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At least 109 records · Page 6

Synthesis of MSnO{sub 3} (M = Ba, Sr) nanoparticles by reverse micelle method and particle size distribution analysis by whole powder pattern modeling

Highlights: ► BaSnO{sub 3} and SrSnO{sub 3} nanoparticles synthesized using the reverse micelle method. ► Particle size and size distribution studied by whole powder pattern modeling. ► Nanoparticles are of optimal size for investigation in dye-sensitized solar cells. -- Abstract: Light-to-electricity conversion efficiency in dye-sensitized solar cells critically depends not only on the dye molecule, semiconducting material and redox shuttle selection but also on the particle size and particle size distribution of the semiconducting photoanode. In this study, nanocrystalline BaSnO{sub 3} and SrSnO{sub 3} particles have been synthesized using the microemulsion method. Particle size distribution was studied by whole powder pattern modeling which confirmed narrow particle size distribution with an average size of 18.4 ± 8.3 nm for SrSnO{sub 3} and 15.8 ± 4.2 nm for BaSnO{sub 3}. These values are in close agreement with results of transmission electron microscopy. The prepared materials have optimal microstructure for successive investigation in dye-sensitized solar cells.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Synthesis of visible light driven cobalt tailored Ag{sub 2}O/TiON nanophotocatalyst by reverse micelle processing for degradation of Eriochrome Black T

Graphical abstract: Cobalt tailored Ag{sub 2}O/TiON nanophotocatalyst is synthesized using reverse micelle technique and it showed extraordinary photocatalytic activity. Display Omitted Highlights: ► TiON/Ag{sub 2}O/Co nanophotocatalyst is synthesized using microemulsion technique. ► Low temperature anatase phase and outstanding photocatlytic activity is observed. ► Effect of temperature and inert atmosphere on materials phase is investigated. ► Homogeneous dopants distribution and oxygen vacancies are examined. ► Enhancement in surface area, quantum efficiency and optical properties is observed. -- Abstract: An ultra efficient cobalt tailored silver and nitrogen co-doped titania (TiON/Ag{sub 2}O/Co) visible nanophotocatalyst is successfully synthesized using modified reverse micelle processing. Composition, phase, distribution of dopants, functional group analysis, optical properties and morphology of synthesized materials are investigated by means of X-ray diffraction (XRD), transmission electron microscopy (TEM) based techniques and others. Charge states of titanium (Ti) and silver are explored through core-loss electron energy loss spectroscopy (EELS) analysis and X ray photoelectron spectroscopy (XPS). Our characterization results showed that the synthesized nanophotocatalyst consisted of anatase phased qausispherical nanoparticles that exhibited homogeneous distribution of dopants, large surface area, high quantum efficiency and enhanced optical properties. At lower content of doped Co ions, the TiON/Ag{sub 2}O responded with extraordinary photocatalytic properties. The cobalt tailored nanophotocatalyst showed remarkable activity against Eriochrome Black T (EBT). Moreover, comparative degradation behavior of EBT with TiON, Ag{sub 2}O/TiON and Co/Ag{sub 2}O/TiON is also investigated.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Preparation, characterization, and photocatalytic studies on anatase nano-TiO{sub 2} at internal air lift circulating photocatalytic reactor

Graphical abstract: The micro morphological structure of the nano-TiO{sub 2} particles was also observed with TEM, as shown in figure. The TEM images clearly exhibited the homogeneous microstructure of particles with a size of around 10–15 nm. - Highlights: • Nano-TiO{sub 2} was prepared by complex techniques of sol–gel, micro-emulsion and solvent thermal. • The size of TiO{sub 2} was nano level and uniformity. • Nano-TiO{sub 2} exhibited high photo-catalytic activity at internal air lift circulating reactor. • The best nano-TiO{sub 2} dosage was obtained. - Abstract: Anatase nano-titania (TiO{sub 2}) powder was prepared by using a sol–gel process mediated in reverse microemulsion combined with a solvent thermal technique. The structures of the obtained TiO{sub 2} were characterized by TG-DSC, XRD, TEM. The photocatalytic decomposition of methylene blue (MB) on nano-TiO{sub 2} was studied by using an internal air lift circulating photocatalytic reactor. The results show that the anatase structure appears in the calcination temperature range of 400–510 °C, while the transformation of anatase into rutile takes place above 510 °C. The homogeneous microstructure of nano-TiO{sub 2} particles was obtained with a size of around 10–15 nm. In the photocatalytic performance, degradation process follows pseudo first order kinetics with different dosages of photocatalyst and initial MB concentrations and optimal TiO{sub 2} dosage is 0.1 g/L with neutral medium.

