Co{sub 1/3}Mn{sub 1/3}O{sub 2} is miro spherical morphology without any impurities, which can meet with LiNi{sub 1/3}Co{sub 1/3}Mn{sub 1/3}O{sub 2} production standard of China and exhibits good electrochemical performance. Moreover, a waste battery management model is introduced to guarantee the material supply for spent battery recycling.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2017

Recovery of zinc and cadmium from spent batteries using Cyphos IL 102 via solvent extraction route and synthesis of Zn and Cd oxide nanoparticles

Highlights: • First time Cyphos IL102 explored for recovery of Zn/Cd from spent batteries. • Recovery of metals with high purity was achieved at room temperature. • Quantitative extraction was achieved in two stages for Zn and Cd. •Loaded organic phases were used to synthesize ZnO and CdO nanoparticles. •Simple strippants for stripping isotherm was used. - Abstract: The overall aim of this study is to separate and recover zinc and cadmium from spent batteries. For this purpose Cyphos IL 102 diluted in toluene was employed for the extraction and recovery of Zn and Cd from Zn-C and Ni-Cd batteries leach liquor. The influence of extractant concentration for the leach liquors of Zn-C (0.01–0.05 mol/L) and Ni-Cd (0.04–0.20 mol/L) batteries has been investigated. Composition of the leach liquor obtained from Zn-C/Ni-Cd spent batteries is Zn - 2.18 g/L, Mn - 4.59 g/L, Fe - 4.0 × 10{sup −3} g/L, Ni - 0.2 × 10{sup −3} g/L/Cd - 4.28 g/L, Ni - 0.896 × 10{sup −1} g/L, Fe - 0.148 g/L, Co - 3.77 × 10{sup −3} g/L, respectively. Two stage counter current extraction at A/O 1:1 and 3:2 with 0.04 mol/L and 0.2 mol/L Cyphos IL 102 for Zn and Cd, respectively provide more than 99.0% extraction of both the metal ions with almost negligible extraction of associated metal ions. A stripping efficiency of around 99.0% for Zn and Cd was obtained at O/A 1:1 using 1.0 mol/L HNO{sub 3} in two and three counter current stages, respectively. ZnO and CdO were also synthesized using the loaded organic phase and characterized using XRD, FE-SEM and EDX techniques. XRD peaks of ZnO and CdO correspond to zincite and monteponite, respectively. The average particle size was ∼27.0 nm and ∼37.0 nm for ZnO and CdO, respectively. The EDX analysis of ZnO and CdO shows almost 1:1 atomic percentage.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2018

Dual-Readout Immunochromatographic Assay by Utilizing MnO 2 Nanoflowers as the Unique Colorimetric/Chemiluminescent Probe

Manganese dioxide nanoflowers (MnO2 NFs) were synthesized and utilized as a dual readout probe to develop a novel immunochromatographic test strip (ITS) for detecting pesticide residues using chlorpyrifos as the model analyte. MnO2 NFs-labeled antibody for chlorpyrifos was employed as the signal tracer for conducting the ITS. After 10-min competitive immunoreaction, the tracer antibody was captured by the immobilized immunogen on test line in the test strip, resulting in the accumulation of MnO2 NFs. The accumulation of MnO2 NFs led to the appearance of brown color on the test line, which could be easily observed by the naked eye as a qualitative readout. Moreover, MnO2 NFs showed a remarkably enhancing effect on the luminol-H2O2 chemiluminescent (CL) system. Unlike peroxidase-like nanomaterials, the enhancing mechanism of MnO2 NFs was based on its oxidant activity to decompose H2O2 for forming reactive oxygen species. After initiating the CL system in the test zone, strong CL signal was collected as a quantitative readout to sensitively detect chlorpyrifos. Under optimal conditions, the linear range of chlorpyrifos was 0.1–50 ng/mL with a low detection limit of 0.033 ng/mL (S/N = 3). The reliability of the dual-readout ITS was successfully demonstrated by the application on traditional Chinese medicine and environmental water samples. Due to the simultaneous rapid-qualitative and sensitive-quantitative detection, the dual-readout protocol provides a promising strategy for rapid screening and field assay on various areas such as environmental monitoring, food safety and point-of-care testing.

