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At least 847 records · Page 47

Size dependence of magnetorheological properties of cobalt ferrite ferrofluid

Cobalt Ferrite nanoparticles were synthesized using co-precipitation method at reaction temperatures of 40°C and 80°C. X-Ray diffraction studies confirm cubic phase formation. The average crystallite sizes were found to be ∼30nm and ∼48nm for 40°C sample and 80°C sample respectively. Magnetic properties measured using vibrating sample magnetometer show higher coercivety and magnetization for sample prepared at 80°C. Magnetorheological properties of CoFe2O4 ferrofluids were measured and studied.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Facile Synthesis of Spinel Ferrites with Enhanced Magnetic Properties from Two Intractable Metallurgical Resources: Zinc-Bearing Dust and Nickel Laterite Ore

Nickel laterite ore and zinc-bearing dust are multi-metal-associated and intractable resources. Comprehensive and cooperative utilization of zinc-bearing dust and nickel laterite ore for the preparation of spinel ferrites with enhanced magnetic properties by a facile process was proposed. The structure and magnetic properties of as-prepared spinel ferrites were characterized by X-ray diffraction (XRD), Raman spectroscopy, and Physical Property Measurement System (PPMS). The effect of mass ratios of zinc-bearing dust to nickel laterite ore, calcination temperature, and Zn substitution content on the as-prepared samples was investigated in detail. A single phase of Zn-substituted spinel ferrites (x= 0.00, 0.10, 0.20, and 0.30) could be obtained when the mass ratios were controlled at 1:0.4, 1:4:1.8, 1:2:1.5, and 1:1:1.2 after being calcined at 900 {sup ∘}C for 30 min, respectively. The magnetic property tests present that the as-prepared spinel ferrite exhibits enhanced magnetic properties with the saturation magnetization (Ms) value of 66.8 emu g{sup − 1} and the coercivity (Hc) value of 26 Oe when the mass ratio was controlled at 1:1:1.2. This research could provide an effective way to transfer two intractable resources into soft magnetic materials.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

GeoSoilEnviroCARS (Sector 13) at the Advanced Photon Source: a comprehensive synchrotron radiation facility for Earth science research at ambient and extreme conditions

GeoSoilEnviroCARS (GSECARS) is a comprehensive analytical laboratory for Earth and environmental science research using X-ray beams from the Advanced Photon Source, Argonne National Laboratory. State-of-the-art instruments are available for (1) high-pressure/high- or low-temperature diffraction, total scattering, and spectroscopy (Brillouin, Raman, and VIS-IR) using the laser heated diamond anvil cell (DAC); (2) high-pressure/high-temperature diffraction, scattering, and imaging as well as acoustic emission (AE) and ultrasonics using the large-volume press (LVP); (3) powder, single crystal, and surface/interface diffraction; (4) X-ray absorption fine structure spectroscopy; (5) X-ray fluorescence microprobe analysis; and (6) microtomography. As shown here, experiments are facilitated by senior level staff who collaborate on all aspects of the analytical work including experiment design, sample preparation, data collection, data interpretation, and publication preparation. Both technical and scientific synergies occur as a result of the intimate association of the various techniques and scientists experienced in the applications of synchrotron radiation to Earth, environmental, and planetary science problems. The facility includes state-of-the-art instrumentation designed and built in-house, including custom X-ray optics, online and offline laser-based systems, specialized sample environments and positioning systems, as well as pixel-array and multi-crystal energy dispersive X-ray detectors, which are available to be shared among the experimental stations.