36 MATERIALS SCIENCE↗

Optimum lithium loading of a liquid scintillator for neutron and neutrino detection

Neutral particle detection in high-background environments is greatly aided by the ability to easily load 6 Li into liquid scintillators. In this work, we describe a readily available and inexpensive liquid scintillation cocktail stably loaded with a Li mass fraction up to 1%. Compositions that give thermodynamically stable microemulsions (reverse-micellar systems) were explored, using a Compton spectrum quenching technique to distinguish these from unstable emulsions. Scintillation light yield and transmittance were characterized. Pulse shape discrimination (PSD) was measured using a 252 Cf source, showing that electron-like and proton-like recoil events are well-resolved even for Li loading up to 1%, providing a means of background suppression in neutron/neutrino detectors. While samples in this work were prepared with nat Li (7.59% 6 Li), the neutron capture peak was clearly visible in the PSD spectrum; this implies that while extremely high capture efficiency could be achieved with 6 Li-enriched material, a very inexpensive neutron-sensitive detector can be prepared with nat Li.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Influence of calcium nitrate timing on the structural and textural characteristics of mesoporous SiO 2 -CaO nanoparticles

Mesoporous bioactive glass nanoparticles (MBGNPs) are promising materials for drug delivery due to their high pore volume and specific surface area. This study investigates how the timing of calcium nitrate addition affects the structural and textural characteristics of MBGNPs synthesized via a microemulsion-assisted sol-gel method. Delayed calcium nitrate addition reduced calcium incorporation from 14.2 to 9.5 mol% and increased particle size from 178 ± 51 nm to 256 ± 30 nm. The specific surface area values increased with the delayed addition of calcium nitrate, as observed through BET and USAXS/SAXS measurements. The proportion of Q Si n units slightly changed, but no cytotoxicity was observed in osteoblast-like cells. These findings provide valuable insights into optimizing MBGNP synthesis for biomedical applications.

Calcium nitrate tetrahydrate↗

Probing the Chemical Stability of Mixed Ferrites: Implications for Magnetic Resonance Contrast Agent Design

Nanomaterials with mixed composition, in particular magnetic spinel ferrites, are emerging as efficient contrast agents for magnetic resonance imaging. Many factors, including size, composition, atomic structure, and surface properties, are crucial in the design of such nanoparticle-based probes because of their influence on the magnetic properties. Silica-coated iron oxide (IO-SiO{sub 2}) and cobalt ferrite (CoIO-SiO{sub 2}) nanoparticles were synthesized using standard high-temperature thermal decomposition and base-catalyzed water-in-oil microemulsion techniques. Under neutral aqueous conditions, it was found that 50-75% of the cobalt content in the CoIO-SiO{sub 2} nanoparticles leached out of the core structure. Leaching caused a 7.2-fold increase in the longitudinal relaxivity and an increase in the saturation magnetization from {approx}48 to {approx}65 emu/g of the core. X-ray absorption fine structure studies confirmed that the atomic structure of the ferrite core was altered following leaching, while transmission electron microscopy and dynamic light scattering confirmed that the morphology and size of the nanoparticle remained unchanged. The CoIO-SiO{sub 2} nanoparticles converted from a partially inverted spinel cation arrangement (unleached state) to an inverse spinel arrangement (leached state). The control IO-SiO{sub 2} nanoparticles remained stable with no change in the structure and negligible changes in the magnetic behavior. This detailed analysis highlights how important understanding the properties of nanomaterials is in the development of reliable agents for diagnostic and therapeutic applications.

36 MATERIALS SCIENCE↗

Non-destructive thermal wave method applied to study thermal properties of fast setting time endodontic cement

