Temperature-sensitive ferrogel prepared using Fe3O4 nanoparticles are characterized under varying temperature conditions. The nanoparticles were distributed in Nisopropylacrylamide (NIPAm) during their polymerization to form hydrogel. Particle distribution and agglomeration characteristics of the prepared ferrogels were investigated using ultra small angle x-ray scattering (USAXS) at various temperatures through the Lower Critical Solution Temperature (LCST). Transmission electron microscopy (TEM) was used to estimate the particle size distribution. The magnetic property was investigated using direct current superconducting quantum interference device (DC-SQUID) under hydrated conditions. The USAXS analysis showed an increase in the volume of particles without changing the agglomeration characteristics as the temperature is increased during the measurements. The ferrogel did not show any sedimentation or particle detachment from the gel under thermal cycling. Details of our results and analysis are presented.

We compare the characteristics of ferrogels prepared with and without the presence of a uniform magnetic field using Fe3O4 and Fe2O3 nanoparticles immobilized in hydrogels of N-isopropylacrylamide. The spatial distribution and agglomeration of the nanoparticles within the ferrogels were investigated using ultra small angle x-ray scattering (USAXS) and transmission electron microscopy (TEM). Hydrated ferrogels were also studied for magnetization using direct current superconducting quantum interference device (DC-SQUID). Volume size distribution resulting from USAXS data of the Fe3O4-ferrogel prepared under a uniform 225 G magnetic field showed a single broad peak appreciably different from that prepared without magnetic field with three distinct peaks. Volume size distributions resulting from USAXS data of the Fe2O3-ferrogel prepared with and without the presence of a uniform magnetic field both similarly show two peaks. Nanoparticle agglomeration was also determined by analyzing TEM images of ferrogel samples. DC-SQUID measurements of Fe3O4-ferrogel prepared in the presence of a uniform magnetic field showed 9% higher magnetization compared to the Fe3O4-ferrogel prepared without magnetic field. Similarly, DC-SQUID measurements of Fe2O3-ferrogel prepared in the presence of a uniform magnetic field showed 3% higher magnetization compared to the Fe2O3-ferrogel prepared without magnetic field. Thus, the presence of a uniform magnetic field during ferrogel polymerization can enabled the enhancement of the magnetoelastic property of the ferrogel.

Glassy carbon plates were thermochemically gas phase oxidized to obtain monolithic sandwichlike electrode assemblies with high surface area porous films for electrochemical energy storage applications. Film thicknesses were varied by variation of oxidation parameters time, temperature, and oxygen concentration and measured with electron microscopy. The mass density of the porous carbon film material was estimated by fitting a geometrical model to experimental gravimetric data. Optical Raman spectroscopy line scans suggest that the porosity has a gradient between the surface and the film/bulk interface, which is supported by pore-size distribution data obtained from small-angle x-ray scattering (SAXS) on slightly oxidized and fully oxidized samples. Detailed inspection of the power law behavior of SAXS data suggests that the internal surface area of well-oxidized glassy carbon (GC) is compact and extends over the entire probed volume and thus has optimal pore connectivity. This effect goes along with pore enlargement and a relative decrease of internal surface area per volume. Slightly oxidized carbon has no pore space with a compact, high connectivity internal surface area. The corresponding SAXS power law and the x-ray density suggest that this high volumetric surface area must be interpreted as a result of surface roughness, rather than true geometric or volumetric surface area. In consequence, is this surface area of limited use for electrochemical energy storage?

Waspaloy specimens aged at 800°C from 0.5h to 88.5h were evaluated via small angle neutron scattering (SANS), ultra small angle X-ray scattering (USAXS), electrical resistivity, and SEM. The average γ' precipitate size and volume fraction, obtained from modeling the small angle scattering data, was used to calculate a figure of merit of electron scattering. This figure of merit is designed to correlate the electron scattering ability of the material to the precipitate microstructure. The USAXS data shows a secondary precipitate population at smaller diameters that is absent from the SANS data, since the SANS measurements were not obtained at high enough values of Q. It is believed that this secondary population makes the USAXS-derived figure of merit more sensitive to the actual measured resistivity response than the SANS-derived values; however, the SANS derived primary precipitate sizes are believed to more accurate due to a larger sample volume.

This paper presents the results of our analysis of ferrogels prepared using uncoated and polyvinylpyrrolidone (PVP)-coated magnetite (Fe3O4) nanoparticles. The N-isopropylacrylamide (NIPAM) based hydrogel is used with 15-25 nm Fe3O4 nanoparticles different concentrations in the range 1.25 -14%. These samples were analyzed using ultra small angle x-ray scattering (USAXS), Transmission Electron Microscopy (TEM), and Direct-Current Superconducting Quantum Interference Devices (DC-SQUID) magnetometry. Samples prepared with polyvinylpyrrolidone (PVP) coated nanoparticles showed a better single particle distribution compared to uncoated samples. USAXS data indicated that the gels prepared using uncoated nanoparticles have a large two particle agglomerations. In both cases, the volume fraction of the particles in the gel is linearly proportional to the initial particle concentrations. The DC-SQUID magnetometry analysis indicated that the magnetic moment of the gel samples prepared with uncoated particles is ∼ 2emu/g compared to ∼1.5emu/g of those having coated particles.

