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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 865 records · Page 48
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Compositional effects on cure kinetics, mechanical properties and printability of dual-cure epoxy/acrylate resins for DIW additive manufacturing

Interest in 3D printing of thermoset resins has increased significantly in recent years. One approach to additive manufacturing of thermoset resins is printing dual-cure resins with direct ink write (DIW). Dual-cure resins are multi-component resins which employ an in situ curable constituent to enable net-shape fabrication while a second constituent and cure mechanism contribute to the final mechanical properties of the printed materials. In this work, the cure kinetics, green strength, printability, and print fidelity of dual-cure epoxy/acrylate thermoset resins are investigated. Resin properties are evaluated as a function of acrylate concentration and in situ UV exposure conditions. The acrylate cure kinetics are probed using photo-differential scanning calorimetry and the impacts of resin composition and UV cure profile on the acrylate extent of conversion are presented. Continuous and pulsed UV cure profiles are shown to affect total conversion due to variances in radical efficiency at different UV intensities and acrylate concentrations. The effects of acrylate concentration on the kinetics of the epoxy thermal cure and the final mechanical properties are also investigated using dynamic mechanical analysis and three-point bend measurements. The glass transition temperature is dependent on formulation, with increasing acrylate content decreasing the T g . However, the room temperature shear moduli, flexural moduli, strength, strain-to-failure, and toughness values are relatively independent of resin composition. The similarity of the final properties allows for greater flexibility in resin formulation and in situ cure parameters, which can enable the printing of complex parts that require high green strength. We found that the in situ UV print intensities and exposure profiles that are necessary to achieve the best print quality are not, in most cases, the conditions that maximize conversion of the acrylate network. Lastly, this highlights the importance of developing optimized resin compositions which enable complete cure of the acrylate network by promoting acrylate dark cure or thermal cure.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Effect of N 2 - and CO 2 -containing shielding gases on composition modification and carbonitride precipitation in wire arc additive manufactured grade 91 steel

Additive manufacturing (AM) represents a promising technique to fabricate metallic alloys with greater control of the resulting material features as compared to traditional manufacturing routes. Recently, there is greater interest in AM research on 9 wt% Cr ferritic/martensitic (F/M) steels, which are commonly studied for use in the nuclear energy industry. This work aims to prove that wire arc AM can manufacture F/M steels with adequate mechanical properties in multiple processing atmospheres and aims to study how shielding gas composition can be leveraged during fabrication to induce specific precipitation pathways. The effect of shielding gas composition on MX (M=Nb and/or V, Xdouble bondC and/or N) carbonitride precipitation in a 9 wt% Cr ferritic/martensitic (F/M) steel alloy known as Grade 91 was studied using N 2 and CO 2 gas additions to an inert Ar shielding gas atmosphere during wire arc AM. The N and C atoms present in the processing atmospheres were absorbed into the melt pools during fabrication. Due to their differing affinities for precipitate-forming reactions, the varying levels of C and N between the samples contributed to differences in final carbonitride composition and morphologies. Such precipitate behavior is of interest as carbonitrides have been shown to contribute to increased mechanical performance. This increased performance was studied via electron microscopy and tested for strength, ductility, and fracture properties.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Energy absorption of architectured PrintCast interpenetrating composites in tension

Additively manufactured (AM) metal-metal composites consisting of PrintCasted 316 L austenitic stainless-steel lattice structures infiltrated with A356 casting alloy, have recently been developed for use in high energy absorption systems with potential applications ranging from static load bearing to dynamic blast containment structures. This system has a unique mechanical behavior as the volume fraction of lattice increases showing a transition from localized to de-localized failure and dramatic increase in energy absorption capability. In this work, PrintCast A356/316 L composite tensile specimens were produced with lattice volume fractions ranging from 20 % to 50 % to capture the range of this behavior. Finite element simulations support neutron diffraction measurements of stress state. Results illustrate that in tension, the reinforcement material is in tension while the matrix support material is in compression, information offering significant insight into the transition to de-localized failure. Moreover, the simulation results provide further insight into how interfacial bonding (or lack of bonding) affects the energy absorption capabilities of the PrintCast composites.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Radiation damage of a two-dimensional carbon fiber composite (CFC)

