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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 145 records · Page 8
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Morphology and composition of Goldeye (Hiodontidae; Hiodon alosoides) otoliths

In this work, we provide up-todate morphological and compositional data on otoliths of the osteoglossomorph Goldeye (Hiodon alosoides). Using computed tomography (CT) X-ray, we documented the location of each of the three pairs of otoliths (lapilli, sagittae, and asterisci) in relation to the swim bladder, which extended forward in close proximity to the sagittae and asterisci. The lappili were the largest otoliths in terms of surface area and volume, but the sagittae were highly modified, appearing spiral in shape when viewed dorsally, with a surface area to volume ratio more than double that of the lapilli. Using scanning electron microscopy, the surface of each otolith was viewable in great detail, and small otoconia (~10.5 μm diameter) were observed on each, but were most numerous on the sagittae. Additionally, on scanning electron micrographs, the sagittae appeared to be bi-lobed, with asymmetrical lobes each oriented in the same general direction. Using neutron and X-ray diffraction methods, we found three polymorphs of calcium carbonate crystals (aragonite, vaterite, and calcite), sometimes all within the same otolith. However, in general, lapilli and sagittae were composed predominately of aragonite whereas asterisci were composed chiefly of vaterite. With these results, we provide information on a unique species, whose inclusion in future studies would benefit our understanding of fish hearing, fish evolution, and fisheries ecology.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2022

Long term performance of pilot methanogenic digester filled with seashell wastes treating slaughterhouse wastes: Biogas production and environmental impact

High ammonia and organic acids contents of decomposed slaughterhouse waste (SHW) often result in the severe inhibition or even failure of the anaerobic digestion (AD). The two-stage AD system can alleviate the ammonia inhibition; however, addition of alkali is often needed to maintain the neutral condition. In this study, seashell wastes containing high percentage of calcium carbonate (CaCO 3 ) were for the first time added in a pilot scale methanogenic digester treating chicken blood waste to retain the microorganisms and provide pH buffers for the substrate. A long-duration performance of this digester was conducted for 400 days under different organic loading rates (OLRs). The results show that methane yields of the digester were 244.8 and 224.9 mL g –1 COD added at OLR of 0.4 and 0.6 g COD L –1 d –1 , respectively, higher than the results of previous studies treating the similar feedstock. An AD system treating blood wastes of a typical poultry slaughterhouse was also proposed for which energy balance and carbon footprint analyses were conducted. The energy production of 0.35 MJ kg –1 blood and carbon emissions reduction of 0.05 kg CO 2 -eq kg –1 blood can be achieved from treating blood waste of the broiler chicken. Finally, this study reveals that using seashell wastes in an AD treating SHW can facilitate the reuse of aquaculture wastes and improve the sustainability of meat industry.

09 BIOMASS FUELS↗
DOE OSTI2023

Statistical 3D morphology characterization of vaterite microspheres produced by engineered Escherichia coli

Hollow vaterite microspheres are important materials for biomedical applications such as drug delivery and regenerative medicine owing to their biocompatibility, high specific surface area, and ability to encapsulate a large number of bioactive molecules and compounds. We demonstrated that hollow vaterite microspheres are produced by an Escherichia coli strain engineered with a urease gene cluster from the ureolytic bacteria Sporosarcina pasteurii in the presence of bovine serum albumin. We characterized the 3D nanoscale morphology of five biogenic hollow vaterite microspheres using 3D high-angle annular dark field scanning transmission electron microscopy (HAADF-STEM) tomography. Using automated high-throughput HAADF-STEM imaging across several sample tilt orientations, we show that the microspheres evolved from a smaller more ellipsoidal shape to a larger more spherical shape while the internal hollow core increased in size and remained relatively spherical, indicating that the microspheres produced by this engineered strain likely do not contain the bacteria. The statistical 3D morphology information demonstrates the potential for using biogenic calcium carbonate mineralization to produce hollow vaterite microspheres with controlled morphologies.

