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DOE OSTI2023

Single Crystal Growth of Synthetic Sulfide- and Phosphide-Based Minerals for Physical Measurements

In this work, we review recent advances in the use of high-temperature solution growth that allow for the growth of single crystalline samples of synthetic minerals. We outline how low-melting binary or ternary solutions are attractive solvents for solution growth and provide examples of the growth of bismuthinite (Bi 2 S 3 ), galena (PbS) and parkerite (Ni 3 Bi 2 S 2 ). We then focus on the Rh-S, Pd-S and Ni-P phase spaces to discuss how the low-melting regions near transition metal-main group eutectic compositions make excellent solvents for crystal growth of several binary and ternary minerals containing both high melting and volatile elements as well as for the discovery of new materials. We end by discussing the growth of synthetic canfieldite (Ag 8 SnS 6 ) and argyrodite (Ag 8 GeS 6 ) from Ag 2 S–Sn-S-based solutions.

58 GEOSCIENCES↗

DOE OSTI2024

Mineral Deposition on the Rough Walls of a Fracture

Modeling carbonate growth in fractures and pores is important for understanding carbon sequestration in the environment or when supersaturated solutions are injected into rocks. Here, we study the simple but nontrivial problem of calcite growth on fractures with rough walls of the same mineral using kinetic Monte Carlo simulations of attachment and detachment of molecules and scaling approaches. First, we consider wedge-shaped fracture walls whose upper terraces are in the same low-energy planes and show that the valleys are slowly filled by the propagation of parallel monolayer steps in the wedge sides. The growth ceases when the walls reach these low-energy configurations so that a gap between the walls may not be filled. Second, we consider fracture walls with equally separated monolayer steps (vicinal surfaces with roughness below 1 nm) and show that growth by step propagation will eventually clog the fracture gap. In both cases, scaling approaches predict the times to attain the final configurations as a function of the initial geometry and the step-propagation velocity, which is set by the saturation index. The same reasoning applied to a random wall geometry shows that step propagation leads to lateral filling of surface valleys until the wall reaches the low-energy crystalline plane that has the smallest initial density of molecules. Thus, the final configurations of the fracture walls are much more sensitive to the crystallography than to the roughness or the local curvature. The framework developed here may be used to determine those configurations, the times to reach them, and the mass of deposited mineral. Effects of transport limitations are discussed when the fracture gap is significantly narrowed.

calcite↗

DOE OSTI2025

Anthropogenic Influences on the Chemical and Mineral Composition in Pond Sediment by X-Ray Absorption Spectroscopy and X-Ray Powder Diffraction

Manmade detention ponds have historically been impacted by anthropogenic activities such as rainwater runoff, car emissions, and drainage from infrastructures, which can lead to complications for pond ecosystems. Sediment samples collected from the northern, southern, western, and eastern regions of a small pond on a suburban high school campus on Long Island, NY, were analyzed for potential chemical changes resulting from an inundation of water by a broken water main. Incorporating synchrotron X-ray techniques, sediment was analyzed using Submicron Resolution Spectroscopy, Tender Energy X-ray Spectroscopy, and X-ray Powder Diffraction to examine heavy metals, light elements, and minerals. Results include a Zn:Cu ratio increase from 4:1 to 10:1 in the eastern zone and a higher heavy metal presence in the western zone for all elements examined, with greater distribution throughout the pond post-inundation. Lighter elements appear to remain relatively unchanged. The appearance of diopside in the eastern zone post-inundation samples suggests contamination from the water main break, while the presence of carbonate minerals in the western zone is consistent with erosion of asphalt material from the adjacent parking lot.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2014

X-ray fluorescence mapping of mercury on suspended mineral particles and diatoms in a contaminated freshwater system