Carbon fiber composites (CFC) are, among other applications, already in use as low-impedance collimating elements for intercepting TeV-level protons machines, like the CERN Large Hadron Collider. Towards a comprehensive understanding of these materials’ properties and behavior, a series of radiation damage campaigns have been undertaken in order to quantitively investigate the response of AC-150 K CFC to high proton fluences. The CFCs dimensional changes, stability, micro-structural evolution, and structural integrity below and above 5 × 10 20 p/cm 2 fluence threshold were studied. The irradiating particles were protons of kinetic energies in the range of 130–200 MeV. The effects of the irradiation temperature (~90–180°C and 280–500°C) combined with the proton fluence on the dimensional stability and the microstructural evolution of this anisotropic two-dimensional composite structure were studied using precision dilatometry and X-ray diffraction. Our results shed light on the fluence-based limitations for these composite materials. Furthermore, we compare these results with reference unirradiated graphite, and we discuss the similarities and differences in the dimensional changes and post-irradiation annealing properties.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Polymer-cement composites with adhesion and re-adhesion (healing) to casing capability for geothermal wellbore applications

Deterioration of cement/casing adhesion in wellbore scenarios can result in unwanted and potentially harmful leakage with the potential of serious repair costs. In this work, we explore the use of self-healing polymers added to conventional wellbore cements as a way to bring about self-healing and readhering (to steel casing) properties to the composite material. The polymers are pH resistant and seem to improve the cement integrity after exposure to typical chemical and thermal stresses encountered under geothermal wellbore conditions. We find that addition of about 10-15 wt% of polymer to the cement visually increases its resistance to fracturing from exposure to geothermal conditions, while the adhesive strength of cement/stainless steel increases with curing time for a period of about 10 days. Self-healing capability was demonstrated by permeability analysis showing that polymer-cement composites reduce flow by 50-70% at cement bulk and at the cement/steel interface. Use of atomistic simulations imply that these polymers have good wetting properties on the steel surfaces. Analysis of the interactions between steel/polymer and cement/polymer show that they are complementary, resulting in a wider range of bonding patterns. Cracks are likely to expose under-coordinated sites that result in more bonding interactions, which agrees well with the permeability measurements showing high degree of healed cracks and healed (cement-steel) interfacial gaps together with an overall increased in structural integrity of these advanced polymer-cement composite materials.

Rod, Kenton A.↗
DOE OSTI2021

Development and characteristics of ultra high-performance lightweight cementitious composites (UHP-LCCs)

Highlights: • An ultra high-performance lightweight cementitious composite (UHP-LCC) was designed. • The UHP-LCCs had ultra high strength (>120 MPa) and very low density (3 ). • The UHP-LCCs had high structural efficiency, good functional properties and superior durability. • The strategies and mechanisms on achieving UHP-LCCs with excellent performance were proposed. High strength and light weight are two recent opposite development trends of concrete. This study proposed a design concept of an ultra high-performance lightweight cementitious composite (UHP-LCC), which had a compressive strength of higher than 120 MPa and an air-dried density down to around 1800 kg/m{sup 3}. The UHP-LCCs were innovatively developed by incorporating micro-sized hollow particles with a high strength shell (hollow glass microspheres, HGM) into an ultra-high performance cementitious composite (UHPC). The roles of HGM in the UHP-LCCs were investigated by evaluating the reactivity of the HGM and the mechanisms on achieving the excellent mechanical properties, low density and superior durability were revealed. The Chapelle test results showed that the HGM exhibited some pozzolanic reactivity, which facilitated the reaction between the shell of HGM and the alkali hydration products of the paste matrix. This chemical reaction was conducive to improving the HGM-paste interface and enhancing the mechanical properties. With the use of microspheres with a high stiff shell, the fundamental properties of the UHP-LCCs including thermal insulation, sound absorption, resistance to water ingress and electrical resistivity were improved significantly. The strategies for preparing the UHP-LCCs with high structural efficiency and great performance were proposed. The results of this study provide a new approach for designing and producing a lightweight UHPC, which would be a promising material for long-span structures.