The thermal wave method is applied for thermal properties measurement in fast endodontic cement (CER). This new formula is developed upon using Portland cement in gel and it was successfully tested in mice with good biocompatibility and stimulated mineralization. Recently, thermal expansion and setting time were measured, conferring to this material twice faster hardening than the well known Angelus Mineral trioxide aggregate (MTA) the feature of fast hardening (∼7 min) and with similar thermal expansion (∼12 μstrain/ °C). Therefore, it is important the knowledge of thermal properties like thermal diffusivity, conductivity, effusivity in order to match thermally the tissue environment upon its application in filling cavities of teeth. Photothermal radiometry technique based on Xe illumination was applied in CER disks 600 μm thick for heating, with prepared in four particle sizes (25, 38, 45, and 53) μm, which were added microemulsion gel with variation volumes (140, 150, 160, and 170) μl. The behavior of the thermal diffusivity CER disks shows linear decay for increase emulsion volume, and in contrast, thermal diffusivity increases with particles sizes. Aiming to compare to MTA, thermal properties of CER were averaged to get the figure of merit for thermal diffusivity as (44.2 ± 3.6) × 10{sup −3} cm{sup 2}/s, for thermal conductivity (228 ± 32) mW/cm K, the thermal effusivity (1.09 ± 0.06) W s{sup 0.5}/cm{sup 2} K and volume heat capacity (5.2 ± 0.7) J/cm{sup 3} K, which are in excellent agreement with results of a disk prepared from commercial MTA-Angelus (grain size < 10 μm using 57 μl of distilled water)

36 MATERIALS SCIENCE↗

Preparation and characterization of polyethylene glycol diacrylate microgels using electron beam radiation

The use of microemulsion in the development of nanosized gels based on polyethylene glycol diacrylate (PEGDA) is demonstrated. PEGDA was solubilized in n-heptane with use of sodium docusate (AOT) at 0.15M concentration to form reverse micelles. These micelles were than irradiated at 5, 10, 15, 20 and 25 kGy using electron beam (EB) to crosslink the entrapped polymer in the micelles. Ionizing radiation was imparted to the emulsions to generate crosslinking reaction in the micelles formed. The nanosized gels were evaluated in terms of particle diameter using dynamic light scattering (DLS) and the images of the nanosized gels were studied using transmission electron microscopy (TEM). Results show that the size and shape of the particles are influenced by concentration of PEGDA and radiation dose. This study showed that this method can be utilized to produce nanosized gels.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Controlling morphology, mesoporosity, crystallinity, and photocatalytic activity of ordered mesoporous TiO{sub 2} films prepared at low temperature

Partly ordered mesoporous titania films with anatase crystallites incorporated into the pore walls were prepared at low temperature by spin-coating a microemulsion-based reaction solution. The effect of relative humidity employed during aging of the prepared films was studied using SEM, TEM, and grazing incidence small angle X-ray scattering to evaluate the mesoscopic order, porosity, and crystallinity of the films. The study shows unambiguously that crystal growth occurs mainly during storage of the films and proceeds at room temperature largely depending on relative humidity. Porosity, pore size, mesoscopic order, crystallinity, and photocatalytic activity of the films increased with relative humidity up to an optimum around 75%.

36 MATERIALS SCIENCE↗

Nanoparticles of spinel and perovskite ferromagnets and prospects for their application in medicine

In this work, nanoparticles of La{sub 0.75}Sr{sub 0.25}MnO{sub 3} compounds with perovskite structure and AFe{sub 2}O{sub 4} (A = Mn, Fe, Co, Ni, Zn) with spinel structure have been synthesized by precipitation from diethylene glycol and microemulsion using Triton X-100 surfactant. Comparative X-ray diffraction and magnetic studies of the synthesized nanoparticles have been carried out. Magnetic fluids prepared from synthesized nanopowders have been characterized by calorimetric measurements of specific loss power (SLP)

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Enhanced luminescence in Eu-doped ZnO nanocrystalline films

We found an enhancement of Eu{sup 3+} emissions in Eu-doped ZnO nanocrystalline films fabricated by microemulsion method. The Eu{sup 3+} emission intensities were increased by reducing annealing temperatures from 633 K to 533 K. One possible explanation for this phenomenon is that the size reduction enhances the energy transfer from ZnO nanoparticles to Eu{sup 3+} ions. Also, the shift of the charge-transfer band into the low-energy side of the absorption edge is found to be crucial, which seems to expedite the energy transfer from O atoms to Eu{sup 3+} ions. These findings will be useful for the material design of Eu-doped ZnO phosphors.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Electrochemical characterization of aminated acrylic conducting polymer

New attempt has been made to synthesize aminated acrylic conducting polymer (AACP) using precursor of phenylvinylsulfoxide (PVS). The process was conducted via the integration of microemulsion and photopolymerization techniques. It has been utilized for covalent immobilization of amino groups by the adding of N-achryiloxisuccinimide (NAS). Thermal eliminating of benzene sulfenic acids from PVS has been done at 250 °C to form electroactive polyacetylene (PA) segment. Characterization of AACP has been conducted using fourier transform infrared (FTIR), scanning electron microscopy (SEM) and linear sweep cyclic voltammetry (CV). A range of 0.3-1.25μm particle size obtained from SEM characterization. A quasi-reversible system performed as shown in electrochemical study.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Neutron and X-Ray Scattering Studies of New Green Cement, and Nanoconfined Water