Mercury (Hg) bioavailability and geochemical cycling is affected by its partitioning between the aqueous and particulate phases. We applied a synchrotron-based X-ray fluorescence (XRF) microprobe to visualize and quantify directly the spatial localization of Hg and its correlations with other elements of interest on suspended particles from a Hg-contaminated freshwater system. Up to 175 μg g −1 Hg is found on suspended particles, but less than 0.01% is in the form of methylmercury. Mercury is heterogeneously distributed among phytoplankton (e.g., diatoms) and mineral particles that are rich in iron oxides and natural organic matter (NOM). The diatom-bound Hg is mostly found on outer surfaces of the cells, suggesting passive sorption of Hg on diatoms. Our results indicate that localized sorption of Hg onto suspended particles, including diatoms and NOM-coated oxide minerals, may play an important role in affecting the partitioning, reactivity, and biogeochemical cycling of Hg in natural aquatic environments.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS1996

Laboratory Measurements of Mineral Dust Scatterring Phase Function and Linear Polarization

With the goal of improving our understanding of how small mineral dust particles scatter light at visible and near-infrared wafelengths we measured the scattering phase function and linear polarization of small mineral dust particles over the scattering angle range 15 to 170 at three wavelengths (0.47, 0.652,and 0.937 m).

minerals dust dust particles SEM scanning electron↗

NASA NTRS2020

Machiite, Al2Ti3O9, a New Oxide Mineral from the Murchison Carbonaceous Chondrite: A New Ultra-refractory Phase from the Solar Nebula

Machiite (IMA 2016-067), Al2Ti3O9, is a new mineral that occurs as a single euhedral crystal, 4.4 mm in size, in contact with an euhedral corundum grain, 12 mm in size, in a matrix of the Murchison CM2 carbonaceous chondrite. The mean chemical composition of holotype machiite by electron probe microanalysis is (wt%) TiO2 59.75, Al2O3 15.97, Sc2O3 10.29, ZrO2 9.18, Y2O3 2.86, FeO 1.09, CaO 0.44, SiO2 0.20, MgO 0.10, total 99.87, giving rise to an empirical formula (based on 9 oxygen atoms pfu) of (Al1.17Sc0.56Y0.10Ti4+0.08Fe0.06Ca0.03Mg0.01)(Ti4+2.71Zr0.28Si0.01)O9. The general formula is (Al,Sc)2(Ti4+,Zr)3O9. The end-member formula is Al2Ti3O9. Machiite has the C2/c schreyerite-type structure with a = 17.10 Å, b = 5.03 Å, c = 7.06 Å, b = 107°, V = 581 Å3, and Z = 4, as revealed by electron backscatter diffraction. The calculated density using the measured composition is 4.27 g/cm3. The machiite crystal is highly 16O-depleted relative to the coexisting corundum grain (D17O = –0.2 ±2.4‰ and –24.1 ± 2.6‰, respectively; where D17O = d17O – 0.52 ×d18O). Machiite is a new member of the schreyerite (V2Ti3O9) group and a new Sc,Zr-rich ultrarefractory phase formed in the solar nebula, either by gas-solid condensation or as a result of crystallization from a Ca, Al-rich melt having solar-like oxygen isotopic composition (D17O ~ –25‰) under high-temperature (~1400–1500 °C) and low-pressure (~10-4–10-5 bar) conditions in the CAI-forming region near the protosun. The currently observed disequilibrium oxygen isotopic composition between machiite and corundum may indicate that machiite subsequently experienced oxygen isotopic exchange with a planetary-like 16O-poor gaseous reservoir either in the solar nebula or on the CM chondrite parent body. The name machiite is in honor of Chi Ma, mineralogist at California Institute of Technology, for his contributions to meteorite mineralogy and discovery of many new minerals representing extreme conditions of formation.