Ouyang, Hui↗
DOE OSTI2025

Bio-Oil Impact on Water Diffusion and Durability of Bitumen: Influence of Aging and Salinity

Bio-oils derived from inexpensive biomass offer environmentally friendly options for modifying bitumen for improved durability or rejuvenating aged material, although their impact on bitumen moisture resistance can be mixed. A better understanding of water diffusion into bitumen and its interactions with bio-oil compounds would aid the development of effective bio-oils. In this study, the effect of water exposure on bio-oil-modified bitumen blends was examined by de-wetting contact angle measurements and differential FTIR spectroscopy. The bio-oils improved the anti-stripping behavior of the bitumen but also increased water absorption which could weaken cohesive strength. Short-term thermal aging increased water diffusion for all bitumen blends including the control, probably due to the presence of more oxidized compounds. Negative peaks of alkanes and polar groups in the differential FTIR data suggest the co-diffusion of surfactant molecules towards the bitumen-water interface. Basic pH increased de-wetting of some bitumen blends from silica, possibly by attacking the silica surface itself. The presence of salt in solution altered the bitumen surface composition through the formation of salt complexes with bitumen or bio-oil compounds. In particular, the formation of calcium-carboxylate complexes appeared to greatly improve anti-stripping effects of bio-oils. Water diffusion into most of the bitumen blends was insensitive to pH or salt concentration except for a few notable outliers. Identifying the compounds responsible for increasing or decreasing water diffusion in these outlier cases would be valuable developing future bio-oil formations that avoid or promote those compounds.

Hung, Albert M.↗
DOE OSTI2015

Selective Extraction of Rare Earth Elements from Permanent Magnet Scraps with Membrane Solvent Extraction

In this paper, the rare earth elements (REEs) such as neodymium, praseodymium, and dysprosium were successfully recovered from commercial NdFeB magnets and industrial scrap magnets via membrane assisted solvent extraction (MSX). A hollow fiber membrane system was evaluated to extract REEs in a single step with the feed and strip solutions circulating continuously through the MSX system. The effects of several experimental variables on REE extraction such as flow rate, concentration of REEs in the feed solution, membrane configuration, and composition of acids were investigated with the MSX system. A multimembrane module configuration with REEs dissolved in aqueous nitric acid solutions showed high selectivity for REE extraction with no coextraction of non-REEs, whereas the use of aqueous hydrochloric acid solution resulted in coextraction of non-REEs due to the formation of chloroanions of non-REEs. The REE oxides were recovered from the strip solution through precipitation, drying, and annealing steps. Finally, the resulting REE oxides were characterized with XRD, SEM-EDX, and ICP-OES, demonstrating that the membrane assisted solvent extraction is capable of selectively recovering pure REEs from the industrial scrap magnets.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Rapid Quantification of 237 U Specific Activity for Nuclear Forensics

In the event of an unattributed nuclear explosion, rapid assessment of the short-lived uranium isotope activity and mass can provide valuable information for subsequent forensic analysis. Rapid analysis in the field is enabled by using microfluidic chemistry and deployable instrumentation. Here, this work presents a flow chemistry system, controlled in LabVIEW, that integrates three functionalities: (1) selective extraction of uranium from the sample matrix via a 3D-printed supported liquid membrane module; (2) UV–visible absorbance spectrophotometry to measure the total uranium concentration in the strip flow; and (3) a portable CdTe γ-ray spectrometer coupled to a 3D-printed flow cell to measure 237 U activity concentration in the strip solution. The system was calibrated using standard solutions, and its functionality was demonstrated using a solution of depleted uranium spiked with 237 U. Uranium concentrations of 40–5000 μg/mL were directly quantified online using a 100 mm optical flow cell, while concentrations of 0.5–10 μg/mL were quantified online using a colorimetric reagent. The mass concentration measurement takes approximately 60 min while the activity concentration via γ-ray spectrometry varies depending on the activity of 237 U, with 1 kBq/mL requiring about 30 min of acquisition time to obtain <10% uncertainty at 1σ. This platform provides a fieldable approach for quantifying uranium mass and radioactivity relevant to postdetonation nuclear debris.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Water treatment capacity of forward osmosis systems utilizing power plant waste heat

