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All sourcesNASA NTRSDOE OSTI
NASA NTRS2003

Mound Spring Complexes in Central Australia: An Analog for Martian Groundwater Fed Outflow Channels?

The arid inland of Australia contains a diversity of landscapes and landscape processes, often of great antiquity, extending back to the Mesozoic and Paleozoic. The potential of this landscape as a source of Mars analogs has, however, been little explored. The few examples studied so far include radiation-tolerant microbes in thermal springs and hematite-silica hydrothermal alteration near Arkaroola in the Finders Ranges, and aeolian landforms at Gurra Gurra water hole the north east of Arkaroola. Further Australian Mars analog studies were provided by the studies of Bourke and Zimbelman of the paleoflood record of the Todd and Hale Rivers in central Australia. To facilitate study of such analogues, Mars Society Australia has embarked on a project to construct a Mars Analog Research Station near Arkaroola. The international scientific community will soon have the opportunity to participate in Mars analog studies in central Australia utilizing this facility. An area of considerable Mars analog potential is the mound spring complexes that occur at the margins of the Great Artesian Basin (GAB) which underlies 22% of the Australian continent and covers 1.7 million km2. The mound springs are formed when ground water flows to a topographic low, and subsurface strata dips up causing a hydrological head at the surface. Minerals precipitated at the spring discharge zone form low mesas or "mounds", the height of which are controlled by the hydrological head. This paper describes the Dalhousie Mound Spring Complex (DMC) in the northern part of South Australia (Figure 1), and its potential as a Mars analog. Hydrogeology: The DMC consists of a cluster of more than 60 active springs formed by natural discharge from the GAB). Total measured discharge from the GAB is 1.74 GL per day, estimated unfocussed natural leakage through the aquaclude is thought be approximately equal to this figure. Some 54 ML per day are currently discharged by the DMC, 3% of the measured total. The discharged artesian waters are of low to moderate salinity (700 - 9400 ppm), near neutral pH (6.8-7.3) and warm (20-46 C). The elevated temperatures are due to passage of the groundwater through deeply buried (up to 3 km) aquifers in an region of high heat flow, rather than magmatic heating. The waters also contain high levels of dissolved iron and H2S and less than 1 ppm dissolved oxygen. The water is carried in the Late Jurassic Algebuckina Sandstone beneath the aquaclude of the Bulldog Shale. It is brought near the surface by the mid-Cenozoic Dalhousie anticline and the ground water flow focused along a series of faults that breach the anticline's crest.

Clarke, J. D. A.↗
DOE OSTI2020

Preservation of Microalgae, Lignocellulosic Biomass Blends by Ensiling to Enable Consistent Year-Round Feedstock Supply for Thermochemical Conversion to Biofuels

Seasonal variation in microalgae productivity is a significant barrier to economical production of algae biofuels and chemicals. Summer production can be 3–5 times higher than in the winter resulting in uneven feedstock supplies at algae biorefineries. A portion of the summer production must be preserved for conversion in the winter in order to maintain a biorefinery running at capacity. Ensiling, a preservation process that utilizes lactic acid fermentation to limit microbial degradation, has been demonstrated to successfully stabilize algae biomass (20% solids) and algae-lignocellulosic blends (40% algae-60% lignocellulosic biomass, dry basis) for over 6 months, resulting in fuel production cost savings with fewer emissions. Preservation of algae as blends could be beneficial to biorefineries that utilize thermochemical approaches to fuel production as co-processing of algae and lignocellulosic biomass has been observed to enhance biocrude yield and improve oil quality. This study conducts a resource assessment of biomass residues in the southern United States to identify materials available during peak algae productivity and in sufficient quantity to meet the algae storage needs of an algae biofuel industry. Eight feedstocks met the quantity threshold but only three, distillers grains, haylage, and yard waste, were also available in season. Storage experiments utilizing both freshwater and marine strains of microalgae – Scenedesmus acutus, Chlorella vulgaris, Chlorella zofingiensis, Nannochloropsis gaditana, and Porphyridium purpureum – and yard waste were conducted for 30 days. Storage losses were less than 10% in all but one case, and the pH of all but one blend was reduced to less than 4.7, indicating that yard waste is a suitable feedstock for blending with algae prior to storage. To better understand whether the benefits to conversion realized by processing blends might be affected by storage, elemental analysis and bomb calorimetry of pre- and post-storage algae-yard waste blends were conducted to characterize changes occurring during storage. Storing algae biomass as blends with lignocellulosic biomass could be an effective method of mitigating seasonal variability in algae biomass production while retaining the synergistic effect of co-processing algae blends in thermochemical conversion.