Machiite↗

NASA NTRSDate not supplied

Mineral Processing... In Space

NASA is tasked with exploring the solar system and expanding the U.S. economy into space (among other things). Neither is sustainable over the long term without making use of the natural resources available out there, but the operating environments will be very different from anything encountered in all mineral processing history. This update outlines what’s planned, what’s being studied, and the crucial part that the mineral industry will play.

mineral processing↗

DOE OSTI2022

CORE-CM Williston Basin Carbon Ore, Rare Earth, and Critical Minerals

Fact sheet on the Carbon Ore, Rare Earth and Critical Minerals (CORE-CM) Initiative, an Energy & Environmental Research Center and U.S. Department of Energy project. Includes information on the importance of critical minerals and utilizing lignite from the Williston Basin.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2023

CORE-CM Williston Basin Carbon Ore, Rare Earth, and Critical Minerals

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2026

The National Laboratory of the Rockies Strengthens U.S. Critical Minerals Supply Chains

The National Laboratory of the Rockies (NLR) is working to overcome bottlenecks and secure the U.S. critical mineral supply chain - delivering lower-cost, lower-risk pathways from unconventional and secondary feedstocks to validated products. NLR achieves this through cross-sector partnerships to advance U.S. critical minerals across the mining, processing, manufacturing, usage, and end-of-life stages.

29 ENERGY PLANNING, POLICY, AND ECONOMY↗

DOE OSTI2014

Ice Nucleation of Bare and Sulfuric Acid-coated Mineral Dust Particles and Implication for Cloud Properties

Ice nucleation properties of different dust species coated with soluble material are not well understood. We determined the ice nucleation ability of bare and sulfuric acid coated mineral dust particles as a function of temperature (-25 to -35 deg C) and relative humidity with respect to water (RHw). Five different mineral dust species: Arizona test dust (ATD), illite, montmorillonite, quartz and kaolinite were dry dispersed and size-selected at 150 nm and exposed to sulfuric acid vapors in the coating apparatus. The condensed sulfuric acid soluble mass fraction per particle was estimated from the cloud condensation nuclei activated fraction measurements. The fraction of dust particles nucleating ice at various temperatures and RHw was determined using a compact ice chamber. In water-subsaturated conditions, compared to bare dust particles, we found that only coated ATD particles showed suppression of ice nucleation ability while other four dust species did not showed the effect of coating on the fraction of particles nucleating ice. The results suggest that interactions between the dust surface and sulfuric acid vapor are important, such that interactions may or may not modify the surface via chemical reactions with sulfuric acid. At water-supersaturated conditions we did not observed the effect of coating, i.e. the bare and coated dust particles had similar ice nucleation behavior.

Kulkarni, Gourihar R.↗

DOE OSTI2015

Dissolution of the rare-earth mineral bastnaesite by acidic amide ionic liquid for recovery of critical

Rare-earth elements provide the cornerstones to clean sustainable energy and modern technologies such as computers, communications, and transportation. As such, the recovery of rare earths (REs) from minerals such as bastnaesite remains important for modern times. As the light lanthanides (La–Nd) constitute the majority (typically > 98.7 %) of the REs in bastnaesite with the heavy REs (Sm–Lu) contributing the remainder (approximately 1.3 %), an enrichment of heavier REs may serve as an effective means of assisting rare-earth recovery. Such an extractive metallurgy process involving ionic liquids (ILs) leads to an enrichment of heavy REs by nearly an order of magnitude. The acidic IL N,N-dimethylacetamidium bis(trifluoromethylsulfonyl)imide (DMAH+NTf 2 – ) in the IL 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide (BMIM + NTf 2 – ) dissolves froth flotation bastnaesite, synthetic bastnaesite analogues (RECO 3 F), RE 2 O 3 , and RE 2 (CO 3 ) 3 minerals. Furthermore, an overall reaction for the dissolution of bastnaesite is proposed for this IL system. This IL system may provide the initial stages of a greater RE separation scheme for bastnaesite froth flotation concentrates.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2014

Hydrogenase Activity of Mineral-Associated and Suspended Populations of Desulfovibrio desulfuricans Essex 6