36 MATERIALS SCIENCE↗

A comparison of methods used to unveil the genetic and metabolic pool in the built environment

BACKGROUND:A majority of indoor residential microbes originate from humans, pets, and outdoor air and are not adapted to the built environment (BE). Consequently, a large portion of the microbes identified by DNA-based methods are either dead or metabolically inactive. Although many exceptions have been noted, the ribosomal RNA fraction of the sample is more likely to represent either viable or metabolically active cells. We examined methodological variations in sample processing using a defined, mock BE microbial community to better understand the scope of technique-based vs. biological-based differences in both ribosomal transcript (rRNA) and gene (DNA) sequence community analysis. Based on in vitro tests, a protocol was adopted for the analysis of the genetic and metabolic pool (DNA vs. rRNA) of air and surface microbiomes within a residential setting. RESULTS:We observed differences in DNA/RNA co-extraction efficiency for individual microbes, but overall, a greater recovery of rRNA using FastPrep (> 50%). Samples stored with various preservation methods at - 80°C experienced a rapid decline in nucleic acid recovery starting within the first week, although post-extraction rRNA had no significant degradation when treated with RNAStable. We recommend that co-extraction samples be processed as quickly as possible after collection. The in vivo analysis revealed significant differences in the two components (genetic and metabolic pool) in terms of taxonomy, community structure, and microbial association networks. Rare taxa present in the genetic pool showed higher metabolic potential (RNA:DNA ratio), whereas commonly detected taxa of outdoor origins based on DNA sequencing, especially taxa of the Sphingomonadales order, were present in lower relative abundances in the viable community. CONCLUSIONS:Although methodological variations in sample preparations are high, large differences between the DNA and RNA fractions of the total microbial community demonstrate that direct examination of rRNA isolated from a residential BE microbiome has the potential to identify the more likely viable or active portion of the microbial community. In an environment that has primarily dead and metabolically inactive cells, we suggest that the rRNA fraction of BE samples is capable of providing a more ecologically relevant insight into the factors that drive indoor microbial community dynamics.

59 BASIC BIOLOGICAL SCIENCES↗

Deciphering mineralogical changes and carbonation development during hydration and ageing of a consolidated ternary blended cement paste

To understand the main properties of cement, a ubiquitous material, a sound description of its chemistry and mineralogy, including its reactivity in aggressive environments and its mechanical properties, is vital. In particular, the porosity distribution and associated sample carbonation, both of which affect cement's properties and durability, should be quantified accurately, and their kinetics and mechanisms of formation known both in detail and in situ . However, traditional methods of cement mineralogy analysis ( e.g. chemical mapping) involve sample preparation ( e.g. slicing) that can be destructive and/or expose cement to the atmosphere, leading to preparation artefacts ( e.g. dehydration). In addition, the kinetics of mineralogical development during hydration, and associated porosity development, cannot be examined. To circumvent these issues, X-ray diffraction computed tomography (XRD-CT) has been used. This allowed the mineralogy of ternary blended cement composed of clinker, fly ash and blast furnace slag to be deciphered. Consistent with previous results obtained for both powdered samples and dilute systems, it was possible, using a consolidated cement paste (with a water-to-solid ratio akin to that used in civil engineering), to determine that the mineralogy consists of alite (only detected in the in situ hydration experiment), calcite, calcium silicate hydrates (C-S-H), ettringite, mullite, portlandite, and an amorphous fraction of unreacted slag and fly ash. Mineralogical evolution during the first hydration steps indicated fast ferrite reactivity. Insights were also gained into how the cement porosity evolves over time and into associated spatially and time-resolved carbonation mechanisms. It was observed that macroporosity developed in less than 30 h of hydration, with pore sizes reaching about 100–150 µm in width. Carbonation was not observed for this time scale, but was found to affect the first 100 µm of cement located around macropores in a sample cured for six months. Regarding this carbonation, the only mineral detected was calcite.