3D morphology↗
DOE OSTI2021

Formation, structure, and thermal stability evolution of ternesite based on a single-stage sintering process

Highlights: • The synthesis of high-purity ternesite based on a single-stage sintering process was firstly studied. • The formation mechanism and crystallization behaviour of ternesite during sintering were investigated. • The structure perfection and symmetry of ternesite crystals were increased with its growth. • The growth and structural development of ternesite crystals during sintering resulted in a higher thermal stability of itself. Ternesite was prepared via a single-stage solid-state reaction from stoichiometric quantities of the CaCO{sub 3}, SiO{sub 2} and CaSO{sub 4}·2H{sub 2}O precursors. In this paper, the formation, structure, and thermal stability evolution of ternesite during sintering were investigated ex situ after quenching. The optimal sintering temperature for the formation of high-purity ternesite was approximately 1200 °C for 12 h, of which the purity level can reach as high as 96.3%. The results from scanning electron microscopy analysis suggest that the formation of ternesite benefited from the preformation of the intermediate silicate phase. Increasing the sintering temperature from 1100 °C to approximately 1250 °C was favourable for the growth of ternesite crystals, and a prolonged duration can also promote this behaviour. The structural perfection and symmetry of ternesite crystals increased with its growth, which was demonstrated by a multimethod approach. By means of thermal analysis, the growth and structural development of ternesite crystals during sintering eventually resulted in a higher thermal stability.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Comparative analysis of various pretreatments to mitigate fouling and scaling in membrane distillation

Membrane distillation (MD) has shown strong promise for treating hypersaline produced water (PW) streams. Scaling and fouling on the membrane surface, however, have been identified as major challenges for commercialization and widespread application. The focus of this study was to first identify the nature of foulants and scalants on the membrane surface and then investigate the pretreatment strategies that mitigate the extent of fouling and scaling on the membrane surface. Vacuum MD (VMD) was selected for this study because of its higher flux at more moderate feed temperatures that eventually leads better assessment of fouling and scaling on the membrane surface. VMD flux tests were carried out with three different real PW samples at total dissolved solids concentrations in the range of 120-160 g/L. It was found that an efficient pretreatment prior to MD is required to mitigate the fouling potential of the organic matter, mostly suspended constituents, in PW samples. Suspended organics fouled and quickly wetted the MD membrane. Major conventional treatments, including filtration, oxidation, coagulation, air floatation, and aeration were investigated to pretreat the PW before VMD tests. A comprehensive comparative analysis is presented showing that the ultrafiltration and coagulation pretreatments displayed the best performance in mitigating the fouling and scaling, while oxidative pretreatment was found to be effective in reducing the iron concentration to less than 5 ppm. The surface of scaled membranes was carefully characterized to further evaluate the performance of each pretreatment. The components that had the highest tendency to precipitate on the membrane surface were identified as strontium sulfate, calcium carbonate, sodium chloride, iron oxide, and silica. In closing, these findings are supported by thermodynamic estimation of the saturation index.

42 ENGINEERING↗
DOE OSTI2021

Bioinspired energy absorbing material designs using additive manufacturing

Nature provides many biological materials and structures with exceptional energy absorption capabilities. Few, relatively simple molecular building blocks (e.g., calcium carbonate), which have unremarkable intrinsic mechanical properties individually, are used to produce biopolymer-bioceramic composites with unique hierarchical architectures, thus producing biomaterial-architectures with extraordinary mechanical properties. Several biomaterials have inspired the design and manufacture of novel material architectures to address various engineering problems requiring high energy absorption capabilities. For example, the microarchitecture of seashell nacre has inspired multi-material 3D printed architectures that outperform the energy absorption capabilities of monolithic materials. Using the hierarchical architectural features of biological materials, iterative design approaches using simulation and experimentation are advancing the field of bioinspired material design. However, bioinspired architectures are still challenging to manufacture because of the size scale and architectural hierarchical complexity. Notwithstanding, additive manufacturing technologies are advancing rapidly, continually providing researchers improved abilities to fabricate sophisticated bioinspired, hierarchical designs using multiple materials. This review describes the use of additive manufacturing for producing innovative synthetic materials specifically for energy absorption applications inspired by nacre, conch shell, shrimp shell, horns, hooves, and beetle wings. Potential applications include athletic prosthetics, protective head gear, and automobile crush zones.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Sulfate-Controlled Heterogeneous CaCO 3 Nucleation and Its Non-linear Interfacial Energy Evolution

