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DOE OSTI2024

Microbial Reduction of Manganese Oxides From AMD Solids for the Biomining of Critical Minerals / Rare Earth Elements

Abandoned Coal-Mine Drainage (AMD) is a source of critical minerals (CMs) that can be biomined to increase domestic CM production for the growing tech industry while mitigating current AMD hazardous waste. Pennsylvania has ~11,000 abandoned mines, ~500 of which are currently being treated with passive remediation systems (PRS), designed to increase the pH and precipitate AMD waste onsite. Manganese (Mn) that precipitates from AMD waste can co-precipitate with CMs, and the Mn and CMs will accumulate on the PRS solids over the treatment period. This results in high Mn/CM solids that could produce a valuable leachate if resolubilized. Mn reduction and solubilization can occur through microbial driven geochemical changes such as the acidification of the environment, and it is expected that Mn resolubilization will lead to a co-resolubilization of the CMs. Investigation and stimulation of this microbial resolubilization could result in an affordable CM release process that does not require chemical additives into the environment. However the microbial mechanisms that contribute to Mn resolubilization are poorly understood. Here, we have isolated bacteria capable of resolubilizing Mn from AMD PRS. Five of the bacteria isolates have been identified as Bacillus spp. and two as Corynebacterium spp. that ferment glucose to reduce/solubilize Mn MnO2 by acidogenesis. The bacterial isolates are also capable of solubilizing Mn and CMs (Y, Zr, Sb, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu) from AMD PRS precipitated solids through their production of organic acids. Determining the microbial metabolism and genes involved in the resolubilization of manganese is crucial to optimize the biomining of CMs from AMD solid precipitants. This work addresses the growing need to develop novel CM recovery methods from domestic sources.

critical minerals↗

DOE OSTI2024

Scale-Up of Lithium Iron & Aluminum Nickelate Advanced Cathode and Fabrication of A Battery Pack Comprising The Same

Global battery manufacturers are increasingly worried about the serious supply chain constraint caused by rapid fluctuations in cobalt prices over the years. We present a novel cobalt-free, nickel-rich layered cathode material called NFA class (LiNixFeyAlzO2) to tackle this challenge. Spherical NFA(OH)2 precursors were successfully synthesized by incorporating Ni, Fe, and Al elements using a co-precipitation reaction in a continuous stirred tank reactor. The LiNFAO2 cathode, composed of LiNi0.85Fe0.05Al0.1O2, was synthesized and analyzed using X-Ray diffraction, Mössbauer spectroscopy, and scanning electron microscopy (SEM). The material's electrochemical behavior was evaluated through various techniques at different lithiation/delithiation states in two voltage ranges. The cobalt-free material exhibits a high capacity of 190 mAh/g at 0.1C within the voltage range of 3V-4.5V, as demonstrated by electrochemical performance evaluations. Rate and cycling evaluations showed good rate capability and cycling stability, with 88% capacity retention after 100 cycles at C/3 within the voltage range of 3V-4.3V. Our research shows the great potential of cobalt-free NFA cathodes as a feasible option for developing cost-effective lithium-ion batteries.

25 ENERGY STORAGE↗

DOE OSTI2025

Bacterial Biomining Rare Earth Elements in Abandoned Coal Mine Drainage: Solubilization and Sequestration

Bacteria can be used to biomine rare earth elements (REEs) domestically from abandoned coal-mine drainage (AMD) solids. Pennsylvania has ~11,000 abandoned mines, with ~500 AMD passive remediation systems that precipitate AMD REE rich solids onsite. In passive systems, REEs, co-precipitate with manganese (Mn), accumulating as solids that can produce a valuable leachate when resolubilized. REEs like lanthanum (La) are used in battery technology. Microbial metabolic changes that co-resolubilize Mn and REEs could result in an affordable release process that does not require chemical additives and the select sequestering of REEs like La allow for the selective purification from a mixed REE composition. Currently, the microbial mechanisms that contribute to mass REE resolubilization and selective sequestration are poorly understood. We have isolated bacteria (Bacillus mycoides JR07 and Bacillus pseudomycoides KB7) that solubilize Mn oxide, La oxide, and AMD solids by acidogenesis. We have determined that isolates JR07 and KB7 solubilize the La from AMD PRS solids by their production of organic acids. Preliminary results show methylotrophic bacterial isolate B3 can take up soluble La(III), giving an avenue to purification of La from a rich REE leachate. Determining the microbial metabolism and genes involved in the mass resolubilization of REEs and selective biomining of La(III) is crucial to optimize the biomining of AMD solids. Our work addresses the growing need to develop novel REE recovery methods from domestic sources.