09 BIOMASS FUELS↗
DOE OSTI2019

Multi-scale Quantitative Risk Analysis of Seabed Minerals: Principles and Application to Seafloor Massive Sulfide Prospects

The potential for mining hydrothermal mineral deposits on the seafloor, such as seafloor massive sulfides, has become technically possible, and some companies (currently not many) are considering their exploration and development. Yet, no present methodology has been designed to quantify the ore potential and assess the risks relative to prospectivity at prospect and regional scales. Multi-scale exploration techniques, similar to those of the play analysis that are used in the oil and gas industry, can help to fulfill this task by identifying the characteristics of geologic environments indicative of ore-forming processes. Such characteristics can represent a combination of, e.g., heat source, pathway, trap and reservoir that all dictate how and where ore components are mobilized from source to deposition. In this study, the understanding of these key elements is developed as a mineral system, which serves as a guide for mapping the risk of the presence or absence of ore-forming processes within the region of interest (the permissive tract). The risk analysis is carried out using geoscience data, and it is paired with quantitative resource estimation analysis to estimate the in-place mineral potential. Resource estimates are simulated stochastically with the help of available data (bathymetric features in this study), conventional grade–tonnage models and Monte Carlo simulation techniques. In this paper, the workflow for a multi-scale quantitative risk analysis, from the definition to the evaluation of a permissive tract and related prospect(s), is described with the help of multi-beam data of a known hydrothermal vent site.

58 GEOSCIENCES↗
DOE OSTI2019

Semi-supervised machine-learning classification of materials synthesis procedures

Digitizing large collections of scientific literature can enable new informatics approaches for scientific analysis and meta-analysis. However, most content in the scientific literature is locked-up in written natural language, which is difficult to parse into databases using explicitly hard-coded classification rules. In this work, we demonstrate a semi-supervised machine-learning method to classify inorganic materials synthesis procedures from written natural language. Without any human input, latent Dirichlet allocation can cluster keywords into topics corresponding to specific experimental materials synthesis steps, such as “grinding” and “heating”, “dissolving” and “centrifuging”, etc. Guided by a modest amount of annotation, a random forest classifier can then associate these steps with different categories of materials synthesis, such as solid-state or hydrothermal synthesis. Finally, we show that a Markov chain representation of the order of experimental steps accurately reconstructs a flowchart of possible synthesis procedures. Our machine-learning approach enables a scalable approach to unlock the large amount of inorganic materials synthesis information from the literature and to process it into a standardized, machine-readable database.

36 MATERIALS SCIENCE↗
DOE OSTI2020

The Effects of Synthesis Conditions on the Carbon Capture Capacity of Polyethylenimine Impregnated Protonated Titanate Nanotubes