This is the Final report on DE-FG02-90ER45429 for the time period from September 1, 1990 to May 31, 2017. The Principal Investigator is Sow-Hsin Chen, Department of Nuclear Science and Engineering, Massachusetts Institute of Technology (MIT), Cambridge, MA 02139 (email: sowhsin@mit.edu). The Administrative Point of Contact at MIT is Sarah Svenson, Senior Contract Administrator, Office of Sponsored Programs, Tel: 617-253-2495, ssvenson@mit.edu. The DOE Program is the Office of Basic Energy Sciences (BES); Program manager is Dr. P. Thiyagarajan, Neutron Scattering SC-22.2/, Germantown Bldg., Germantown, MD 20874 . During these 27 years, the scientific activities has had a number developing emphases, as reflected from the change of Project Title in 1990 as “Construction of a Small Angle Neutron Scattering Spectrometer for Investigation of Microemulsions and Micellar Solutions in Bulk, in Porous Materials...” to “Neutron and X-Ray Scattering Studies of New Green Cement, and Nanoconfined Water” in the last renewal period, 2015-2017, with many title changes in between. Progress Report for each sub-project period was reported to DOE with detailed activity and budgetary reports. It is fair to summary that the chief activity has been in the use neutron, x-ray and laser spectroscopy to investigate materials properties of complex fluids and soft condensed matter. It started with conducting neutron and X-ray scattering experiments to study the structure and dynamics of glass-forming liquids in general first, then more specifically in the case of supercooled water in confined geometry, and culminating in the final study of new green cement. Experiments were conducted at various DOE supported national neutron facilities including ORNL, ANL, BNL and Los Alamos, as well as at NIST/NCNR. Whenever possible, experiments were also performed at numerous world-class facilities, such as those at Saclay and the Institut Laue Langevin (ILL) in Grenoble, France, and at National Synchrotron Radiation Research Center (NSRRC) in recent years in Taiwan, etc. Leveraging on the large number of international collaborate activities, a substantial percentage of activities were supported with collaborators’ own funding sources. These have help to carry out DOE’s mission and produce impressive research products far beyond what was possible with only DOE funding supports. The chief product during this period, 1990-2017, includes (1) Three hundred and eight scientific articles published in peer-reviewed and high-impacted scientific journals during 1990-2017, and a dozen monographs including four books for scientists and graduate students, (2) Twenty-four scientific conferences organized and 209 papers presented at many national and international conferences, (3) educate and train 9 post-doctoral fellows and 28 students including 22 Ph.D. students, 3 M.S. students, and 3 in other categories by providing a research experience in neutron and X-Ray scattering techniques, most of them were supported wholly or in part in the scientific topic of this award during the funding period and (4) numerous high-visibility awards and honors. This final report summarizes and details these research activities and products. At the close of this funding period, the fund from DOE has been totally spent.

07 ISOTOPE AND RADIATION SOURCES↗

Unusual Physical and Chemical Properties of Ni in Ce1-xNixO2-y Oxides: Structural Characterization and Catalytic Activity for the Water Gas Shift Reaction

The structural and electronic properties of Ce{sub 1-x}Ni{sub x}O{sub 2-y} nanosystems prepared by a reverse microemulsion method were characterized with synchrotron-based X-ray diffraction, X-ray absorption spectroscopy, Raman spectroscopy, and density functional calculations. The Ce{sub 1-x}Ni{sub x}O{sub 2-y} systems adopt a lattice with a fluorite-type structure with an acute local order where Ni displays a strongly distorted (oxygen) nearest-neighbor coordination and the presence of Ni atoms as first cation distances, pointing to the existence of Ni-O-Ni entities embedded into the ceria lattice. A Ni {leftrightarrow} Ce exchange within the CeO{sub 2} leads to a charge redistribution and the appearance of O vacancies. The Ni?O bonds in Ce{sub 1-x}Ni{sub x}O{sub 2-y} are more difficult to reduce than the bonds in pure NiO. The specific structural configuration of Ni inside the mixed-metal oxide leads to a unique catalyst with a high activity for the water gas shift (CO + H{sub 2}O {yields} H{sub 2} + CO{sub 2}) reaction and a simultaneous reduction of the methanation activity of nickel. Characterization results indicate that small particles of metallic Ni at the interface position of a ceria network may be the key for high WGS activity and that the formate?carbonate route is operative for the production of hydrogen.