Unveiling the effects of an environmental abundant anion “sulfate” on the formation of calcium carbonate (CaCO 3 ) is essential to understand the formation mechanisms of biominerals like corals and brachiopod shells, as well as the scale formation in desalination systems. However, it was experimentally challenging to elucidate the sulfate–CaCO 3 interactions at the explicit first step of CaCO 3 formation: nucleation. In addition, there is limited quantitative information on the precise control of nucleation kinetics. Here, heterogeneous CaCO 3 nucleation is monitored in real time as a function of sulfate concentrations (0–10 mM Na 2 SO 4 ) using synchrotron-based grazing incidence X-ray scattering techniques. The results showed that sulfate can be incorporated in the nuclei, resulting in a nearly 90% decrease in the CaCO 3 nucleation rate, causing a 120% increase in the CaCO 3 nucleus size, and inhibiting the vaterite-to-calcite phase transformation. Moreover, this work quantitatively relates sulfate concentrations to the effective interfacial energies of CaCO 3 and finds a non-linear trend, suggesting that CaCO 3 heterogeneous nucleation is more sensitive at a low sulfate concentration. This study can be readily extended to study other additives and obtain quantitative relationships between additive concentrations and CaCO 3 interfacial energies, a key step toward achieving natural and engineered controls on CaCO 3 nucleation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Effect of Bicarbonate, Calcium, and pH on the Reactivity of As(V) and U(VI) Mixtures

Natural or anthropogenic processes can increase the concentration of uranium (U) and arsenic (As) above the maximum contaminant levels in water sources. Bicarbonate and calcium (Ca) can have major impacts on U speciation and can affect the reactivity between U and As. We therefore investigated the reactivity of aqueous U and As mixtures with bicarbonate and Ca for acidic and neutral pH conditions. In experiments performed with 1 mM U and As mixtures, 10 mM Ca, and without added bicarbonate (pCO 2 = 3.5), aqueous U decreased to <0.25 mM at pH 3 and 7. Aqueous As decreased the most at pH 3 (~0.125 mM). Experiments initiated with 0.005 mM As and U showed similar trends. X-ray spectroscopy (i.e., XAS and EDX) and diffraction indicated that U-As-Ca- and U-Ca-bearing solids resemble uranospinite [Ca(UO 2 ) 2 (AsO 4 ) 2 ·10H 2 O] and becquerelite [Ca(UO 2 ) 6 O 4 (OH) 6 ·8(H 2 O)]. These findings suggest that U-As-Ca-bearing solids formed in mixed solutions are stable at pH 3. However, the dissolution of U-As-Ca and U-Ca-bearing solids at pH 7 was observed in reactors containing 10 mM bicarbonate and Ca, suggesting a kinetic reaction of aqueous uranyl-calcium-carbonate complexation. Our study provides new insights regarding U and As mobilization for risk assessment and remediation strategies.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2024