The interactions between sulfate-reducing microorganisms and iron oxides influence a number of important redox-sensitive biogeochemical processes including the formation of iron sulfides. Enzymes, such as hydrogenase which catalyze the reversible oxidation of molecular hydrogen, are known to mediate electron transfer to metals and may contribute to the formation and speciation of ferrous sulfides formed at the cell–mineral interface. In the present study, we compared the whole cell hydrogenase activity of Desulfovibrio desulfuricans strain Essex 6 growing as biofilms on hematite (hematite-associated) or as suspended populations using different metabolic pathways. Hematite-associated cells exhibited significantly greater hydrogenase activity than suspended populations during sulfate respiration but not during pyruvate fermentation. The enhanced activity of the hematite-associated, sulfate-grown cells appears to be dependent on iron availability rather than a general response to surface attachment since the activity of glass-associated cells did not differ from that of suspended populations. Hydrogenase activity of pyruvate-fermenting cells was stimulated by addition of iron as soluble Fe(II)Cl2 and, in the absence of added iron, both sulfate-reducing and pyruvate-fermenting cells displayed similar rates of hydrogenase activity. These data suggest that iron exerts a stronger influence on whole cell hydrogenase activity than either metabolic pathway or mode of growth. The location of hydrogenase to the cell envelope and the enhanced activity at the hematite surface in sulfate-reducing cells may influence the redox conditions that control the species of iron sulfides on the mineral surface.

58 GEOSCIENCES↗

DOE OSTI2019

Identification of hydrogen species in alunite-type minerals by multi-nuclear solid-state NMR spectroscopy

The various hydrogen species present in a series of synthetic hydroniumjarosite ((H3O)Fe3(SO4)2(OH)6), and ammonioalunite ((NH4)Al3(SO4)2(OH)6) as well synthetic potassium (Cr3+ and V3+) and hydronium (V3+, Cr3+, and Ga3+) analogues were identified and quantified by 1H and 2H MAS NMR spectroscopy. The results confirm the defect mechanism proposed for alunite (Nielsen et al., Am Miner 2007, 92, 587), and allow for identification and quantification of even a few percent structural defects. For the paramagnetic samples, the isotropic shift for G2-OH group (V3+, Cr3+, and Fe3+) span more than 1100 ppm, which is related to different d-electron configuration (d2, d3, and d5). Analysis of 1H and 27Al MAS NMR shows that the synthetic ammonioalunite contains small amounts (5-10%) of hydronium. Furthermore, the close structural relationship between of hydronium and gallium alunite is reflected by the 27Al and 71Ga quadrupole coupling parameters. Thus, the current work demonstrates the applicability of solid state NMR spectroscopy for identification and quantification of hydrogen species in both dia- and paramagnetic minerals.

jarosite, alunite, gallium alunite, solid state NM↗

DOE OSTI2021

Key predictors of soil organic matter vulnerability to mineralization differ with depth at a continental scale

Abstract Soil organic matter (SOM) is the largest terrestrial pool of organic carbon, and potential carbon-climate feedbacks involving SOM decomposition could exacerbate anthropogenic climate change. However, our understanding of the controls on SOM mineralization is still incomplete, and as such, our ability to predict carbon-climate feedbacks is limited. To improve our understanding of controls on SOM decomposition, A and upper B horizon soil samples from 26 National Ecological Observatory Network (NEON) sites spanning the conterminous U.S. were incubated for 52 weeks under conditions representing site-specific mean summer temperature and sample-specific field capacity (−33 kPa) water potential. Cumulative carbon dioxide respired was periodically measured and normalized by soil organic C content to calculate cumulative specific respiration (CSR), a metric of SOM vulnerability to mineralization. The Boruta algorithm, a feature selection algorithm, was used to select important predictors of CSR from 159 variables. A diverse suite of predictors was selected (12 for A horizons, 7 for B horizons) with predictors falling into three categories corresponding to SOM chemistry, reactive Fe and Al phases, and site moisture availability. The relationship between SOM chemistry predictors and CSR was complex, while sites that had greater concentrations of reactive Fe and Al phases or were wetter had lower CSR. Only three predictors were selected for both horizon types, suggesting dominant controls on SOM decomposition differ by horizon. Our findings contribute to the emerging consensus that a broad array of controls regulates SOM decomposition at large scales and highlight the need to consider changing controls with depth.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2019

