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At least 19 records

Thickness measurements of nanoscale brine films on silica surfaces under geologic CO 2 sequestration conditions using synchrotron X-ray fluorescence

In reservoirs used for geologic CO 2 sequestration, brine films remaining on mineral surfaces can influence flow, diffusion, and reactions. We have examined how the capillary (disjoining) potential influences the thickness of a KCsI 2 brine film on both smooth and rough SiO 2 surfaces [root mean square roughness (Rrms), 1.6 and 330 nm, respectively], under confinement with supercritical (sc) CO2. The thicknesses of brine films coating interior surfaces of SiO 2 windows in a high-pressure cell were determined through synchrotron X-ray fluorescence of two tracer ions (I - and Cs +) at 7.8 MPa and 40°C (representative of conditions at about 0.78 km below the land surface), with scCO 2 as the immiscible confining fluid. The measured area-averaged film thicknesses on the 330 nm Rrms silica surface ranged from 265 to 249 nm for capillary potentials measured within a narrow range from 0.18 to 3.7 kPa. Over this same range of potentials, film thicknesses measured on the smooth (1.6 nm Rrms) silica surface were about 2 nm, although equilibrium does not seem to have been achieved. The measured average brine film thicknesses were critically controlled by surface roughness, with very weak variation in response to the fairly narrow range of tested capillary potentials.

58 GEOSCIENCES↗

Synchrotron X-ray microfluorescence measurement of metal distributions in Phragmites australis root system in the Yangtze River intertidal zone

This study investigates the distributions of Br, Ca, Cl, Cr, Cu, K, Fe, Mn, Pb, Ti, V and Zn in Phragmites australis root system and the function of Fe nanoparticles in scavenging metals in the root epidermis using synchrotron X-ray microfluorescence, synchrotron transmission X-ray microscope measurement and synchrotron X-ray absorption near-edge structure techniques. The purpose of this study is to understand the mobility of metals in wetland plant root systems after their uptake from rhizosphere soils. Phragmites australis samples were collected in the Yangtze River intertidal zone in July 2013. The results indicate that Fe nanoparticles are present in the root epidermis and that other metals correlate significantly with Fe, suggesting that Fe nanoparticles play an important role in metal scavenging in the epidermis.

Feng, Huan↗

National Synchrotron Light Source II storage ring vacuum systems

The National Synchrotron Light Source II, completed in 2014, is a 3-GeV synchrotron radiation (SR) facility at Brookhaven National Laboratory and has been in steady operation since. With a design electron current of 500 mA and subnanometer radians horizontal emittance, this 792-m circumference storage ring is providing the highest flux and brightness x-ray beam for SR users. The majority of the storage ring vacuum chambers are made of extruded aluminium. Chamber sections are interconnected using low-impedance radiofrequency shielded bellows. SR from the bending magnets is intercepted by water-cooled compact photon absorbers resided in the storage ring chambers. This paper presents the design of the storage ring vacuum system, the fabrication of vacuum chambers and other hardware, the installation, the commissioning, and the continuing beam conditioning of the vacuum systems.

43 PARTICLE ACCELERATORS↗

Spherical quartz crystals investigated with synchrotron radiation

The quality of x-ray spectra and images obtained from plasmas with spherically bent crystals depends in part on the crystal's x-ray diffraction across the entire crystal surface. We employ the energy selectivity and high intensity of synchrotron radiation to examine typical spherical crystals from alpha-quartz for their diffraction quality, in a perpendicular geometry that is particularly convenient to examine sagittal focusing. The crystal's local diffraction is not ideal: the most noticeable problems come from isolated regions that so far have failed to correlate with visible imperfections. In conclusion, excluding diffraction from such problem spots has little effect on the focus beyond a decrease in background.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

A modular reactor design for in situ synchrotron x-ray investigation of atomic layer deposition processes

Synchrotron characterization techniques provide some of the most powerful tools for the study of film structure and chemistry. The brilliance and tunability of the Advanced Photon Source allow access to scattering and spectroscopic techniques unavailable with in-house laboratory setups and provide the opportunity to probe various atomic layer deposition (ALD) processes in situ starting at the very first deposition cycle. Here, we present the design and implementation of a portable ALD instrument which possesses a modular reactor scheme that enables simple experimental switchover between various beamlines and characterization techniques. As first examples, we present in situ results for (1) X-ray surface scattering and reflectivity measurements of epitaxial ZnO ALD on sapphire, (2) grazing-incidence small angle scattering of MnO nucleation on silicon, and (3) grazing-incidence X-ray absorption spectroscopy of nucleation-regime Er{sub 2}O{sub 3} ALD on amorphous ALD alumina and single crystalline sapphire.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