36 MATERIALS SCIENCE↗
DOE OSTI2020

UO 2 + 5 vol% ZrB 2 nano composite nuclear fuels with full boron retention and enhanced oxidation resistance

The boron isotope ( 10 B) can be used as a neutron absorber in UO 2 to control the reactivity of nuclear fuel pellets, however, the boron source can react with oxygen source in UO 2 to form B 2 O 3 that vaporize readily at temperatures above 1200 °C. Unfortunately, the sintering of UO 2 fuel requires hours holding at high temperature (>1700 °C), resulting in an inevitable B loss during sintering and unpredictable B concentration in final product. It is challenging to incorporate boron through a conventional sintering method. In this work, we demonstrated that spark plasma sintering (SPS), a field assisted sintering technology, can effectively densify UO 2 + 5 vol% ZrB 2 composite fuel pellets by rapid consolidation at 1600 °C for a short duration of 5 min under an applied pressure of 40 MPa. Further, thermogravimetric analysis (TGA) measurements confirm that ZrB 2 is fully retained inside the composite fuel pellets. Inside the composite fuel pellets, nano sized ZrB 2 particles are uniformly distributed along the grain boundaries of the UO 2 matrix. The ZrB 2 particle transforms to a glassy B 2 O 3 phase covering the sample surface and grain boundaries of UO 2 matrix after a simple post-sintering annealing at 1000 °C in flowing Argon gas for 4 h. The formed glassy B 2 O 3 slows down the diffusion of oxygen ions and postpones the onset temperature for oxidation of UO 2 from 400 °C to 550 °C. This study demonstrates the capability of SPS, an advanced fuel manufacturing technique, to achieve a full retention of ZrB 2 in UO 2 oxide fuel and increase oxidation resistance through a simple post-sintering annealing. The reported work holds great engineering potential for development of advanced oxide fuel for nuclear application.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2026

Optimizing a chemical cleaning protocol to determine the nickel isotopic composition of ancient seawater from carbonates

Reconstructing the ancient marine cycle of Ni, a trace metal in the oceans essential to enzymes regulating the C, N, and O cycles, would inform how Ni bioavailability shaped early life. The Ni isotopic composition of seawater (δ 60 Ni SW ) through time could provide insight, but this approach requires sedimentary archives that faithfully record δ 60 Ni SW . Carbonates are an often-used record of seawater chemistry, but contaminants could bias the measured δ 60 Ni of bulk sediment. To isolate the true carbonate-bound δ 60 Ni signal, we optimized a chemical cleaning protocol designed to minimize non‑carbonate Ni contributions and maximize carbonate recovery. We analyzed ODP Site 1007 sediments and evaluated oxidative and reductive pre-cleaning steps and carbonate dissolution protocols. Our results show that only reductive cleaning significantly altered the subsequent carbonate leachate composition, lowering Ni/Ca ratios by up to 60% and δ 60 Ni values by as much as 0.4 ‰. In contrast, δ 60 Ni values were largely insensitive to premature carbonate dissolution during pre-cleaning or to partial leaching of silicates during carbonate dissolution, even at higher acid molarities or longer reaction times. We recommend an evidence-based protocol that removes hydro-soluble salts and clays, applies reductive cleaning and oxidative cleaning for certain sample compositions, and dissolves carbonate using 0.5 M acetic acid, adjusted to pH 5. Using these results, we infer a ∼ 0.9 ‰ Ni isotopic fractionation between chemically cleaned deep-water carbonates (+0.4 ± 0.1 ‰) and deep seawater. This method development is a key step toward accurately reconstructing ancient marine Ni cycles.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Optimal toolpath design of additive manufactured composite cylindrical structures

Structural design optimization for additive manufacturing is primarily focused on planar layer-by-layer processes and design of composite cylindrical structures does not often accommodate manufacturing constraints. In this study, we propose to optimize the toolpath trajectory of additively manufactured composite cylinders comprised of multiple thin cylindrical annuli. Additionally, our printing process is based on direct ink writing in which short carbon fibers in a thermoset resin are extruded through a moving nozzle to build up a structure. Since the fibers are primarily aligned in the flow direction of the extrudate, the printing trajectory influences the material properties of the composite structure. To accommodate this, we define the toolpaths as contours of parameterized level-set functions. This parameterization allows us to optimize the material properties and impose manufacturing constraints such as no-overlap, no-sag, minimum radius of curvature, and continuity of the toolpaths. Several examples illustrate the optimization procedure.