36 MATERIALS SCIENCE↗

Morphology-controlled LiFePO{sub 4} cathodes by a simple polyol reaction for Li-ion batteries

LiFePO{sub 4} cathodes with secondary nanorod structures and nano-plate morphologies were synthesized by varying the reaction time in a polyol refluxing process without the use of any characteristic structure directing agents. The X-ray diffraction studies indicate the highly crystalline nature of the prepared samples. Electron microscopy investigations revealed the morphology of the samples after 1 to 16 h polyol reaction to be secondary nanorod bundles whereas the olivine sample recovered after 32 h polyol reaction displayed nano-plate morphology. The dimensions of the obtained samples varied from a few tens to a few hundred nanometers. When employed in a lithium test cell, the LiFePO{sub 4} cathodes reacted for 1, 4, 8, 16 and 32 h delivered discharge capacities of 161, 162, 171, 143 and 155 mAhg{sup −1}, respectively, with a well-defined plateau at 3.4 V and impressive capacity retentions until 50 cycles. Interestingly, among the prepared electrodes, the LiFePO{sub 4} nanorod bundle cathode prepared under 1 h reaction time maintained the highest average reversible capacities of 123 and 103 mAhg{sup −1} at C-rates as high as 3.2 and 6.4 C. The crystal growth mechanism during the polyol refluxing method can be explained by the stages of precursor dissolution and nucleation, oriented crystal growth and alignment by self-assembly, aggregation and partial dissolution and complete re-crystallization. - Highlights: • Study of LiFePO{sub 4} crystal formation by tuning reaction times in a simple polyol process • Nano-structured LiFePO{sub 4} is formed by varying reaction times in a simple polyol process. • Self-assembled secondary LiFePO{sub 4} nanorod bundles are obtained under 1 h reaction time. • Secondary structures are formed via a template-free self-assembly process. • The olivine nanorod bundle cathode demonstrated enhanced electrochemical properties.

36 MATERIALS SCIENCE↗

Estimatation of talc properties after milling

As we know Talc is a natural mineral which is used in different areas for different purposes. The principle of this paper is analysis of structural properties of the natural talc therefore the different types of structural treatments were used. Talc powder was dry milled by vibration. Then the samples were alkalized by hydrochloric acid. To study its structural property the specific surface area and cumulative pore volume values of the starting material were 10.1 m{sup 2}/g and 0.09 cm{sup 3}/g. It was observed that the acid treatments were main reason to increase of the specific surface area. A small increment in the V{sub cp} was observed for all prepared samples. The treated samples were examined by using X-ray diffraction techniques.

36 MATERIALS SCIENCE↗

Learning-based Computational Study of the Thermodynamic, Structural, and Dynamic Properties of Molten Salt at the Atomic and Electronic Scale and Experimental Validations (Final Report for Project 19-16909)

The project completed several milestones related to the work scope to determine thermophysical properties of the molten salt FLiNaK. A combined approach to integrate advanced computations with neutron scattering experimental interrogation was used to quantify the structure and mass transport of pure FLiNaK and FLiNaK with additives. The additives investigated included Ce, Cs, Zr, and Cr. The primary outcome of the computational work was the development of a neutral network force field interatomic potential (referred to as the NNFF model in this document). The computational work also involved ab initio calculations to determine the ground truth and molecular dynamics simulations to provide computational analogs to the experimental campaign. The experimental work used enriched F 7 LiNaK prepared by Argonne National Laboratory. The use of enriched F 7 LiNaK reduced parasitic neutron absorption and significantly improved data collection and data quality. Several graduate students were supported during the course of the project, which included a one year no-cost extension. These students were trained in advanced computational methods, advanced neutron scattering methods, neutron scattering data analysis and interpretation, and molten salt sample preparation.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Silver-mediated separations: A comprehensive review on advancements of argentation chromatography, facilitated transport membranes, and solid-phase extraction techniques and their applications