Forward osmosis (FO) has the potential to improve the energy efficiency of membrane-based water treatment by leveraging waste heat from steam electric power generation as the primary driving force for separation. In this study, we develop a comprehensive FO process model, consisting of membrane separation, heat recovery, and draw solute regeneration (DSR) models. We quantitatively characterize three alternative processes for DSR: distillation, steam stripping, and air stripping. We then construct a mathematical model of the distillation process for DSR that incorporates hydrodynamics, mass and heat transport resistances, and reaction kinetics, and we integrate this into a model for the full FO process. Finally, we utilize this FO process model to derive a first-order approximation of the water production capacity given the rejected heat quantity and quality available at U.S. electric power facilities. We find that the upper bound of FO water treatment capacity using low-grade heat sources at electric power facilities exceeds process water treatment demand for boiler water make-up and flue gas desulfurization wastewater systems.

20 FOSSIL-FUELED POWER PLANTS↗
DOE OSTI2016

Performance of an i -SANEX System Based on a Water-Soluble BTP under Continuous Irradiation in a γ-Radiolysis Test Loop

Here, the i -SANEX solvent formulation consisting of nominally 0.2 M TODGA/5% 1-octanol/dodecane was γ-irradiated under realistic conditions in the Idaho National Laboratory radiolysis test loop, in contact with both extraction and stripping aqueous phases. The extraction aqueous phase was 4.5 M HNO 3 , and the stripping aqueous phase was 0.018 M SO 3 –Ph–BTP/0.35 M HNO 3 . When irradiated in contact with only the 4.5 M HNO 3 phase, the TODGA solvent maintained excellent extraction performance for americium, cerium, europium, and neodymium to a maximum absorbed dose of nearly 0.9 MGy. The results for preliminary static, batch irradiations were consistent with test loop findings. When the aqueous phase was changed to that containing the aqueous soluble BTP, the irradiated aqueous phase showed a dramatic color change, but this does not appear to have had adverse effect on solvent extraction performance. The distribution ratios for both the lanthanides and actinides were invariant with absorbed dose, and the separation factors were essentially unchanged to a maximum absorbed dose of 174 kGy. The results of inductively coupled plasma mass spectrometry analysis of the aqueous and organic phases showed that ruthenium and strontium were not extracted in the presence of the irradiated BTP-aqueous phase. Molybdenum was extracted under both conditions. Further, the buildup of corrosion products of stainless steel in the presence of the BTP was not dramatically greater than in the nitric acid-only system. Phase separation times were not adversely affected by irradiation for either system. The results presented here indicate that the performance of the TODGA/SO 3 –Ph–BTP, i -SANEX process under test loop radiolysis is much better than expected based on a literature report using single-phase batch irradiation experiments, and better than might be predicted based on diglycolamide radiolysis studies alone.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2019

Assessment of Impacts of Dissolved Organic Matter and Dissolved Iron on the Performance of Amidoxime-Based Adsorbents for Seawater Uranium Extraction