Capture and storage of carbon dioxide emitted from power plants, which burn fossil fuels, is one of the best ways to mitigate climate change. Polyethylenimine (PEI) impregnated protonated titanate nanotubes (PEI-PTNTs) are efficient amine-modified solid adsorbents for post combustion carbon capture. This study is to investigate the effects of synthesis conditions of titanate nanotubes on the carbon capture capacity of PEI-PTNTs. PTNTs are synthesized using hydrothermal treatment of TiO 2 anatase powder at different temperatures and in different days, followed by washing with dilute HCl solution and deionized water. PEI-PTNTs are prepared by loading PEI (M.W. = 10,000) onto PTNTs at a weight ratio of 1:1 using a wet impregnation process. PTNTs and PEI-PTNTs are characterized using transmission electron microscopy, porosity and surface area analysis, powder X-ray diffraction, and Fourier transform infrared spectroscopy. CO 2 adsorption is conducted at 75 °C using simulated flue gas, and CO 2 desorption is performed at 110 °C by purging the adsorbent with dry nitrogen gas. CO 2 adsorption experiments demonstrate that the PEI-PTNTs synthesized at 130 °C within 3 or 5 days, have the highest CO 2 capture capacity. These optimized PEI-PTNTs have a significant potential to capture CO 2 from power plants.

Materials Science↗
NASA NTRS2003

Alpha-amylase from the Hyperthermophilic Archaeon Thermococcus thioreducens

Extremophiles are microorganisms that thrive in, from an anthropocentric view, extreme environments such as hot springs. The ability of survival at extreme conditions has rendered enzymes from extremophiles to be of interest in industrial applications. One approach to producing these extremozymes entails the expression of the enzyme-encoding gene in a mesophilic host such as E.coli. This method has been employed in the effort to produce an alpha-amylase from a hyperthermophile (an organism that displays optimal growth above 80 C) isolated from a hydrothermal vent at the Rainbow vent site in the Atlantic Ocean. alpha-amylases catalyze the hydrolysis of starch to produce smaller sugars and constitute a class of industrial enzymes having approximately 25% of the enzyme market. One application for thermostable alpha-amylases is the starch liquefaction process in which starch is converted into fructose and glucose syrups. The a-amylase encoding gene from the hyperthermophile Thermococcus thioreducens was cloned and sequenced, revealing high similarity with other archaeal hyperthermophilic a-amylases. The gene encoding the mature protein was expressed in E.coli. Initial characterization of this enzyme has revealed an optimal amylolytic activity between 85-90 C and around pH 5.3-6.0.

Bernhardsdotter, E. C. M. J.↗
NASA NTRS2004

Measured Fluid Flow in an Active H2O-CO2 Geothermal Well as an Analog to Fluid Flow in Fractures on Mars: Preliminary Report

Water in the Earth's crust generally contains dissolved gases such as CO2. Models for both 'Blue Mars' (H2O-driven processes) and 'White Mars' (CO2-driven processes) predict liquid H2O with dissolved CO2 at depth. The fate of dissolved CO2 as this mixture rises toward the surface has not been quantitatively explored. Our approach is a variation on NASA's 'Follow the Water' as we 'Follow the Fluid' from depth to the surface in hydrothermal areas on Earth and extrapolate our results to Mars. This is a preliminary report on a field study of fluid flow in a producing geothermal well. For proprietary reasons, the name and location of this well cannot be revealed, so we have named it 'Earth1' for this study.

Kieffer, Susan W.↗
DOE OSTI2018

Tailor-Made Microporous Metal–Organic Frameworks for the Full Separation of Propane from Propylene Through Selective Size Exclusion

Adsorptive separation of olefin/paraffin mixtures by porous solids can greatly reduce the energy consumption associated with the currently employed cryogenic distillation technique. Here, the complete separation of propane and propylene by a designer microporous metal–organic framework material is reported. The compound, Y 6 (OH) 8 (abtc) 3 (H 2 O) 6 (DMA) 2 (Y-abtc, abtc = 3,3',5,5'-azobenzene-tetracarboxylates; DMA = dimethylammonium), is rationally designed through topology-guided replacement of inorganic building units. Y-abtc is both thermally and hydrothermally robust, and possesses optimal pore window size for propane/propylene separation. It adsorbs propylene with fast kinetics under ambient temperature and pressure, but fully excludes propane, as a result of selective size exclusion. Multicomponent column breakthrough experiments confirm that polymer-grade propylene (99.5%) can be obtained by this process, demonstrating its true potential as an alternative sorbent for efficient separation of propane/propylene mixtures.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Quantifying EGS Reservoir Complexity with an Integrated Geophysical Approach-Improved Resolution Ambient Seismic Noise Interferometry

