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At least 91 records · Page 5

Advanced grazing-emission X-ray fluorescence spectroscopy with small-angle neutron scattering for in-vivo surface composition and defect/morphology surface evolution in tokamak PMI

The dynamic and extreme conditions of thermonuclear fusion tokamak plasmas render material surfaces almost impossible to examine in real-time, surface-sensitive conditions. However, combining particle-probe techniques that are not charge-state dependent open the possibilities of in-vivo diagnosis of the plasma-material interface. The reconstituted surfaces of plasma-facing components ranging from first-wall to divertor-component regions in the device vary depending on the complex plasma transport characteristics of the device. For example, in ITER it is predicted that fluxes of the order 10 22 to 10 24 and incident charged-particle energies of 100’s to 1000’s of eV will reach the surface while in the divertor regions within the private-flux and near the inner and outer-strike points would vary from a few eV to 100’s of eV governed by the complex Chodura magnetic sheath dynamics. This means that the penetration range of most charged-particle fluxes would range between 1-100’s of nm (e.g. for fuel particles of D and T and He).

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Tools for Visualization and Analysis of Small-Angle Neutron Scattering Data: Descriptions and Examples

A great deal of progress has been made in improving the data reduction experience for the SANS instruments at the SNS and HFIR at ORNL. The existing data reduction toolset, drtsans, makes it possible to integrate data analysis and visualization tools into the data reduction scripts, thereby providing new opportunities for more automated data processing for users of the SNS and HFIR. Here, the first set of tools developed is described with usage examples.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

More Tools for Visualization and Analysis of Small-Angle Neutron Scattering Data: Descriptions and Examples

With the adoption of drtsans as the data reduction software for the GP-SANS, Bio-SANS and EQ-SANS instruments at ORNL, tools for data visualization and analysis that can be integrated into drtsans scripts are needed to further improve the user experience. New tools that do not need to be incorporated directly into data reduction scripts can also positively impact users during their experiments. In this report, a new set of tools is presented that complements the previous set released. The set includes tools for both fitting data and for visualizing data.

42 ENGINEERING↗

Another Set of Python Tools for Visualizing and Manipulating Small-Angle Neutron Scattering Data: Descriptions and Examples

The GP-SANS, Bio-SANS and EQ-SANS instruments at ORNL utilize drtsans for data reduction. drtsans is built on Python, and it can be run using python scripts and Jupyter notebooks. The flexibility afforded by Python makes it possible to incorporate additional actions into the scripts used for data reduction, such as analysis and visualization. Here, a new set of tools for visualizing and manipulating SANS data that can be incorporated into the data reduction scripts for the ORNL SANS instruments, or employed during post–processing, is presented that expands the capabilities of the two previously-released tool sets.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

Soft Matter Sample Environments for Time-Resolved Small Angle Neutron Scattering Experiments: A Review

With the promise of new, more powerful neutron sources in the future, the possibilities for time-resolved neutron scattering experiments will improve and are bound to gain in interest. While there is already a large body of work on the accurate control of temperature, pressure, and magnetic fields for static experiments, this field is less well developed for time-resolved experiments on soft condensed matter and biomaterials. We present here an overview of different sample environments and technique combinations that have been developed so far and which might inspire further developments so that one can take full advantage of both the existing facilities as well as the possibilities that future high intensity neutron sources will offer.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

Field angle dependent vortex lattice phase diagram in MgB 2

Using small-angle neutron scattering we have studied the superconducting vortex lattice (VL) phase diagram in MgB 2 as the applied magnetic field is rotated away from the c axis and towards the basal plane. The field rotation gradually suppresses the intermediate VL phase which exists between end states aligned with two high-symmetry directions in the hexagonal basal plane for H || c. Above a critical angle, the intermediate state disappears, and the previously continuous transition becomes discontinuous. Finally, the evolution towards the discontinuous transition can be parametrized by a vanishing twelvefold anisotropy term in the VL free energy.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Nanometric modulations of the magnetic structure of the element Nd

The rare earth neodymium arguably exhibits the most complex magnetic ordering and series of magnetic phase transitions of the elements. Here we report the results of small-angle neutron scattering (SANS) measurements as a function of temperature and applied magnetic field to study magnetic correlations on nanometer length scales in Nd. We support these results with additional neutron diffraction, thermodynamic and synchrotron x-ray measurements. The SANS measurements reveal the presence of modulation vectors characterizing the ordered spin configuration which exhibit changes in magnitude and direction that are phase dependent. Between 5.9 and 7.6 K an additional modulation vector is observed with magnitude Q = 0.12 Å -1 . This scattering appears to originate from order of the Nd layers which contain a center of inversion. Tracking this modulation vector as a function of magnetic field indicates a phase boundary at ≈1 T. The modulation vectors observed in this study establish the presence of nanometer length scale spin textures which are likely stabilized by frustrated Ruderman–Kittel–Kasuya–Yosida (RKKY) interactions.

36 MATERIALS SCIENCE↗

How to avoid multiple scattering in strongly scattering SANS and USANS samples

Small Angle Neutron Scattering (SANS) and Ultra Small Angle Neutron Scattering (USANS) are the only available experimental techniques to provide seamless non-destructive measurements of the geometry of the accessible and inaccessible pore structure of rocks from sub-nanopore size to the scale of macropores. They have therefore become the measurement of choice for tight reservoir rocks such as organic rich shales. A simplifying assumption in the analysis is, however, that during the path of neutrons through the sample each neutron is only scattered once. Shales are samples with a high scattering power and Multiple Scattering (MS) may occur which requires special modelling for deconvolution of the results. The approach to avoid MS is to simply reduce the sample thickness to <0.15–0.5 mm. Here, in this work, we present a systematic method on wavelength selection and preparation of samples to optimise extraction of microstructural data and minimise parasitic errors. Experimentally measured SAS transmission (TSAS) values are used as a practical criterion for estimation of the extent of MS. Generous beamtime allocations allowed robust testing revealing that sample thicknesses can be twice as thick as predicted using the standard protocol. Analysing thicker samples is particularly beneficial for statistically relevant characterisation of heterogeneous samples making the new protocol the method of choice for such samples.