The use of silver(I) ions in chemical separations, also known as argentation separations, is a powerful approach for the selective separation and analysis of many natural and synthetic organic compounds. In this review, a comprehensive discussion of the most common argentation separation techniques, including argentation-liquid chromatography (Ag-LC), argentation-gas chromatography (Ag-GC), argentation-facilitated transport membranes (Ag-FTMs), and argentation-solid phase extraction (Ag-SPE) is provided. For each of these techniques, notable advancements, optimized separations, and innovative applications are discussed. The review begins with an explanation of the fundamental chemistry underlying argentation separations, mainly the reversible π-complexation between silver(I) ions and carbon-carbon double bonds. Within Ag-LC, the use of silver(I) ions in thin-layer chromatography, high-performance liquid chromatography, as well as preparative LC are explored. This discussion focuses on how silver(I) ions are employed in the stationary and mobile phase to separate unsaturated compounds. For Ag-GC and Ag-FTMs, different silver compounds and supporting media are discussed, often with relation to olefin-paraffin separations. Ag-SPE has been widely employed for the selective extraction of unsaturated compounds from complex matrices in sample preparation. This comprehensive review of Ag-LC, Ag-GC, Ag-FTMs, and Ag-SPE techniques emphasizes the immense potential of argentation separations in separations science and serves as a valuable resource for researchers seeking to learn, optimize, and utilize argentation separations.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Laser Time-of-Flight Mass Spectrometry for Space

A miniature reflection time-of-flight mass spectrometer for in situ planetary surface analysis is described. The laser ablation mass spectrometer (LAMS) measures the regolith's elemental and isotopic composition without high-voltage source extraction or sample preparation. The compact size (< 2 x 10(exp 3) cubic cm) and low mass (approximately 2 kg) of LAMS, due to its fully coaxial design and two-stage reflectron, fall within the strict resource limitations of landed science missions to solar system bodies. A short-pulse laser focused to a spot with a diameter approximately 30-50 micrometers is used to obtain microscopic surface samples. Assisted by a microimager, LAMS can interactively select and analyze a range of compositional regions (with lateral motion) and with repeated pulses can access unweathered, subsurface materials. The mass resolution is calibrated to distinguish isotopic peaks at unit masses, and detection limits are on resolved to a few ppm. The design and calibration method of a prototype LAMS device is described, which include the development of preliminary relative sensitivity coefficients for major element bulk abundance measurements.

Brinckerhoff, W. B.↗

Novel Biocomposites Based on Sunflower Oil and Alfa Fibers as Renewable Resources

The aim of this work is to develop biocomposites based on modified sunflower oil as resin and short natural fibers from Alfa plants (Stipa tenacissima) as reinforcement. Epoxidized sunflower oil (ESFO) was chemically modified via acrylation reaction to obtain acrylated epoxidized sunflower oil resin (AESFO). The AESFO resin was then copolymerized with styrene as co-monomer in the presence of boron trifluoride (BF{sub 3}) as cationic initiator and cobalt octoate (Co) as catalyst. Experimental conditions of this modification were optimized by varying styrene, Co and BF{sub 3} wt%. The styrene was varied from 30, 40 to 50 wt% while the catalyst (Co) was varied from 0, 0.01, 0.02 to 0.03 wt%. Two different percents of BF{sub 3} were considered: 0.5 and 1 wt%. The prepared samples were evaluated according to their appearance and then characterized in terms of tensile properties (stress at break, Young’s modulus and elongation at break) to determine the best ratio of styrene/BF{sub 3}/Co. Alfa fibers, used as bio-reinforcement, were treated with a 5% NaOH solution and characterized by Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM) and thermo gravimetric analysis (TGA). Biocomposites were prepared by using untreated (UAF) and treated Alfa fibers (TAF) at a ratio of 5 wt% and characterized in terms of tensile properties and morphology by SEM. The best results were obtained with TAF. Then, the ratio of TAF was varied (5, 7.5 and 10 wt%) and the tensile and thermal properties of the biocomposites were characterized. The results showed that the best results were obtained with the ratio of 7.5 wt%.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Simultaneous shunt protection and back contact formation for CdTe solar cells with single wall carbon nanotube layers

Thin film photovoltaic (PV) devices and modules prepared by commercial processes can be severely compromised by through-device low resistance electrical pathways. The defects can be due to thin or missing semiconductor material, metal diffusion along grain boundaries, or areas containing diodes with low turn-on potentials. We report the use of single wall carbon nanotube (SWCNT) layers to enable both protection against these defects and back contact formation for CdTe PV devices. Samples prepared with a SWCNT back contact exhibited good efficiency and did not require shunt protection, while devices prepared without shunt protection using a standard metal back contact performed poorly. We describe the mechanism by which the SWCNT layer functions. In addition to avoiding the need for shunt protection by other means, the SWCNT film also provides a route to higher short circuit currents.