The primary goal of the project was met, as improved resolution (from kilometers to tens/hundreds of meters and to a depth of at least 3 km) was added to the seismic interferometry-estimated parameters relative to the work reported in AltaRock Energy Inc. (2014) for the Dixie Valley Geothermal Wellfield. A procedure for initial fault identification, using seismic interferometry, was developed. The project team further improved, and applied a new, cost-effective, and non-invasive exploration method, developed and validated since 2010, during two previous experiments, at Dixie Valley and Soda Lake, Nevada. The method, initially designed for hydrothermal exploration, was adapted to EGS exploration conditions, which require deeper crustal information. Regions of elevated energy for both the 2-7 Hz and 5-15 Hz frequency bands are located above intersections of multiple faults. Thus, an unprecedented, innovative seismic field deployment and ambient seismic noise and signal processing were successfully used to estimate crustal structure and to identify fault locations at depths up to 3 km, at a cost per kilometer of survey that in some cases may be as much as ten times less than the cost of a controlled-source survey. Based on valid and useful seismic data collected and analyzed during Phase I, in Phase II the team has further quantified statistically the advantage of using seismic analysis, in combination with other geological and geophysical techniques, for EGS target identification. A power spectral density analysis of the passive-seismic empirical Green’s functions reveals significantly higher power recorded over the exploration area at the power plant, and in the drilling area, near the BB station 10201, especially on the horizontal components. In this study, the most important relationship observed during the prior report, namely the one between velocity and temperature was explored. The areas that show anomalously high predicted temperature in the geostatistics occur where multiple faults intersect. Not surprisingly, such areas span between the Dixie Valley range front fault and the basin-ward Piedmont faults, in the vicinity of numerous wells. These locations also fall in the area of high EGS favorability from the prior 2014 study. The anomalies also coincide with the high power spectral density values. The result of altering all favorability criteria for the new data reached a maximum of 1/8th of a point and were not large enough to change any favorability value reported in the 2014 study. The new data reinforce the results obtained from the previous 2014 study. The current high-resolution ambient seismic noise project provided excellent results in defining faults in the wellfield. As such the identification of known faults by the project demonstrated the utility of this method for identifying faults at an exploration stage in geothermal development. Such fault identification, while extremely useful in exploration investigation, has not added sufficient new data for the generation of significantly different DVGW favorability maps in the current project. We believe the cost savings of our passive-seismic technique for EGS, over common industry active-source survey techniques, may have a minimum of 30%, and a maximum of 90%. There are many significant non-cost benefits of passive seismic surveys. Our passive-source method provides an environmentally-friendly seismic survey with minimal to negligible impacts. The economic benefit is greater EGS project feasibility.

15 GEOTHERMAL ENERGY↗
NASA NTRS1983

Evaluation of radiometric and geometric characteristics of LANDSAT-D imaging system

With vegetation masked and noise sources eliminated or minimized, different carbonate facies could be discriminated in a south Florida scene. Laboratory spectra of grab samples indicate that a 20% change in depth of the carbonate absorption band was detected despite the effects of atmospheric absorption. Both bright and dark hydrothermally altered volcanic rocks can be discriminated from their unaltered equivalents. A previously unrecognized altered area was identified on the basis of the TM images. The ability to map desert varnish in semi-arid terrains has economic significance as it defines areas that are less susceptible desert erosional process and suitable for construction development.