microbiology↗

DOE OSTI2024

Scale-Up of Lithium Iron & Aluminum Nickelate Advanced Cathode and Fabrication of A Battery Pack Comprising The Same

25 ENERGY STORAGE↗

DOE OSTI2025

Microbial Biomining for the Release and Recovery of Rare Earth Elements in Abandoned Coal Mine Drainage

Microbes can be used for biomining rare earth elements (REEs) from abandoned coal-mine drainage (AMD) solids. Domestically Pennsylvania has ~11,000 abandoned mines, with ~500 AMD passive remediation systems (PRSs) that precipitate REE rich solids. In passive systems, REEs, co-precipitate with manganese (Mn), accumulating as a valuable leachate when resolubilized. REEs like lanthanum (La) are used in battery technology. Microbial metabolism that co-resolubilize Mn and REEs could result in an affordable release process that does not require the addition of hazardous chemical additives. Microbial sequestering of La can be used for selective purification from a mixed REE composition. Currently, the microbial mechanisms that contribute to mass REE resolubilization and selective sequestration are poorly understood. We have isolated bacteria (Bacillus mycoides JR07 and Bacillus pseudomycoides KB7) that solubilize Mn oxide, La oxide, and AMD solids by acidogenesis. Preliminary results show methylotrophic bacterial isolate B3 can take up soluble La, which may have a potential application in the purification of La from a mixed REE leachate. Determining the microbial metabolism and genes involved in the REE resolubilization and selective biomining of La is crucial to optimize the biomining of AMD solids. Our work addresses the growing need to develop novel REE recovery methods from domestic sources.

microbiology↗

DOE OSTI2025

CRADA Final Report: CRADA Number NFE-22-09311 with Agriwater Tech

Livestock wastewater management is a critical concern in the United States, with an annual production of approximately 1.37 billion tons of waste, surpassing human waste by three to twenty times. The mismanagement of manure wastewater poses significant threats to freshwater sources, ecosystems, and public health. Through this project, we proposed an innovative solution using electrocoagulation (EC) treatment. The EC technique is an electrochemical process involving the intentional corrosion of aluminum and iron electrodes to introduce trivalent ions into the solution, facilitating the co-precipitation and coagulation of contaminants and making the removal of water from sludge easier. The project's primary objective is to use EC to convert liquid animal manure into clean water for farm irrigation, drinking, and maintenance. This solution is vital for various farms including those facing drought, pursuing zero-discharge, and seeking Environmental Protection Agency (EPA) permits for livestock farm manure discharge into rivers. Preliminary research shows EC's potential to significantly reduce turbidity and phosphate levels in livestock wastewater, forming the basis for scalable onsite treatment. The goal of this proposed project is to develop an innovative farm-wastewater-treatment process to achieve clean water, fertilizer, and reduced greenhouse gases through electrification of current processes such as coagulation, dewatering, inactivation of viruses and bacteria, and filtration for recycling surface water from farm lagoons.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

CRADA Final Report: CRADA Number NFE-22-09311 with Agriwater Tech

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2024

Preparation and Characterization of Materials for Low- to Intermediate-Temperature CO2 Adsorption

Global carbon dioxide emissions are rising and the use of fossil fuels in several sectors are the leading causes. As global population and economies continue to grow significantly, the most practical method of lowering such emissions is to capture CO2. Although other technologies are more developed, adsorption is very promising and has attracted much attention. To ensure this technology’s success, it is essential to have suitable CO2 adsorbent materials. In this work, several new hydrotalcites (HTs) with different initial concentrations of ion precursors were prepared for the first time by the co-precipitation method—it was possible to verify that the ion concentrations influence the characteristics of the materials. The prepared HTs were characterized by thermogravimetric analysis (TG), X-Ray diffraction (XRD), surface area measurements and temperature-programmed desorption of CO2 (TPD-CO2) to relate their CO2 capture capacity to their physicochemical properties; the CO2 adsorption equilibrium isotherms were determined at 35 and 300 °C for the prepared samples, as well as for some commercial materials: magnesium oxide, calcium oxide, aluminium oxide and Zeolite 13X. After determining which materials present the best CO2 adsorption capacity, these were submitted to adsorption-desorption cycles to study their stability. The main objective of the work was to prepare and study different CO2 adsorbents for processes that are carried out at low and intermediate temperatures. From the experimental results, it was possible to conclude that the Zeolite 13X showed the best capacity at 35 °C, 3.38 mmol·g−1 (@ pCO2 = 1 bar), and a prepared calcined HT (c-HT2) was the best at 300 °C, 0.97 mmol·g−1 (@ pCO2 = 1 bar). Moreover, it seems there is an optimum initial concentration of the ions’ solutions for the tested HTs, which depends on the final application—c-HT1 showed a better capacity at 35 °C and c-HT2 at 300 °C. From the adsorption-desorption cycles—performed at 35 and 300 °C with the best materials using a magnetic suspension microbalance at 1 bar of CO2 partial pressure —, a working cyclic capacity of 2.69 mmol∙g−1 was achieved by the Zeolite at 35 °C; in turn, c-HT2 showed a working cyclic capacity of 0.79 mmol∙g−1 at 300 °C.