Research on extraction of uranium from seawater has been active in recent years because this technology can provide an additional supply of uranium for nuclear fuel from a much larger uranium reservoir (the oceans) and the processes are more environment friendly. One critical challenge of the development of this technology is to make uranium adsorbents perform well not just in the oversimplified laboratory system (e.g. artificial seawater) but also in the complex real seawater matrix, which is comprised of many competing ions and natural organic substances. Here, we conducted a systematic study using a continuous-flow seawater flume system to assess the potential impacts of dissolved organic matter (DOM) and dissolved iron on the uranium uptake performance (including adsorbent reusability) of amidoxime-based adsorbents. In the 28-day exposure, the adsorbent exposed in dissolved Fe-spiked seawater (low DOM/high Fe) and humic acid-spiked seawater (high DOM/high Fe) showed lower uranium adsorption loadings (73% and 56% of adsorption loading, respectively) than the same adsorbent exposed in seawater without spiking (low DOM/low Fe). Interestingly, the uranium adsorption loading of the reused adsorbent (after uranium stripping by a mild bicarbonate elution) in the dissolved Fe-spiked seawater dropped substantially to only 24% of the loading in the unspiked clean seawater counterpart; while not much change was observed in the performance of adsorbent exposed to the humic acid-spiked seawater. From comparison of FTIR signatures of adsorbent before and after the seawater exposure, we found that the amidoxime ligands in the adsorbent exposed to dissolved Fe-spiked seawater had severer degradation than the adsorbents exposed to humic acid-spiked seawater and unspiked clean seawater. Notably, unlike the adsorbent exposed to dissolved Fe-spiked seawater, the adsorbent exposed to humic acid-spiked seawater didn’t adsorb elevated level of Fe compared to the adsorbent in the unspiked clean seawater. This suggests that the species of Fe in the humic acid-spiked seawater (primarily humic acid bound Fe) didn’t interact with amidoxime-based adsorbent; while the Fe species in the Fe-spiked seawater strongly interacted with adsorbent and caused significant degradation of amidoxime ligands. On the other hand, highly variable uranium adsorption loadings were observed in adsorbent in contact with humic acid-spiked seawater, but not in the adsorbents exposed to dissolved Fe-spiked seawater and seawater without spike. Our observations thus indicate that seawater receiving high inputs of DOM and dissolved Fe, such as coastal waters, is not ideal for efficient extraction of uranium.

Uranium, Seawater, amidoxime-based adsorbents, dis↗
DOE OSTI2025

Advanced Analysis of X-ray Fluorescence Measurements of the Interfacial Density of Eu Ions at Liquid–Liquid Interfaces for Solvent Back-Extraction

X-ray fluorescence near total reflection (XFNTR) is the primary technique used to measure the element-specific interfacial density of ions at liquid−liquid interfaces. Fluorescence from ions in the bulk liquids can complicate the determination of the interfacial density; consequently, measurements have been previously limited to samples without ions in the upper phase and with concentrations on the order of 10 μM or less in the lower phase. We modify the analysis of XFNTR data to account for ions in both bulk phases, then demonstrate its use in the context of rare-earth separations processes. In a model of ion stripping (i.e., back-extraction), dodecane solutions of di(2-ethylhexyl)- phosphoric acid (HDEHP) loaded with Eu(III) at the 1 mM level are placed in contact with either pure water or aqueous solutions of nitric or citric acid at pH 3. XFNTR measurements of equilibrated, quiescent samples reveal that citric acid solutions produce a disproportionately large depletion of ions from the interface compared to that from the bulk organic solution, whereas stripping by pure water or nitric acid solutions is negligible. As a result, this advance in the methodology of XFNTR may have broad applicability to the investigation of metal ions in chemical and biological processes at liquid−liquid interfaces.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2015

Origin of Multiple Peaks in the Potentiodynamic Oxidation of CO Adlayers on Pt and Ru-Modified Pt Electrodes

The research of the electrooxidation mechanism of CO ad on Pt based catalysts is very important for designing more effective CO-tolerant electrocatalysts for fuel cells. We have studied the origin of multiple peaks in the cyclic voltammograms of CO stripping from polycrystalline Pt and Ru modified polycrystalline Pt (Pt/Ru) surfaces in both acidic and alkaline media by differential electrochemical mass spectrometry (DEMS), DFT calculations, and kinetic Monte Carlo (KMC) simulations. A novel CO ad electrooxidation kinetic model on heterogeneous Pt and Pt/Ru catalysts is proposed to account for the multiple peaks experimentally observed. In this model, OH species prefer to adsorb at low-coordination sites or Ru sites and, thus, suppress CO repopulation from high-coordination sites onto these sites. Therefore, CO ad oxidation occurs on different facets or regions, leading to multiplicity of CO stripping peaks. This work provides a new insight into the CO electrooxidation mechanism and kinetics on heterogeneous catalysts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2018