Problems of Developing Solid Mineral Deposits on the Sea and Ocean Floor

Brief characteristics of the mineral raw material potential of the deep-sea deposits of ferromanganese nodules in the area of the Clarion-Clipperton Zone leased by Russia in the Pacific Ocean are presented. The creation at the Moscow Mining Institute (MGI) of the USSR’s first Scientific and Technical Problems Laboratory and the results of its work on extraction of minerals from the sea and ocean floor are reviewed. The research works carried out by MGI on underwater mining of ilmenite-rutile-zirconium sands on the Baltic Sea shelf and Iturup Island and tin under conditions of northern seas and the development of the technogenic placer of the East Siberian Sea are analyzed. The concept of using the kinetic energy of coaxially swirled fluid jets in hydrotransport-hoisting devices of vortex slurry preparation, which was tested in the Black Sea and an air-lift mud intake by mechanical and hydraulic loosening for extracting diamond-containing gravel-pebble rocks on the Namibia shelf is given.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2026

How exudates production along a phosphorus gradient influences mineral dissolution across contrasting soil development stages

Harnessing rhizosphere processes offers a valuable opportunity to optimize nutrient use efficiency in agroecosystems. In nutrient-limited soils, plants discharge part of photosynthate surplus via root exudation, including carboxylates, which may enhance mineral dissolution and nutrient mobilization. We aimed to assess how plant responses to nutrient limitation translated into changes in exudate profiles, and how these exudates, in turn, drive bioweathering processes across soils of contrasting mineralogy and weathering degree. We conducted a hydroponic experiment with Lupinus albus grown under five phosphorus (P) concentrations (5, 10, 20, 30, and 50 µM) over seven weeks. We measured plant biomass and root traits, performed a metabolomics analysis and quantified seven carboxylates in root exudates using gas chromatography-mass spectrometry. To assess bioweathering processes across contrasted soil domains, we conducted batch dissolution tests with exudates using three soil horizons—35 each with distinct physicochemical properties: enriched in organic matter, iron oxides, or primary silicates. At the intermediate level of P supply, shoot biomass was comparable to that under high P, but plants produced more root biomass and a higher total carboxylate exudation rate. Despite low carboxylate concentrations (<100 ppb), exudates promoted the dissolution of Ca, Mg, Si, Fe, P and K in all horizons. Yet, the degree of element released varied among horizons. These findings highlight the importance of root exudates in enhancing mineral dissolution, with effects dependent on soil physicochemical properties. The results suggest that managing agroecosystems under moderate nutrient limitation could be a sustainable strategy to increase root-to-shoot ratios, enhance bioweathering processes and nutrient release in soil solution.

Pollet, Sasha L.↗

DOE OSTI2019

Density–stiffness scaling in minerals upon disordering: Irradiation vs. vitrification

When subjected to irradiation or vitrification, minerals become disordered at the atomic scale, which, in turn, affect their density and stiffness. However, the nature of the relationship between structural disorder, density, and stiffness remains poorly understood. In this work, based on molecular dynamics simulations, we investigate the effect of irradiation- and vitrification-induced disordering in a series of silicate minerals. We show that irradiation- and vitrification-induced disordering yield comparable, yet not fully equivalent variations in density and stiffness. Interestingly, we report the existence of a power law density–stiffness scaling exhibiting a scaling exponent that is similar to that observed in porous assembled cellular materials.

36 MATERIALS SCIENCE↗