Figueiredo, Anabela↗

NASA NTRS1974

Development of space stable thermal control coatings for use on large space vehicles

The development of a large scale manufacturing method for the production of a stable zinc orthotitanate pigment by means of an oxalate co-precipitation method is examined. Pigments were prepared at various temperatures, and major emphasis was placed on the determination of the important parameters of post-precipitation firing and treatment. A large-scale process for the modification of a glass resin binder was developed and paints were formulated using the binder.

Gilligan, J. E.↗

NASA NTRS1983

Carbon, oxygen and their interaction with intrinsic point defects in solar silicon ribbon material: A speculative approach

Some background information on intrinsic point defects is provided and on carbon and oxygen in silicon in so far as it may be relevant for the efficiency of solar cells fabricated from EFG ribbon material. The co-precipitation of carbon and oxygen and especially of carbon and silicon self interstitials are discussed. A simple model for the electrical activity of carbon-self-interstitial agglomerates is presented. The self-interstitial content of these agglomerates is assumed to determine their electrical activity and that both compressive stresses (high self-interstitial content) and tensile stresses (low self-interstitial content) give rise to electrical activity of the agglomerates. The self-interstitial content of these carbon-related agglomerates may be reduced by an appropriate high temperature treatment and enhanced by a supersaturation of self-interstitials generated during formation of the p-n junction of solar cells. Oxygen present in supersaturation in carbon-rich silicon may be induced to form SiO, precipitates by self-interstitials generated during phosphorus diffusion. It is proposed that the SiO2-Si interface of the precipates gives rise to a continuum of donor stables and that these interface states are responsible for at least part of the light inhancement effects observed in oxygen containing EFG silicon after phosphorus diffusion.

Goesele, U.↗

NASA NTRS1987

Phase purity of NiCo2O4, a catalyst candidate for electrolysis of water

NiCo2O4 is shown to be difficult to obtain as a pure phase, and may never have been so obtained. High resolution x-ray diffractometry is required for its precise characterization. Film XRD is not likely to show the asymmetry in the spinel diffraction lines, caused by poorly crystallized NiO, as seen in diffractometer traces. The Co3O4 which is expected to accompany NiO as an impurity in NiCo2O4 syntheses has the same diffraction pattern as the binary oxide. Firings of the co-precipitated hydroxides at 300, 350, and 400 C, including one in pure O2, failed to produce single phase cobaltate. Scanning electron microscopy showed all the sintered products to range over several orders of magnitude in agglomerate/particle size. Surface areas by BET were all in the range 40 to 110 m sq/g, equivalent to particles of 200 to 100 Angstrom diameter. The spinel diffraction line breadths were compatible with those approximate dimensions.