14 SOLAR ENERGY↗

TEM characterization of a simultaneously neutron-irradiated and helium-injected PM2000 ODS alloy

Transmission electron microscopy (TEM) discs of PM2000 were coated on one side with a ~4 µm thick NiAl film and irradiated in HFIR to a neutron displacement damage dose of 21.2 dpa at 500°C. The dpa are primarily produced by fast neutrons, while the in situ He injection (ISHI) to 1230 appm derives from the thermal neutron two-step 59 Ni(n,α) reaction. A uniform He injection profile extends up to about 8 µm below the NiAl coating, hence the remaining material experiences only dpa damage (21.2 dpa at 500°C). This report summarizes analytical TEM analyses to compare the two different regions, i.e., simultaneous He-injection/displacement damage versus displacement damage only, or high and very low He/dpa ratios, respectively. TEM analyses of the He implanted region reveals a high density of small (<2 nm) He bubbles predominantly associated with dislocation loops in the matrix. Because of a very large grain size, no grain or subgrain boundaries were observed in the samples prepared by focused ion beam (FIB) micromachining. The only voids formed were associated with large ODS particles, all of which were amorphous, irrespective of particle size and level of He. The ODS particles range in size from 15-30 nm, and most particles have a single faceted void attached to it that ranges in size from 5 to 15 nm. On the non-implanted side of the sample, no He bubbles could be detected, and faceted voids were found on ~10% of the ODS particles. The He-implanted side contains both <100>{100} and ½<111>{111} dislocation loops and a low density of line dislocations, whereas the un-implanted side possesses predominantly line dislocations with a lower density of dislocation loops. In both regions, nanoscale fcc precipitates exhibiting a cube-on-cube orientation relationship with the bcc matrix were observed. Chemical analysis using energy dispersive x-ray spectroscopy (EDS) indicates this phase is rich in Al and Ti. It was also noted that substantial Cr segregation occurs around the dislocation loops, concurrent with Fe depletion. The clusters of fcc precipitates that do not appear to be associated with the existing loops or line dislocations. The amorphous Y-Al-O particles contain a high Al concentration (>20 at%) and Cr segregation/Fe-depletion at the periphery.

Jung, Hee Joon↗

Electrical conductivity of Ca{sub 1-x}Sr{sub x}Ti{sub 0.65}Fe{sub 0.35}O{sub 3-{delta}}, x = 0, 0.5 and 1, polycrystalline compounds in the 300-500 K range

Highlights: Black-Right-Pointing-Pointer Fe-doped Sr and Ca titanates were synthesized by chemical and solid state reaction. Black-Right-Pointing-Pointer SPM images show striking differences in samples prepared by the two routes. Black-Right-Pointing-Pointer Impedance spectroscopy measurements show different electrical behaviors. Black-Right-Pointing-Pointer Correlations between the two macroscopic observations are shown. -- Abstract: Bulk and grain boundary electrical conductivity of oxygen deficient Ca{sub x}Sr{sub 1-x}Ti{sub 0.65}Fe{sub 0.35}O{sub 3-{delta}}, x = 0, 0.5 and 1.0, polycrystalline specimens were evaluated by impedance spectroscopy measurements in the 5 Hz-13 MHz frequency range from 300 to 500 K. The ceramic powders were synthesized by solid state reaction and by a chemical route, the polymeric precursor technique. The X-ray diffraction of the samples at room temperature shows the following perovskite crystalline structures: cubic for x = 0 and orthorhombic for x = 0.5 and 1.0. The impedance plots are composed of two semicircles ascribed to grains (bulk) and interfaces (grain boundaries) contributions. The impedance data show that sintered pellets using powders prepared by solid state synthesis present higher intergranular and intragranular resistivity values than pellets prepared by the chemical route. Observations of scanning probe microscopy topographic images of the surfaces of the sintered pellets show evident differences between the grain morphology of the pellets prepared with powders synthesized by the two routes.