Modulating the Contact Angle between Nonpolar Polymers and SiO 2 Nanoparticles

Polymer–nanoparticle interactions play an important role in determining the morphology and properties of polymer nanocomposites and controlling the polymeric reactions involving heterogeneous catalysts. Here, in this study, we modulate the interactions between nonpolar polymers and nanoparticles by modifying the nanoparticle surface chemistry and quantify the interaction strength through direct contact angle measurements. We investigate the interactions of three nonpolar polymers, polystyrene, polyethylene, and polycyclooctene, with silica nanoparticles whose surface chemistry has been modified by atomic layer deposition of titania and calcium carbonate and by alkyl silanization. Significant differences in polymer–nanoparticle interactions are observed, which can be attributed to differences in the polarizability of the polymers and oxide surface composition. Compared to fully hydrogenated polycyclooctene, polycyclooctene is shown to have stronger interactions with most metal oxides; however, this trend is reversed following alkyl silanization of the silica nanoparticles, which makes the surface of the particles less polar. These differences in interactions can be leveraged to make polymer nanocomposites with unique properties and enable the selective conversion of polymers without the need for separations.

36 MATERIALS SCIENCE↗
DOE OSTI2024

In Situ Monitoring the Nucleation and Growth of Nanoscale CaCO 3 at the Oil–Water Interface

Interfaces can actively control the nucleation kinetics, orientations, and polymorphs of calcium carbonate (CaCO 3 ). Prior studies have revealed that CaCO 3 formation can be affected by the interplay between chemical functional moieties on solid–liquid or air–liquid interfaces as well as CaCO 3 ’s precursors and facets. Yet little is known about the roles of a liquid–liquid interface, specifically an oil–liquid interface, in directing CaCO 3 mineralization which are common in natural and engineered systems. Here, in this study, by using in situ X-ray scattering techniques to locate a meniscus formed between water and a representative oil, isooctane, we successfully monitored CaCO 3 formation at the pliable isooctane–water interface and systematically investigated the pivotal roles of the interface in the formation of CaCO 3 (i.e., particle size, its spatial distribution with respect to the interface, and its mineral phase). Different from bulk solution, ∼5 nm CaCO 3 nanoparticles form at the isooctane–water interface. They stably exist for a long time (36 h), which can result from interface-stabilized dehydrated prenucleation clusters of CaCO 3 . There is a clear tendency for enhanced amounts and faster crystallization of CaCO 3 at locations closer to isooctane, which is attributed to a higher pH and an easier dehydration environment created by the interface and oil. Our study provides insights into CaCO 3 nucleation at an oil–water interface, which can deepen our understanding of pliable interfaces interacting with CaCO 3 and benefit mineral scaling control during energy-related subsurface operation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Mine Tailings Valorization by Electrochemically Stimulated Mineralization from Mildly Acidic Conditions

This study presents a high-efficiency electrochemical process for the mineralization of calcium carbonate (CaCO 3 ) from mildly acidic mine tailing supernatant water. Electrochemical pH control was used to promote carbonate speciation and precipitation from CO 2 -saturated solutions, achieving >1 mol CaCO 3 precipitated per mol e - at applied potentials between -1.4 and -1.6 V vs Ag/AgCl. Product morphology and polymorph selectivity were tunable via applied potential, yielding calcite and vaterite phases. Experiments using real mine tailings water confirmed selective calcite precipitation, despite the presence of sulfate and other trace elements. These results highlight a viable route for coupling CO 2 utilization with mine tailings valorization.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Exponential crystallization in corals

Corals form their reef-building aragonite (CaCO 3 ) skeletons via transient precursor phases yet understanding of the dynamics of these early-stage transformations remains incomplete. Using time-independent myriad mapping (MM) at 50 nm resolution, we map five mineral phases near the skeleton surface of Stylophora pistillata corals grown in varying seawater pH. All precursors, crystalline and amorphous, exhibit a consistent exponential decay from the growth front, with a shared decay length of 0.7 ± 0.1 μm, independent of time, phase, or pH. This spatial decay, paired with the constant growth rate of the skeleton, reveals a decay time of 5.1 ± 0.5 minutes. The dominant precursor is not amorphous but crystalline: calcium carbonate hemihydrate (CCHH, CaCO₃·½H₂O). These results suggest that exponential crystallization kinetics govern coral biomineralization and may be a widespread feature in biogenic, geologic, and synthetic systems—traceable long after initial mineral deposition.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2022