Singer, J.↗

NASA NTRS2003

Characterization of Al-Cu-Mg-Ag Alloy RX226-T8 Plate

Aluminum-copper-magnesium-silver (Al-Cu-Mg-Ag) alloys that were developed for thermal stability also offer attractive ambient temperature strength-toughness combinations, and therefore, can be considered for a broad range of airframe structural applications. The current study evaluated Al-Cu-Mg-Ag alloy RX226-T8 in plate gages and compared performance with sheet gage alloys of similar composition. Uniaxial tensile properties, plane strain initiation fracture toughness, and plane stress tearing resistance of RX226-T8 were examined at ambient temperature as a function of orientation and thickness location in the plate. Properties were measured near the surface and at the mid-plane of the plate. Tensile strengths were essentially isotropic, with variations in yield and ultimate tensile strengths of less than 2% as a function of orientation and through-thickness location. However, ductility varied by more than 15% with orientation. Fracture toughness was generally higher at the mid-plane and greater for the L-T orientation, although the differences were small near the surface of the plate. Metallurgical analysis indicated that the microstructure was primarily recrystallized with weak texture and was uniform through the plate with the exception of a fine-grained layer near the surface of the plate. Scanning electron microscope analysis revealed Al-Cu-Mg second phase particles which varied in composition and were primarily located on grain boundaries parallel to the rolling direction. Fractography of toughness specimens for both plate locations and orientations revealed that fracture occurred predominantly by transgranular microvoid coalescence. Introduction High-strength, low-density Al-Cu-Mg-Ag alloys were initially developed to replace conventional 2000 (Al-Cu-Mg) and 7000 (Al-Zn-Cu-Mg) series aluminum alloys for aircraft structural applications [1]. During the High Speed Civil Transport (HSCT) program, improvements in thermal stability were demonstrated for candidate aircraft wing and fuselage skin materials through the addition of silver to Al-Cu-Mg alloys based on Al 2519 chemistry [2]. Thermal stability of the resulting Al-Cu-Mg-Ag alloys, C415-T8 and C416-T8, was due to co-precipitation of the thermally stable . (AlCu) and ' (Al2Cu) strengthening phases [1-4]. The strength and toughness behavior was investigated for these alloys produced as 0.090-inch thick rolled sheet in the T8 condition and after various thermal exposures. The mechanical properties were shown to be competitive with conventional aircraft alloys, 2519-T8 and 2618-T8 [2]. During the Integral Airframe Structure (IAS) program, advanced aluminum alloys were examined for use in an integrally stiffened airframe structure where the skin and stiffeners would be machined from plate and extruded frames would be mechanically attached (see Figure 1) [5]. Advantages of integrally stiffened structure include reduced part count, and reduced assembly times compared to conventional built-up airframe structure. The near-surface properties of a thick plate are of significance for a machined integrally stiffened airframe structure since this represents the skin location. Properties measured at the mid-plane of the plate are more representative of the stiffener web. RX226 was developed to exploit strength-toughness improvements and thermal stability benefits of Al-Cu-Mg-Ag alloys in plate gages. This study evaluated the microstructure and properties of three gages of plate produced in the T8 condition.

Lach, Cynthia L.↗

NASA NTRS2004

Sintering of BaCe(0.85)Y(0.15)O3-(Beta) With/Without SrTiO Dopant

The sintering behavior of BaCe(0.85)Y(0.15)O3-(Beta) doped with SrTiO is described. Complete reaction and crystallization of perovskite phase by solid state was achieved by calcining at 1200 degrees C for 24 hours.Smaples were sintered at 1450 degrees C, 1550 degrees C, and 1650 degrees C. SrTiOsub3 enhanced sintering, while optimal dopant level was different for powders synthesized by solid state and co-precipitation. Both powders exhibit similar grain growth behavior.

Dynys, Fred↗

NASA NTRS2015

Insights into the Martian Regolith from Martian Meteorite Northwest Africa 7034

Everything we know about sedimentary processes on Mars is gleaned from remote sensing observations. Here we report insights from meteorite Northwest Africa (NWA) 7034, which is a water-rich martian regolith breccia that hosts both igneous and sedimentary clasts. The sedimentary clasts in NWA 7034 are poorly-sorted clastic siltstones that we refer to as protobreccia clasts. These protobreccia clasts record aqueous alteration process that occurred prior to breccia formation. The aqueous alteration appears to have occurred at relatively low Eh, high pH conditions based on the co-precipitation of pyrite and magnetite, and the concomitant loss of SiO2 from the system. To determine the origin of the NWA 7034 breccia, we examined the textures and grain-shape characteristics of NWA 7034 clasts. The shapes of the clasts are consistent with rock fragmentation in the absence of transport. Coupled with the clast size distribution, we interpret the protolith of NWA 7034 to have been deposited by atmospheric rainout resulting from pyroclastic eruptions and/or asteroid impacts. Cross-cutting and inclusion relationships and U-Pb data from zircon, baddelleyite, and apatite indicate NWA 7034 lithification occurred at 1.4-1.5 Ga, during a short-lived hydrothermal event at 600-700 C that was texturally imprinted upon the submicron groundmass. The hydrothermal event caused Pb-loss from apatite and U-rich metamict zircons, and it caused partial transformation of pyrite to submicron mixtures of magnetite and maghemite, indicating the fluid had higher Eh than the fluid that caused pyrite-magnetite precipitation in the protobreccia clasts. NWA 7034 also hosts ancient 4.4 Ga crustal materials in the form of baddelleyites and zircons, providing up to a 2.9 Ga record of martian geologic history. This work demonstrates the incredible value of sedimentary basins as scientific targets for Mars sample return missions, but it also highlights the importance of targeting samples that have not been overprinted by metamorphic processes, which is the case for NWA 7034.