From Microparticles to Nanowires and Back: Radical Transformations in Plated Li Metal Morphology Revealed via in Situ Scanning Electron Microscopy

We report that Li metal is the preferred anode material for all-solid-state Li batteries. However, a stable plating and stripping of Li metal at the anode–solid electrolyte interface remains a significant challenge particularly at practically feasible current densities. This problem usually relates to high and/or inhomogeneous Li-electrode–electrolyte interfacial impedance and formation and growth of high-aspect-ratio dendritic Li deposits at the electrode–electrolyte interface, which eventually shunt the battery. To better understand details of Li metal plating, we use operando electron microscopy and Auger spectroscopy to probe nucleation, growth, and stripping of Li metal during cycling of a model solid-state Li battery as a function of current density and oxygen pressure. We find a linear correlation between the nucleation density of Li clusters and the charging rate in an ultrahigh vacuum, which agrees with a classical nucleation and growth model. Moreover, the trace amount of oxidizing gas (≈10 –6 Pa of O 2 ) promotes the Li growth in a form of nanowires due to a fine balance between the ion current density and a growth rate of a thin lithium-oxide shell on the surface of the metallic Li. Interestingly, increasing the partial pressure of O 2 to 10 –5 Pa resumes Li plating in a form of 3D particles. In conclusion, our results demonstrate the importance of trace amounts of preexisting or ambient oxidizing species on lithiation processes in solid-state batteries.

25 ENERGY STORAGE↗
DOE OSTI2022

Li Morphology Evolution during Initial Cycles in a Gel Composite Polymer Electrolyte

Understanding and controlling lithium morphology evolution and lithium dendrite formation and growth during cycling is one of the key challenges for high-energy lithium metal batteries. This challenge applies to liquid electrolyte batteries as well as solid-state and semi-solid-state batteries. Our current knowledge about the evolution of the Li morphology is mostly obtained from liquid electrolyte-based studies in a Li–Li symmetrical cell configuration. The knowledge obtained in such conditions may not readily transfer into solid-state or semi-solid-state batteries. In this work, Li morphology evolution during initial cycling in a full cell configuration with the LiNi 0.6 Co 0.2 Mn 0.2 O 2 (NMC 622) cathode and a semi-solid-state gel composite electrolyte is monitored via post-mortem photographs and scanning electron microscopy at multiple length scales. The gel composite electrolyte contains a cross-linked poly(ethylene oxide)-based polymer electrolyte, ceramic fillers, and a liquid plasticizer. The results show that severe surface pitting occurs as early as the second stripping cycle. Pit formation and continuous dissolution during the stripping process are the main cause of the Li surface roughening and dendrite growth mechanism in the model gel composite electrolyte. Comparing Li dendrite growth mechanisms in liquid, polymer, and ceramic solid electrolytes, the dendrite growth mechanism observed in this model electrolyte resembles that of the liquid electrolyte the most. This study suggests that strategies to control Li morphology and prevent dendrite growth in a gel composite electrolyte should be similar to strategies applicable to liquid electrolytes.

25 ENERGY STORAGE↗
DOE OSTI2020

Solubility-Dependent Protective Effects of Binary Alloys for Lithium Anode

Recently, alloys have been widely utilized as protection layers for homogenized Li growth. However, the protective mechanisms for different alloys are not clearly understood. In this work, guided by the binary phase diagrams, Mg, Au, Zn, Al, Fe, and Cu protective layers have been selected for study of their protective abilities and mechanisms. The selected metals can be classified into three categories according to the nature of their associated alloy protective layers: (1) metals with high solubility in Li while not forming any intermediate line compounds, e.g., Mg, which is good for fast Li stripping; (2) metals with limited solid solubility but forming stable line compounds with Li upon the lithiation, e.g., Au, Zn, and Al, where the formed stable line compounds Li x Au, Li x Zn, and Li x Al will hamper Li kinetics; (3) metals with negligible mutual solubility and no line compound formation with Li, e.g., Fe and Cu, which block the Li stripping path and therefore result in the highest polarization voltage.

25 ENERGY STORAGE↗