Salisbury, J. W.↗
NASA NTRS1992

Expert system-based mineral mapping using AVIRIS

Integrated analysis of imaging spectrometer data and field spectral measurements were used in conjunction with conventional geologic field mapping to characterize bedrock and surficial geology at the northern end of Death Valley, California and Nevada. A knowledge-based expert system was used to automatically produce image maps from Airborne Visible/Infrared Imaging Spectrometer (AVIRIS) data showing the principal surface mineralogy. The imaging spectrometer data show the spatial distribution of spectrally distinct minerals occurring both as primary rock-forming minerals and as alteration and weathering products. Field spectral measurements were used to verify the mineral maps and field mapping was used to extend the remote sensing results. Geographically referenced image-maps produced from these data form new base maps from which to develop improved understanding of the processes of deposition and erosion affecting the present land surface. The 'northern Grapevine Mountains' (NGM) study area was reported on in numerous papers. This area is an unnamed northwestward extension of the range. Most of the research here has concentrated on mapping of Jurassic-age plutons and associated hydrothermal alteration, however, the nature and scope of these studies is much broader, pertaining to the geologic history and development of the entire Death Valley region. AVIRIS data for the NGM site were obtained during May 1989. Additional AVIRIS data were acquired during September 1989 as part of the Geologic Remote Sensing Field Experiment (GRSFE). The area covered by these data overlaps slightly with the May 1989 data. Three and one-half AVIRIS scenes total were analyzed.

Kruse, Fred A.↗
NASA NTRS2008

Gusev Crater on Mars: Wet and Dry

The Mars Exploration Rover Spirit has traversed over 7.5 km in 1470 sols of operations at the Gusev Crater landing site. Chemical and mineralogical evidence from approximately 200 in-situ samples indicate various degrees of exposure to liquid water, from wet and saturated to dry and unaltered. (1) Six samples with concentrations of amorphous silica between 60 and 95 wt% were discovered in a small valley less than 50 meters in length. Associated enrichments in titanium oxide, relatively insoluble at low pH, suggest that these silica deposits formed as a result of acidic leaching processes. Liquid water interactions with these surface materials were necessary to remove cations solubilized in the low pH environment or to concentrate silica in solution prior to precipitation. (2) Hydrated ferric sulfates are found in subsurface deposits which have the unmistakable chemical signatures of nearby rocks. The movement of hydrothermal fluids and/or fumarolic vapors through local rocks prior to precipitation of these materials is suggested by these observations. (3) Goethite (alpha-FeOOH), a mineral phase which requires water to form, represents 20% to 35% of the iron in numerous rock samples (Clovis Class) on the West Spur of the Columbia Hills. Alteration of iron under aqueous conditions is clearly indicated by this presence of goethite. (4) Nearly isochemical signatures are found in elemental analyses of over ten distinct samples (Wishstone/Watchtower class rocks), yet the ratio of ferric iron to total iron varies from 0.4 to 0.95. Small quantities of water, insufficient to flush cations from the samples, were likely responsible for this weathering. (5) Bromine, a trace element readily mobilized by water, is found in high concentrations in certain rock interiors and is enhanced in subsurface soils, consistent with transport to localized cold traps by water thin-films. (6) Also relevant to the characterizing the role of liquid water is the discovery of an areally extensive ultramafic sequence of rocks where over 70% of the iron is in unaltered olivine and the ferric to total iron ratio is 0.1. This result indicates that certain materials at the martian surface have been protected from aqueous alteration.