McCubbin, Francis M.↗

NASA NTRS2017

Acidic Fluids Across Mars: Detections of Magnesium-Nickel Sulfates

Calcium, magnesium and ferric iron sulfates have been detected by the instrument suites on the Mars rovers. A subset of the magnesium sulfates show clear associations with nickel. These associations indicate Ni(2+) co-precipitation with or substitution for Mg(2+) from sulfate-saturated solutions. Nickel is ex-tracted from primary rocks almost exclusively at pH values less than 6, constraining the formation of these Mg-Ni sulfates to mildly to strongly acidic conditions. There is clear evidence for aqueous alteration at the rim of Endeavour Crater (Meridiani Planum), in the Murray formation mudstone (Gale Crater), and near Home Plate (Gusev Crater). The discovery of Mg-Ni sulfates at these locations indicates a history of fluid-rock interactions at low pH.

Yen, A. S.↗

NASA NTRS2022

Effect of Ni2+, Zn2+, and Co2+ on green rust transformation to magnetite

In this study, we investigated Ni2+, Zn2+, and Co2+ mineralogical incorporation and its effect on green rust transformation to magnetite. Mineral transformation experiments were conducted by heating green rust suspensions at 85 °C in the presence of Ni2+, Zn2+, or Co2+ under strict anoxic conditions. Transmission electron microscopy and powder X-ray diffraction showed the conversion of hexagonal green rust platelets to fine grained cubic magnetite crystals. The addition of Ni2+, Zn2+, and Co2+ resulted in faster rates of mineral transformation. The conversion of green rust to magnetite was concurrent to significant increases in metal uptake, demonstrating a strong affinity for metal sorption/ co-precipitation by magnetite. Dissolution ratio curves showed that Ni2+, Zn2+, and Co2+ cations were incorporated into the mineral structure during magnetite crystal growth. The results indicate that the transformation of green rust to magnetite is accelerated by metal impurities, and that magnetite is a highly effective scavenger of trace metals during mineral transformation. The implications for using diagenetic magnetite from green rust precursors as paleoproxies of Precambrian ocean chemistry are discussed.

Hydrosulfate green rust↗

DOE OSTI2020

Cathode materials for lithium ion batteries

A process of forming a coated cathode active material include preparing a cathode material precursor by co-precipitation; coating the cathode material precursor with an electrochemically inert coating material precursor by precipitation to form a coated cathode material precursor; lithiating the coated cathode material precursor with a lithium source material to form a lithiated coated cathode material precursor; and sintering the lithiated coated cathode material precursor to form a cathode active material coated with an electrochemically inert material.

Wu, Huiming↗

DOE OSTI2020

Uranium Partitioning upon Ammonia Gas Treatment on Phyllosilicate Minerals

In the past, > 200,000 kg of U was released to the Hanford Site vadose zone from disposal and leakage of waste byproducts from plutonium production during World War II and the Cold War (Zachara et al., 2007). U is highly mobile due to the presence of carbonates and oxidizing conditions, with K{sub d} of 0.1 - 8 mL/g at the site (Zachara et al., 2007; Szecsody et al., 2013; Serne et al., 2008). NH{sub 3} (gas) injection is being investigated as a remediation technique as it is an in situ method that will not introduce additional liquid that could drive contaminants deeper into vadose zone towards groundwater. Objectives: To understand the impact of alkaline injection on geochemical processes in the Hanford Site vadose zone, including: 1)Long-term fate of uranium (U); 2)Dissolution and re-precipitation of secondary minerals. Apparent K{sub d}'s increase significantly with NH{sub 3} gas treatment, especially for six-month aging. - K{sub d} decreases after aeration, primarily due to U desorption at lower pH. U removal is still significantly greater than natural conditions (K{sub d} < 8 vs. > 100 mL/g). - Three-day aeration has higher loading than six-month after ammonia gas treatment and aeration. However, significantly greater desorption of U occurs with aeration in the six-month aged sample potentially due to transformation into different, more soluble solid phases with longer term aging. - U removal is primarily due to (1) co-precipitation of U with secondary minerals and (2) adsorption to minerals' surface, although further research is required to identify dominant mechanisms. Future experiments will focus on garnering a better understanding of the solid phase U speciation. Solids will be characterized using SEM-EDS, EMPA, XPS, XAFS, and TEM to better understand the effects of basic treatments on initial minerals and formation of secondary precipitates.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