42 ENGINEERING↗
DOE OSTI2025

Impact of gasoline composition on the effects of nitric oxide on autoignition and knock in a DISI engine

Modern spark-ignition engines use exhaust gas recirculation (EGR) to dilute the charge and suppress knock, enabling the use of higher compression ratios and/or more optimum combustion phasing for higher efficiency. The effectiveness of EGR is affected by the composition of the fuel and its chemical-kinetic interactions with combustion products. Among those, nitric oxide (NO) has been shown to strongly affect autoignition reactivity. However, the impact of fuel composition of the effect of NO on reactivity is not well-understood. Here, in this study, engine experiments were conducted to assess the impact of NO seeded to the intake on knock-limited operation of two gasoline fuels (high cycloalkane content, or HCA, and high olefin content, or HO). Results showed that compositionally-different fuels responded differently to NO. HCA, which was less knock-limited than HO for NO < 200 ppm, became more knock-limited for NO > 200 ppm. Moreover, it was found that differences in knock between fuels were caused by differences in autoignition chemistry and not in the sequential autoignition process of the end gas that occurs due to thermal stratification. Chemical kinetic simulations were performed to better understand the experimental results. For HCA, intermediate-temperature heat release had a greater impact on autoignition reactivity than low-temperature heat release, while the opposite was observed for HO. For both fuels, NO enhances the magnitude of low-temperature heat release via NO + HO 2 → NO 2 + OH. The effect of NO on reactivity was stronger for HCA because OH produced from NO helped to overcome the OH quenching effect of cyclopentane, a main species in HCA. In contrast, HO had relatively strong inherent low-temperature chemistry arising from iso-octane, which reduced the impact of NO on reactivity. For the range of NO mole fractions tested in this study, in-cylinder NO increased fuel’s knock propensity, especially for fuels with mild low-temperature chemistry.

Autoignition↗
DOE OSTI2024

Investigation of the notch sensitivity of tailorable long fiber discontinuous prepreg composite laminates

Tailorable discontinuous fiber composite laminates provide relative formability beyond that of continuous fiber laminates, while achieving improved mechanical performance over comparable stochastic systems. Here, in this work, the notch sensitivity of engineered prepreg platelet molded composite (PPMC) laminates is investigated using the open-hole tension (OHT) test and compared to available data for stochastic PPMCs and continuous fiber laminates made with the same material. The press-formed thermoplastic composites (AS4/PEKK) were molded with a quasi-isotropic stacking sequence. The discontinuous PPMC laminate was found to be notch insensitive with OHT strengths ranging from 145.4 MPa (CV $=$ 7%) for d/w $=$ 0.5 to 229.3 MPa (CV $=$ 9%) for d/w $=$ 0.25. The highly ordered meso-structure of the engineered PPMC laminate yields comparatively excellent mechanical properties for relatively thin laminates in contrast to stochastic systems. Both net- and gross-section failures were observed for d/w $=$ 0.25, which suggests that the engineered PPMC laminates studied here maintain a degree of inherent, internal stress concentrations that compete with those caused by geometric features such as a circular hole. Computational simulations of the OHT tests with explicitly represented platelets were found to be in good agreement with experimental measurements. The progressive failure analysis was used to conduct a numerical investigation of the stacking sequence and platelet meso-morphology.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Surviving nanoscale interfacial stability in extreme thermal expansion contrast Zn(CN) 2 -epoxy resin matrix composites

Here, we report the remarkable stability at the nanoscale matrix-filler interface in a series of overall low coefficient of thermal expansion (CTE) zinc cyanide (ZC)/epoxy resin composites. These interfaces demonstrate the stability of highly contrasting materials. These composites are designed to optimize the properties of both materials: epoxy resins are valued for their high strength, superb chemical resistance, low dielectric properties, and adhesive abilities. ZC, a model flexible framework, exhibits negative thermal expansion (NTE) behavior and compensates for the epoxy resin’s detrimentally large thermal expansion values. Filled resins minimize the native 65 ppm/°C CTE values to 19 ppm/° C over a wide temperature range while maintaining linearity, yielding composites compatible with typical metal and ceramic substrates’—commonly bonded to the resin— 0–20 ppm/° C CTE values. Additionally, with significant intrinsic differences in the materials, we use wide-angle X-ray diffraction and atomic force microscopy to elucidate thermal movement. The ZC/epoxy interface is surprisingly resilient over 1,000 cycles between -55° C and 75° C, extremes typical to aerospace applications. Further, we show that the resin viscosity remains less than 21 Pa*s at up to 30 vol% ZC, an important consideration for workability. We also discuss settling distribution, glass transition temperature, flexural strength, and longevity. All results point favorably towards practical implementation in low thermal expansion application needs: filling the gap in component design.