36 MATERIALS SCIENCE↗

Bio‐based glycerol plasticizers for flexible poly(vinyl chloride) blends

Abstract A series of glycerol‐based compounds were investigated for their application as plasticizers for flexible poly(vinyl chloride) (PVC) blends. The effect of plasticizer chemical structure on the performance, migration behavior, and blend morphology were evaluated and compared to blends produced using the commercial plasticizer dioctyl terephthalate (DOTP). Blends containing 40 phr (parts per hundred rubber) of glycerol‐based plasticizer showed a considerable reduction (between 54 to 86°C) in glass transition temperature ( T g ) relative to neat PVC ( T g ~ 80°C). Tensile testing of samples prepared with the glycerol analogs demonstrated higher ductility (elongation at break values of up to 97%) than DOTP (elongation at break value of 75%) at identical plasticizer loadings. The surface morphologies showed excellent incorporation of the glycerol plasticizers functionalized with alkyl chains longer than four carbons in length into the PVC matrix, whereas droplet formation was observed in blends with shorter chain glycerol derivatives. Leaching behavior of the plasticized samples were evaluated into different media and showed that plasticizers comprised of branched, or longer alkyl chains produced 2‐ to 4‐fold lower migration rates compared to those with shorter alkyl chains into polar solutions.

Halloran, Matthew W.↗

Automated High‐Throughput Fatigue Testing of Freestanding Thin Films

Abstract Mechanical testing at small length scales has traditionally been resource‐intensive due to difficulties with meticulous sample preparation, exacting load alignments, and precision measurements. Microscale fatigue testing can be particularly challenging due to the time‐intensive, tedious repetition of single fatigue experiments. To mitigate these challenges, this work presents a new methodology for the high‐throughput fatigue testing of thin films at the microscale. This methodology features a microelectromechanical systems‐based Si carrier that can support the simultaneous and independent fatigue testing of an array of samples. To demonstrate this new technique, the microscale fatigue behavior of nanocrystalline Al is efficiently characterized via this Si carrier and automated fatigue testing with in situ scanning electron microscopy. This methodology reduces the total testing time by an order of magnitude, and the high‐throughput fatigue results highlight the stochastic nature of the microscale fatigue response. This manuscript also discusses how this initial capability can be adapted to accommodate more samples, different materials, new geometries, and other loading modes.

Barrios, Alejandro↗

X-ray linear dichroic tomography of crystallographic and topological defects

Abstract The functionality of materials is determined by their composition 1–4 and microstructure, that is, the distribution and orientation of crystalline grains, grain boundaries and the defects within them 5,6 . Until now, characterization techniques that map the distribution of grains, their orientation and the presence of defects have been limited to surface investigations, to spatial resolutions of a few hundred nanometres or to systems of thickness around 100 nm, thus requiring destructive sample preparation for measurements and preventing the study of system-representative volumes or the investigation of materials under operational conditions 7–15 . Here we present X-ray linear dichroic orientation tomography (XL-DOT), a quantitative, non-invasive technique that allows for an intragranular and intergranular characterization of extended polycrystalline and non-crystalline 16 materials in three dimensions. We present the detailed characterization of a polycrystalline sample of vanadium pentoxide (V 2 O 5 ), a key catalyst in the production of sulfuric acid 17 . We determine the nanoscale composition, microstructure and crystal orientation throughout the polycrystalline sample with 73 nm spatial resolution. We identify and characterize grains, as well as twist, tilt and twin grain boundaries. We further observe the creation and annihilation of topological defects promoted by the presence of volume crystallographic defects. The non-destructive and spectroscopic nature of our method opens the door to operando combined chemical and microstructural investigations 11,18 of functional materials, including energy, mechanical and quantum materials.

Science & Technology - Other Topics↗