Probing elemental speciation in hydrochar produced from hydrothermal liquefaction of anaerobic digestates using quantitative X-ray diffraction

Valorization of hydrochar, a solid byproduct from hydrothermal liquefaction (HTL) of anaerobically-digested agriculture wastes (digestates), requires fundamental knowledge of elemental speciation. This study investigated the effects of reaction temperatures (320–360 °C), digestate pH (3.5–8), and digestate cellulose-to-lignin ratios (0.2–1.8) on the speciation (chemical form) and composition of organics and inorganics in hydrochars produced during hydrothermal treatment. Quantitative X-ray diffraction (XRD) method was the primary technique used to characterize hydrochars. The comprehensive XRD pattern processing including the Rietveld refinement protocols demonstrated that the organic phase was comprised of mostly crystalline monocyclic, heterocyclic, and polycyclic aromatics with diverse aliphatic and aromatic substituents, while the inorganic mineral phase consisted of calcium-phosphates, magnesium-phosphates, calcium-carbonates, and magnesium-carbonates. Further, XRD results were validated by the elemental yields of products and the distribution of chemical functionalities measured using solid-state nuclear magnetic resonance (NMR) spectroscopy. The characterization data were used to evaluate proposed mechanistic pathways using compositional analysis of biocrude and aqueous-phase coproducts. Mechanistic pathways developed in the study suggested that benzoic acids, phenols, benzaldehydes, phenolic aldehydes, α-dicarbonyls, and α-hydroxycarbonyls were responsible for the precipitation of organics through various reactions depending on operating conditions. Meanwhile, the formation of inorganic compounds appeared to be consistently represented by reactions including dehydration, hydrolysis, endergonic reduction, and structure rearrangement of native minerals in the digestates. This study provides basic knowledge needed to create and assess potential elemental speciation pathways. In addition, the results of the study facilitate the specification of process conditions to optimize targeted utilization routes of hydrochar for more economically-feasible and sustainable HTL processing.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

The corrosion behavior of borosilicate glass in the presence of cementitious waste forms

Borosilicate glasses are widely used for radioactive waste disposal due to their ability to incorporate a variety of contaminants and radionuclides while exhibiting high durability in various disposal scenarios. This research evaluated the dissolution of borosilicate glass using both single-pass-flow-through (ASTM C1662-18) and product consistency test (ASTM C1285-21) methods with different solutions, including a cementitious-contacted water (called grout-contacted, GC, from this point) and solutions with varying levels of dissolved cementitious species such as Si, Ca, Al. Here, the results indicated that the presence of Ca plays a crucial role in suppressing glass corrosion, as evidenced by the slower normalized dissolution rates, which were one order of magnitude lower for boron and two orders of magnitude lower for rhenium, observed in both Ca-amended and GC solutions compared to the pH 12 buffer solution. This effect is attributed to the formation of a dense, low-porosity, and strongly bonded calcium silicate hydrate (CSH) layer on the glass surface, which implies that a glass corrosion process is influenced by ion exchange involving alkali ions Na + , K + , Ca 2+ , and hydrogen-containing species. A small number of glass particles treated in the GC solution showed minor corrosion pits in the form of shallow craters with an average diameter of approximately 500 μm. This observation is correlated with a significant reduction, 2000 to 3000 times lower, in the cumulative volume of glass pores, indicating that smaller pore voids were “sealed” in the presence of Ca 2+ ions, likely attributed to the formation of CSH precipitation or other corrosion products such as calcium carbonate saturated from the grout solution. These findings suggest that the presence of dissolved Ca in the GC solution can slow down the dissolution of borosilicate glass, contrary to the expected trend of higher dissolution rates resulting from exposure to high alkaline and thus higher pH solutions.