High-energy synchrotron study of in-pile-irradiated U–Mo fuels

Here synchrotron scattering analysis results on U–7wt.%Mo fuel specimens irradiated in the Advanced Test Reactor to three burnup levels (3.0, 5.2, and 6.3 × 1021 fission/cm3) are reported. Mature fission gas bubble superlattice was observed to form at intermediate burnup. The superlattice constant was determined to be 11.7 and 12.0 nm by wide-angle and small-angle scattering respectively. Grain sub-division takes place throughout the irradiation and causes the collapse of the superlattice at high burnup. The bubble superlattice expands the U–Mo lattice and acts as strong sink for radiation-induced defects. The evolution of dislocation loops was, therefore, suppressed until the bubble superlattice collapsed.

metallic nuclear fuel↗

Study of liquid gallium at high pressure using synchrotron x-ray

Liquid gallium has been studied at high pressure up to 2 GPa and ambient temperature in a diamond anvil cell using high energy synchrotron x-ray beam. The total x-ray scattering data of liquid gallium were collected up to Q = 12 A{sup -1} and analyzed using pair distribution functions (PDF). The results indicate that the first nearest neighbor peak and second nearest neighbor (shoulder) peak of PDF in liquid gallium does not change with pressure, whereas the higher order (i.e., third and fourth) nearest neighbor peaks shift towards shorter distance with increasing pressure. Reverse Monte Carlo modeling based on the observed data shows that the coordination number in the liquid gallium increases with pressure from 10.5 at 0.3 GPa to 11.6 at 2 GPa. An atomic arrangement similar to the crystalline phase of Ga(II) with coordination number of 12 is proposed for the locally dense-packed rigid unit in liquid gallium. The volume compression data derived from the structure modeling yield a bulk modulus of 12.1(6) GPa for liquid gallium.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Analysis of rapidly synthesized guest-filled porous complexes with synchrotron radiation: practical guidelines for the crystalline sponge method

This report describes complete practical guidelines and insights for the crystalline sponge method, which have been derived through the first use of synchrotron radiation on these systems, and includes a procedure for faster synthesis of the sponges. These guidelines will be applicable to crystal sponge data collected at synchrotrons or in-house facilities, and will allow researchers to obtain reliable high-quality data and construct chemically and physically sensible models for guest structural determination. A detailed set of synthetic and crystallographic guidelines for the crystalline sponge method based upon the analysis of expediently synthesized crystal sponges using third-generation synchrotron radiation are reported. The procedure for the synthesis of the zinc-based metal–organic framework used in initial crystal sponge reports has been modified to yield competent crystals in 3 days instead of 2 weeks. These crystal sponges were tested on some small molecules, with two being unexpectedly difficult cases for analysis with in-house diffractometers in regard to data quality and proper space-group determination. These issues were easily resolved by the use of synchrotron radiation using data-collection times of less than an hour. One of these guests induced a single-crystal-to-single-crystal transformation to create a larger unit cell with over 500 non-H atoms in the asymmetric unit. This led to a non-trivial refinement scenario that afforded the best Flack x absolute stereochemical determination parameter to date for these systems. The structures did not require the use of PLATON/SQUEEZE or other solvent-masking programs, and are the highest-quality crystalline sponge systems reported to date where the results are strongly supported by the data. A set of guidelines for the entire crystallographic process were developed through these studies. In particular, the refinement guidelines include strategies to refine the host framework, locate guests and determine occupancies, discussion of the proper use of geometric and anisotropic displacement parameter restraints and constraints, and whether to perform solvent squeezing/masking. The single-crystal-to-single-crystal transformation process for the crystal sponges is also discussed. The presented general guidelines will be invaluable for researchers interested in using the crystalline sponge method at in-house diffraction or synchrotron facilities, will facilitate the collection and analysis of reliable high-quality data, and will allow construction of chemically and physically sensible models for guest structural determination.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

In-situ synchrotron energy-dispersive x-ray diffraction study of thin Pd foils with Pd:D and Pd:H concentrations up to 1:1

Time resolved, in-situ, energy dispersive x-ray diffraction was performed in an electrolysis cell during electrochemical loading of palladium foil cathodes with hydrogen and deuterium. Concentrations of H:Pd (D:Pd) up to 1:1 in 0.1 M LiOH (LiOD) in H{sub 2}O (D{sub 2}O) electrolyte were obtained, as determined by both the Pd lattice parameter and cathode resistivity. In addition, some indications on the kinetics of loading and deloading of hydrogen from the Pd surface were obtained. The alpha-beta phase transformations were clearly delineated but no new phases at high concentration were determined.

36 MATERIALS SCIENCE↗