Yen, Albert↗
DOE OSTI2019

Ceria-based nanoflake arrays integrated on 3D cordierite honeycombs for efficient low-temperature diesel oxidation catalyst

A new, surfactant-free hydrothermal method has been developed for the growth of CeO 2 -based nanoflake arrays onto three-dimensional-channeled cordierite honeycomb substrates. Herein, a leaching-crystallization mechanism was proposed where the hydrothermal reaction, only involving cerium nitrate and water, leached the cordierite surface slightly and induced the formation of CeO 2 nanoparticles subsequently. Further continued reaction reincorporated Al and Si atoms leached from cordierite into CeO 2 , finally recrystallizing Ce-Al-Si composite nanoflake structures. Here, by using atomic layer deposition process, well-dispersed, size-controlled Pt nanoparticles were uniformly decorated on the CeO 2 -based nanoflakes to form the Pt/ CeO 2 nano-array-based monolithic catalyst. Despite 5-50 times reduction in the active material usage compared with the traditional wash-coated catalyst, the Pt/CeO 2 nano-array monolithic catalyst exhibited good catalytic oxidation activities over various individual gases, such as propylene, propane, CO, and NO oxidation, with 90% conversion efficiencies at temperatures below 200 °C. Under the simulated exhaust condition of low-temperature diesel combustion (LTC-D) developed by US DRIVE, the monolithic catalyst with low Pt loading (˜1 g/l) exhibits 90% conversion of catalytic oxidation over CO and hydrocarbonsat temperatures as low as ˜180 °C, much superior to the performance of traditional washcoated catalysts.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Hydrothermal Preparation, Crystal Chemistry, and Redox Properties of Iron Muscovite Clay

The development of functional materials based on Earthabundant, environmentally benign compositions is critical for ensuring their commercial viability and sustainable production. In this paper we present an investigation into the crystal chemistry and electrochemical properties of the muscovite clay KFe 2.75 Si 3.25 O 10 (OH) 2 . We first report a low-temperature hydrothermal reaction that allows for a significant degree of control over sample crystallinity, particle morphology, and cation distribution through the lattice. A complex sequence of stacking faults is identified and characterized using a combination of Mössbauer spectroscopy and total scattering neutron experiments. We then show the existence of a reversible electrochemical process using galvanostatic cycling with complementary cyclic voltammetry suggesting that the redox activity occurs primarily on the surface of the particles. We conclude by determining that the ability to (de)intercalate Li ions from the material is hindered by the strong negative charge on the transition metal silicate layers, which prevents the displacement of the interlayer K ions. This work calls attention to a hugely Earth-abundant family of minerals that possesses useful electrochemical properties that warrant further exploration.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1985

Planetary ecology; Proceedings of the Sixth International Symposium on Environmental Biogeochemistry, Santa Fe, NM, October 10-14, 1983

Topics presented include biological evolution and planetary chemistry; C-1 compounds; transport, deposition, and weathering; sulfur transformations; ground water; transformation processes for nitrogen oxides; and soils. Papers are presented on immunological studies on the organic matrix of recent and fossil invertebrate shells; biogenic gases in sediments deposited since Miocene times on the Walvis Ridge, South Atlantic Ocean; aspects of the biogeochemistry of Big Soda Lake, NV; mesophilic manganese-oxidizing bacteria from hydrothermal discharge areas at 21 deg North on the East Pacific Rise; and autotrophic growth and iron oxidation and inhibition kinetics of Leptospirillum ferrooxidans. Consideration is also given to thermophilic archaebacteria occurring in submarine hydrothermal areas; fate of sulfate in a soft-water, acidic lake; geochemical conditions in the ground water environment; microbial transformations as sources and sinks for nitrogen oxides; and the biogeochemistry of soil phosphorus.

Caldwell, D. E.↗
DOE OSTI2025

Whole Algae Hydrothermal Liquefaction and Upgrading: A review of progress and challenges and insight into the future