This work investigates an alternative way to modify the pore size of a 100 mg/cc resorcinol formaldehyde (R/F) aerogel without any significant change to the aerogel target density. This was successfully accomplished by an addition of hydrophilic polymer additive [Poly Vinyl Alcohol (PVA) or Poly Acrylic Acid (PAA)] to the R/F precursor solution which acts as an impurity in the reaction. The polymer can modify the cross linking or aggregation of the primary particles which can change the structure formation of the aerogel, thus changing the pore size. This paper will discuss this process modification and the fabrication of hollow, large pore R/F aerogel spheres that are used for direct drive inertial confinement fusion (ICF) cryogenic ice layering experiments at the University of Rochester Laboratory for Laser Energetics (LLE). The aerogels were characterized using scanning electron microscopy (SEM), nitrogen gas adsorption, and ultra small angle x-ray scattering (USAXS).

An overview is given of the development of advanced nanoporous carbons as storage ma-terials for natural gas (methane) and molecular hydrogen in on-board fuel tanks for next-generation clean automobiles. The carbons are produced in a multi-step process from corncob, have surface areas of up to 3500 m2/g, porosities of up to 0.8, and reversibly store, by physisorp-tion, record amounts of methane and hydrogen. Current best gravimetric and volumetric storage capacities are: 250 g CH4/kg carbon and 130 g CH4/liter carbon (199 V/V) at 35 bar and 293 K; and 80 g H2/kg carbon and 47 g H2/liter carbon at 47 bar and 77 K. This is the first time the DOE methane storage target of 180 V/V at 35 bar and ambient temperature has been reached and exceeded. The hydrogen values compare favorably with the 2010 DOE gravimetric and volu-metric targets for hydrogen. A prototype adsorbed natural gas (ANG) tank, loaded with carbon monoliths produced accordingly and currently undergoing a road test in Kansas City, is de-scribed. A preliminary analysis of the surface and pore structure is given that may shed light on the mechanisms leading to the extraordinary storage capacities of these materials. The analysis includes pore-size distributions from nitrogen adsorption isotherms; spatial organization of pores across the entire solid from small-angle x-ray scattering (SAXS); pore entrances from scanning electron microscopy (SEM) and transmission electron microscopy (TEM); H2 binding energies from temperature-programmed desorption (TPD); and analysis of surface defects from Raman spectra. For future materials, expected to have higher H2 binding energies via appropriate sur-face functionalization, preliminary projections of H2 storage capacities based on molecular dy-namics simulations of adsorption of H2 on graphite, are reported.

The microstructures of thick plasma-sprayed yttria-stabilized zirconia (8% mass fraction yttria) deposits were studied in a series of Porod small-angle neutron scattering (SANS) and multiple small-angle neutron scattering (MSANS) experiments. Three main void components were identified in the deposits: intrasplat cracks, interlamellar planar pores, and globular pores. The SANS and MSANS measurements were analyzed using the traditional theory for Porod scattering and a recently developed three-component model for MSANS evaluation. The average size, volume fraction, internal surface area, and orientation distribution for each void component within the deposits were determined. This study focused on gaining a better understanding of the effects of initial feedstock particle size and annealing temperatures on the microstructure of deposits sprayed under equivalent particle-impact conditions. Quantitative results are presented for each of four deposit samples: one prepared using the as-received feedstock particle wide-size distribution and three prepared from feedstock powder of different and relatively narrow particle size ranges with average sizes of 32, 47, and 88 μm. Except for the coarse (88 μm) feedstock powder, only mild monotonic variations were found in the microstructural anisotropies, the porosities (13 ± 1%), and the internal surface areas in the as-sprayed deposits. The internal surface area was independent of the feedstock particle size, even with the coarse feedstock. When the deposits were annealed at high temperatures (1100 and 1400 °C), the microstructures were altered with a reduction of the total internal surface area and a mild coarsening of the voids. These changes in the microstructural evolution were well-captured and described by the three-component model. The results were compared and related with those obtained from scanning electron microscopy images and elastic moduli measurements.

An enhanced multiple small-angle neutron scattering (MSANS) formulation has been developed to interpret the beam-broadening, arising from coarse, concentrated pore/grain microstructures in porous ceramics and similar materials. Prolific scattering from such systems precludes single-scattering studies (apart from Porod surface determinations). Previous MSANS techniques, which have been developed to extract the mean pore dimensions, either treat a range of scattering morphologies, while assuming that the scattering is in the diffraction limit, or they consider refraction effects, while assuming that the scattering features are spherical. Many systems of interest violate both these assumptions. In the enhanced formulation, the previous method, which allowed fully for refraction, is extended to non-spherical scattering morphologies. Applications of the MSANS formulation to sintering studies of Si3N4 and silica gels, and to the microstructural characterization of plasma-spray coatings are currently of interest.