42 ENGINEERING↗
DOE OSTI2023

Biologically inspired reinforcement using polydopamine of polymer bound composites

Interfacial strength plays a critical role in the mechanical properties of a composite system. In this work, a proven mock high explosive (HE), 5-iodo-2’-deoxyuridine (IDOX) was coated by the adhesive promoting polymer polydopamine (PDA), then formulated with an Estane binder system to form an improved HE mock composite. An extensive comparison study of mechanical properties was performed to determine the effects, if any, of PDA on the composite system. To aid in interpretation of the mechanical test data, neutron reflectometry experiments were performed to determine the thickness and structure of the as deposited PDA films. The mechanical performance of PDA-treated IDOX was then compared to untreated specimens by compression testing in the Brazilian disk geometry. The results strongly suggested that the structure of PDA consists of two layers: one low in density caused by polymer agglomerates attaching to the substrate during polymerization, and the second high in density caused by controlled linear deposition of polydopamine. Finally, the mechanical testing showed that PDA greatly increased the stiffness and yield strength of IDOX based mocks without causing any disruption to the underlying crystal system.

42 ENGINEERING↗
DOE OSTI2024

Pathways to formulate lightweight and ultra-lightweight 3D printable cementitious composites

Here, this paper studies the pathways to formulate lightweight and ultra-lightweight 3D printable cementitious composites. A hybrid approach was proposed by combining the advantages of traditional chemical-induced foaming (foaming approach) and lightweight particulate inclusions (synthetic foam approach). A comprehensive experimental program was conducted to evaluate the effects of foaming agents and fly ash cenosphere (FAC) on the printability, microstructure, mechanical and thermal properties of 3D printed samples. The results showed that the hybrid approach could produce a mixture with a density as low as 470 kg/m 3 while ensuring good flowability and buildability owing to the lubricating effect of foaming and supporting skeleton formed by FAC. In addition, a three-step homogenization procedure was also developed to predict the effective elastic modulus and thermal conductivity of 3D printable cementitious composites and cementitious foam. The findings of the study highlighted the effectiveness of the hybrid approach in formulating 3D printable ultra-lightweight cementitious composites in thermal insulation and acoustic applications.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Evaluation of Phase Change Plaster/Paste Composites for Building Envelopes

Thermal energy storage (TES) materials increase a building’s thermal mass and provide the flexibility to shave and time-shift energy use. These materials are needed to enable grid-interactive efficient buildings, allowing building occupants to lower costs by leveraging free ambient heating/cooling as well as shifting consumption to cheaper electricity periods. Phase change materials (PCMs) that store heat through a solid-liquid/solid-solid transformation are of particular interest for TES because of their ability to store large amounts of energy across a constant temperature or very small temperature range. Furthermore, previous studies on PCM building envelopes evaluated products that may only be incorporated as part of new construction and are not easily applicable to existing, energy-intensive buildings. In this work, we leverage laboratory PCM characterization and whole-building energy simulation to study the energy and cost savings of PCM plaster/paste coatings, which can be applied post construction to both new builds and retrofits of existing buildings (about 40% of residential buildings in the United States fall into the retrofit category). We evaluated the energy impact of PCM plaster/paste composites for a single-family residential building in the United States, including layer design (location and thickness), composite properties (phase change temperature, energy density, and shape of the enthalpy curve), and U.S. climate zone. The enthalpy curve shape of PCM shows that phase change temperature and energy density are not the only two parameters that must be considered for PCM selection. Maximizing the energy density amid the effective TES zone is key to boosting energy savings. We also studied PCM price targets with the aim of achieving reasonable payback periods based on both block and time-of-use electricity rates. Moreover, we developed an empirical equation to provide a rough estimate of the energy savings potential of incorporating PCM without the need to perform detailed simulations. These results will help guide the selection and design of PCM plaster/paste composite elements for residential building envelopes.

ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATION↗
DOE OSTI2022

Carrot rhamnogalacturonan I structure and composition changed during 2017 in California

Detailed composition, fine structure, and function were determined for carrot pomace fiber remaining after commercial juice extraction from carrots harvested at four different times during 2017, in different California, USA locations. This pomace was treated with commercial enzymes and the changes in carbohydrate composition were analyzed. The enzyme-treated carrot pomace contained pectic oligosaccharides that were branched, unsaturated, partially acetylated and methylated rhamnogalacturonan I (RG-I) with arabinogalacto-oligosaccharide side chains as well as free galacto-oligosaccharides and galacturono-oligosaccharides detected by MALDI-TOF MS and NMR analysis. The molecular weight and degree of galacto-oligosaccharide polymerization decreased while water solubility increased following enzymatic treatment. While carrot soluble dietary fiber remained relatively constant, insoluble dietary fiber and total dietary fiber increased during the year. The carrot pomace fiber structure changed between the June and September harvests so that it was more susceptible to enzymatic degradation, and its shape became more linear. The diversity of carrot RG-I oligosaccharide structures was the greatest in the enzyme-treated pomace harvested in September and the RG-I became almost completely debranched by the enzyme treatment for the pomace harvested in December. The structural properties of these carrot pomace fiber fractions suggest that they can function as a low viscosity beverage food ingredient, and the rhamnogalacturonan I structure indicated the potential for anti-viral, immuno-modulatory and prebiotic properties. Furthermore, the rhamnogalacturonan structural composition changes during the growing season highlights the need for bioactivity monitoring of carrot pomace obtained from different sources, and harvested at different times during the year.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2022

Model-based compositional predictions for a differential scanning calorimetry/thermogravimetric analysis-mass spectrometry system used for heat of vaporization measurements

A Differential Scanning Calorimetry/Thermogravimetric Analysis (DSC/TGA) procedure for determination of Heat of Vaporization (HOV) of fuel and surrogate fuel mixtures has been previously utilized for evaluation of oxygenate impacts on spark ignition fuels. This analysis has been further leveraged with mass spectrometry (MS) to elucidate vapor phase compositional changes during evaporation. In this study we focus on a simple system of three compounds (ethanol, n-hexane, and n-octane) to provide a model-based understanding of the evaporation process under these experimental conditions. An Aspen Plus model was set up to provide liquid and vapor phase concentration predictions during mixture evaporation using the initial mixture composition, and measured temperature and mass loss profiles from DSC/TGA experiments. Agreements between the trends of the MS ion count profiles and model composition predictions provide a degree of validation of this modeling approach that can allow the interpretation and extrapolation of DSC/TGA measurements for more complex fuel mixtures.

33 ADVANCED PROPULSION SYSTEMS↗
DOE OSTI2026

Synchrotron resolved microscale mineralogy and elemental composition of individual plinthic and manganiferous nodules from agricultural soils

Iron and manganese oxides are strong sorbents and elemental scavengers in the environment that can form macroscopic nodules in soils. Despite their importance in the geochemical cycling of nutrients and contaminants, nodules are rarely characterized. When analyzed, they are often combined into bulk samples, obscuring individual characteristics. This study investigates the composition and mineralogy of individual plinthic and manganiferous nodules in soil from cropping systems in the Farming Systems Project in Beltsville, Maryland. Elemental composition indicates the accumulation of contaminants and nutrients, including copper in all nodules and high levels of phosphorus in select nodules. Sequential extractions determine that highly crystalline minerals comprise the nodules, locking away these nutrients and contaminants. Bulk X-ray diffraction (XRD) demonstrated distinct mineralogies in the plinthic and manganiferous nodules, with the former comprised of quartz, goethite, and kaolinite, and the latter consisting of quartz, Mn 2 O 3 , and hematite. Synchrotron and laboratory-based X-ray fluorescence (XRF) mapping gives critical insight into the elemental distribution within the nodules and elucidates spatial elemental associations, including the coupling of manganese and iron in the manganiferous nodules. XRF maps paired with µXRD provide microscale spatial resolution in mineralogy, which resolved several phases not apparent in bulk XRD, manganese’s association with goethite, and minerals indicative of redox transformations, including magnetite and maghemite. These novel results provide critical insight into the microscale mineralogy and individual elemental composition of plinthic and manganiferous nodules, as well as how they alter bulk soil geochemistry in ways largely unaccounted for in research on soil systems.

36 MATERIALS SCIENCE↗