This report summarizes the research at Pacific Northwest National Laboratory (PNNL) to evaluate the economic viability and environmental impact of using microalgae to produce fuels and other products via hydrothermal liquefaction (HTL). Over the past several years, PNNL has examined key aspects of feedstock cost and availability, formatting and conversion techniques, and the utilization of all HTL products. Investigations of feedstock cost led to opportunities to work with cost-advantaged algal feedstocks that can be provided at minimal cost for HTL processing. Cost-advantaged algae include wastewater-grown algae and harvested algal blooms. Although farm-cultivated algae offer the best possible biomass composition and scalability for HTL processing, the cost of the feedstock is too high to yield an economically competitive biofuel. Processing cost-advantaged feedstocks creates other unique challenges in adapting HTL to upgrade biomass with higher than typical ash content and less preferred composition (low lipid). Despite the challenges, HTL of cost-advantaged algae results in economically competitive pricing scenarios and significant advantages in reducing net emissions below 70% of the petroleum baseline. The utilization of a variety of potential non-fuel products from algal HTL, such as the use of HTL solids as a cement additive, provides a significant reduction in net emissions by offsetting emissions from other carbon-intense products. This report presents an analysis of the research conducted at PNNL to develop an economically and environmentally beneficial process for algae HTL.

09 BIOMASS FUELS↗
DOE OSTI2023

Biofuel Air Emissions Analysis

U.S. has goals to produce 3 billion gallons of sustainable aviation fuel (SAF) annually by 2030, increasing to 35 billion gallons by 2050 to decarbonize the aviation sector. Meeting these production targets will require large number of biorefineries to be set up. However, ability to comply with federal air quality standards is prerequisite to being issued a construction permit. Negotiating the permitting process for a new biorefinery can be quite onerous and cost the investors significant time and money. Although there can be numerous reasons for delayed biorefinery construction, air permitting is fraught with pitfalls because the permitting process relies on precedence, which the future SAF biorefineries lack. NREL's Biofuel Air Emissions Analysis project is unique and innovative in terms of the tools, approaches, and analyses provided. NREL is the only national laboratory that is actively working at the intersection of Federal air quality regulations, emissions and air quality analysis across the supply chain, and process design. This project is focused on providing much needed data and analyses that address biorefinery air permitting. This project develops models and quantitative analyses and measures progress towards meeting air quality regulatory requirements. These models and methods are applied to analyze air permitting related to wastewater sludge to biofuel conversion pathways using hydrothermal liquefaction (HTL), impacts of HTL pathway on local and regional air quality including an assessment of health and equity impacts. In addition to filling research gaps, this project also disseminates the findings to the relevant stakeholders at BETO, other national labs, and regulatory agencies.

air quality↗
DOE OSTI2020

Solution-Based, Anion-Doping of Li 4 Ti 5 O 12 Nanoflowers for Lithium-Ion Battery Applications

Solution–based, anionic doping represents a convenient strategy with which to improve upon the conductivity of candidate anode materials such as Li 4 Ti 5 O 12 (LTO). As such, novel synthetic hydrothermally–inspired protocols have primarily been devised herein, aimed at the large–scale production of unique halogen–doped, micron–scale, three–dimensional, hierarchical LTO flower–like motifs. Although fluorine (F) doping has been explored, the use of chlorine (Cl) dopants is the primary focus here. Several experimental variables, such as dopant amount, lithium hydroxide concentration, and titanium butoxide purity, were probed and perfected. Furthermore, the Cl doping process did not damage the intrinsic LTO morphology. The analysis, based on interpreting a compilation of SEM, XRD, XPS, and TEM–EDS results, was used to determine an optimized dopant concentration of Cl. Electrochemical tests demonstrated an increased capacity via cycling of 12 % for a Cl–doped sample as compared with pristine LTO. Moreover, the Cl–doped LTO sample described in this study exhibited the highest discharge capacity yet reported at an observed rate of 2C for this material at 143mAh g –1 . Overall, these data suggest that the Cl dopant likely enhances not only the ion transport capabilities, but also the overall electrical conductivity of our as–prepared structures. Furthermore, to help explain these favorable findings, theoretical DFT calculations were used to postulate that the electronic conductivity and Li diffusion were likely improved by the presence of increased Ti 3+ ion concentration coupled with widening of the Li migration channel.

25 ENERGY STORAGE↗