36 MATERIALS SCIENCE↗
DOE OSTI2020

From particle attachment to space-filling coral skeletons

Reef-building corals and their aragonite (CaCO 3 ) skeletons support entire reef ecosystems, yet their formation mechanism is poorly understood. Here we used synchrotron spectromicroscopy to observe the nanoscale mineralogy of fresh, forming skeletons from six species spanning all reef-forming coral morphologies: Branching, encrusting, massive, and table. In all species, hydrated and anhydrous amorphous calcium carbonate nanoparticles were precursors for skeletal growth, as previously observed in a single species. The amorphous precursors here were observed in tissue, between tissue and skeleton, and at growth fronts of the skeleton, within a low-density nano- or microporous layer varying in thickness from 7 to 20 µm. Brunauer-Emmett-Teller measurements, however, indicated that the mature skeletons at the microscale were space-filling, comparable to single crystals of geologic aragonite. Nanoparticles alone can never fill space completely, thus ion-by-ion filling must be invoked to fill interstitial pores. Such ion-by-ion diffusion and attachment may occur from the supersaturated calcifying fluid known to exist in corals, or from a dense liquid precursor, observed in synthetic systems but never in biogenic ones. Concomitant particle attachment and ion-by-ion filling was previously observed in synthetic calcite rhombohedra, but never in aragonite pseudohexagonal prisms, synthetic or biogenic, as observed here. Models for biomineral growth, isotope incorporation, and coral skeletons’ resilience to ocean warming and acidification must take into account the dual formation mechanism, including particle attachment and ion-by-ion space filling.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2024

A molecular view of peptoid-induced acceleration of calcite growth

The extensive deposits of calcium carbonate (CaCO 3 ) generated by marine organisms constitute the largest and oldest carbon dioxide (CO 2 ) reservoir. These organisms utilize macromolecules like peptides and proteins to facilitate the nucleation and growth of carbonate minerals, serving as an effective method for CO 2 sequestration. However, the precise mechanisms behind this process remain elusive. In this study, we report the use of sequence-defined peptoids, a class of peptidomimetics, to achieve the accelerated calcite step growth kinetics with the molecular level mechanistic understanding. By designing peptoids with hydrophilic and hydrophobic blocks, we systematically investigated the acceleration in step growth rate of calcite crystals using in situ atomic force microscopy (AFM), varying peptoid sequences and concentrations, CaCO 3 supersaturations, and the ratio of Ca 2+ / HCO 3 − . Mechanistic studies using NMR, three-dimensional fast force mapping (3D FFM), and isothermal titration calorimetry (ITC) were conducted to reveal the interactions of peptoids with Ca 2+ and HCO 3 − ions in solution, as well as the effect of peptoids on solvation and energetics of calcite crystal surface. Our results indicate the multiple roles of peptoid in facilitating HCO 3 − deprotonation, Ca 2+ desolvation, and the disruption of interfacial hydration layers of the calcite surface, which collectively contribute to a peptoid-induced acceleration of calcite growth. These findings provide guidelines for future design of sequence-specific biomimetic polymers as crystallization promoters, offering potential applications in environmental remediation (such as CO 2 sequestration), biomedical engineering, and energy storage where fast crystallization is preferred.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Shapes of ideal stalagmites

Stalagmites are isolated columns of calcium carbonate growing on a cave floor; their growth is driven by the constant dripping of supersaturated solutions from the roof of the cave. In this paper, we derive a closed-form expression for the shape of a steadily growing stalagmite. Our analysis gives rise to three distinct shapes, all of them observable in nature, with the shape characterized by a single dimensionless parameter. Transitions between different shapes occur at a specific value of this parameter, with additional selection rules determining the shape and size of stalagmites evolving under specific cave conditions. Our theory shows that the stalagmite shape influences the 13 C isotope shifts, which are an important source of paleoclimatic information.

invariant growth↗