08 HYDROGEN↗

Laser‐Induced Nanodroplet Injection and Reconfigurable Double Emulsions with Designed Inner Structures

Abstract Microfabrication of complex double emulsion droplets with controlled substructures, which resemble biological cells, is an important but a highly challenging subject. Here, a new approach is proposed based on laser‐induced injection of water nanodroplets into a liquid crystal (LC) drop. In contrast to the conventional top‐down microfluidic fabrication, this method employs a series of bottom‐up strategies such as nanodroplet injection, spontaneous and assisted coalescence, elastically driven actuation, and self‐assembly. Each step is controlled precisely by adjusting the laser beam, interfacial tension, and its gradients, surface anchoring, and elasticity of the LC. Whispering gallery mode illumination is used to monitor the injection of droplets. A broad spectrum of double emulsions with a predesigned hierarchical architecture is fabricated and reconfigured by temperature, laser‐induced coalescence, and injection. The proposed bottom‐up method to produce customized microemulsions that are responsive to environmental cues can be used in the development of drug delivery systems, biosensors, and functional soft matter microstructures.

42 ENGINEERING↗

High‐Performance Rechargeable Lithium‐Chlorine Batteries with ALD Conformal Starburst Porous Graphene Positive Electrodes

Abstract Rechargeable alkali metal‐chlorine batteries are emerging as a promising high‐energy‐density solution. However, they confront significant challenges, including the primary issue stemming from the weak binding affinity of cathode materials for Cl 2 , which leads to a sluggish and inadequate supply of Cl 2 during the redox reactions, resulting in a shortened cycle life and low Coulombic efficiency (CE), particularly when operating at ultrahigh specific capacity outputs. Herein, an Al 2 O 3 ‐skinned heterostructured starburst porous graphene with conformal metasurfaces (Al 2 O 3 @rGO) is reported, crafted from a hierarchical porous starburst graphene arranged in a unique layered structure by the PTFE microemulsion skin effect, leveraging subsequent fluidized bed atomic layer deposition (FBALD) of Al 2 O 3 groups. Al 2 O 3 @rGO features superhydrophilicity, effective adsorption, fast kinetics from stable dynamic respiratory interface, high electrical and thermal conductivity anisotropy, intelligent thermal management and safe operation over a wide temperature range. Consequently, the Li‐Cl 2 @Al 2 O 3 @rGO battery achieves an ultrahigh discharge specific capacity of 5000 mAh g −1 at ≈100% CE, and even delivers stable cycling over 200 cycles with 2000 mAh g −1 at an average CE of 99.8% under low temperature environment of ‐40 °C. The scalable heterostructure approach offers a sustainable perspective of the development of functionalized metamaterials and metasurfaces for next‐generation safe and energy‐dense batteries and broader applications.

Chemistry↗

Thin film confinement reduces compatibility in symmetric ternary block copolymer/homopolymer blends

Here, the thin film phase behavior of ternary blends consisting of symmetric poly(styrene) (PS)– b –poly(dimethylsiloxane)(PDMS), PS, and PDMS was investigated using X–ray reflectivity (XRR) and atomic force microscopy (AFM). This system is strongly segregated, and the homopolymers are approximately the same length as the corresponding blocks of the copolymer. The XRR and AFM data are used to quantify changes in domain spacing ( L ) and morphology evolution with increasing homopolymer content (Φ H ). In 100 nm thick films, from Φ H = 0 to 0.20, the system maintains a perfect parallel lamellar structure and domains swell as predicted based on theory; however, from Φ H = 0.30 to 0.50, a morphology transition to a “dot pattern” morphology (tentatively identified as perforated lamellae) and mixed morphologies were observed before macrophase separation. In thicker films, dot patterns were observed for a broad range of Φ H before macrophase separation. The absence of the bicontinuous microemulsion phase reported for bulk blends and thin films of perpendicular lamellae and the presence of dot patterns/perforated lamellae are attributed to preferential migration of the PDMS homopolymer to the wetting layers located at the substrate and free air interfaces, which leads to an asymmetric composition within the film and morphology transition.

36 MATERIALS SCIENCE↗