(U)SANS↗

A Unified User-Friendly Instrument Control and Data Acquisition System for the ORNL SANS Instrument Suite

In an effort to upgrade and provide a unified and improved instrument control and data acquisition system for the Oak Ridge National Laboratory (ORNL) small-angle neutron scattering (SANS) instrument suite—biological small-angle neutron scattering instrument (Bio-SANS), the extended q-range small-angle neutron scattering diffractometer (EQ-SANS), the general-purpose small-angle neutron scattering diffractometer (GP-SANS)—beamline scientists and developers teamed up and worked closely together to design and develop a new system. We began with an in-depth analysis of user needs and requirements, covering all perspectives of control and data acquisition based on previous usage data and user feedback. Our design and implementation were guided by the principles from the latest user experience and design research and based on effective practices from our previous projects. In this article, we share details of our design process as well as prominent features of the new instrument control and data acquisition system. The new system provides a sophisticated Q-Range Planner to help scientists and users plan and execute instrument configurations easily and efficiently. The system also provides different user operation interfaces, such as wizard-type tool Panel Scan, a Scripting Tool based on Python Language, and Table Scan, all of which are tailored to different user needs. The new system further captures all the metadata to enable post-experiment data reduction and possibly automatic reduction and provides users with enhanced live displays and additional feedback at the run time. We hope our results will serve as a good example for developing a user-friendly instrument control and data acquisition system at large user facilities.

47 OTHER INSTRUMENTATION↗

Laponite-Incorporated UiO-66-NH2-Polyethylene Oxide Composite Membranes for Protection against Chemical Warfare Agent Simulants

A strategy is developed to enhance the barrier protection of polyethylene oxide (PEO)-metal–organic framework (MOF) composite films against chemical warfare agent simulants. To achieve enhanced protection, an impermeable high-aspect-ratio filler in the form of Laponite RD (LRD) clay platelets was incorporated into a composite PEO film containing MOF UiO-66-NH 2 . The inclusion of the platelets aids in mitigating permeation of inert hydrocarbons (octane) and toxic chemicals (2-chloroethyl ethyl sulfide, 2-CEES) of dimensions/chemistry similar to prominent vesicant threats while still maintaining high water vapor transport rates (WVTR). By utilizing small-angle neutron scattering, small-angle X-ray scattering, and wide-angle X-ray scattering, the LRD platelet alignment of the films was determined, and the structure of the films was correlated with performance as a barrier material. Performance of the membranes against toxic chemical threats was assessed using permeation testing of octane and 2-CEES, a common simulant for the vesicant mustard gas, and breathability of the membranes was assessed using WVTR measurements. To assess their robustness, chemical exposure (in situ diffuse reflectance infrared Fourier transform spectroscopy) and mechanical (tensile strength) measurements were also performed. It was demonstrated that the barrier performance of the film upon inclusion of the LRD platelets exceeds that of other MOF-polymer composites found in the literature and that this approach establishes a new path for improving permselective materials for chemical protection applications.

36 MATERIALS SCIENCE↗

Small-angle scattering interferometry with neutron orbital angular momentum states

Methods to prepare and characterize neutron helical waves carrying orbital angular momentum (OAM) were recently demonstrated at small-angle neutron scattering (SANS) facilities. These methods enable access to the neutron orbital degree of freedom which provides new avenues of exploration in fundamental science experiments as well as in material characterization applications. However, it remains a challenge to recover phase profiles from SANS measurements. We introduce and demonstrate a novel neutron interferometry technique for extracting phase information that is typically lost in SANS measurements. An array of reference beams, with complementary structured phase profiles, are put into a coherent superposition with the array of object beams, thereby manifesting the phase information in the far-field intensity profile. We demonstrate this by resolving petal-structure signatures of helical wave interference for the first time: an implementation of the long-sought recovery of phase information from small-angle scattering measurements.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Accessibility of Pores to Methane in New Albany Shale Samples of Varying Maturity Determined Using SANS and USANS

The accessibility of pores to methane has been investigated in Devonian New Albany Shale Formation early-mature (Ro = 0.50%) to post-mature (Ro = 1.40%) samples. A Marcellus Shale Formation sample was included to expand the maturation range to Ro 2.50%. These are organic matter-rich rocks with total organic carbon (TOC) values of 3.4 to 14.4% and porosity values of 2.19 to 6.88%. Contrast matching small-angle neutron scattering (SANS) and ultra-small angle neutron scattering (USANS) techniques were used to generate porosity-related data before and after pressure cycling under hydrostatic (in a vacuum and at 500 bar of deuterated methane) and uniaxial stress (0 to ca. 350 bar) conditions. Our results showed that the accessible porosity was small for the samples studied, ranging from zero to 2.9%. No correlation between the accessible porosity and TOC or mineralogical composition was revealed, and the most likely explanation for porosity variation was related to the thermal transformation of organic matter and hydrocarbon generation. Pressure caused improvements in accessible porosity for most samples, except the oil window sample (Ro = 0.84%). Our data show that densification of methane occurs in nanopores, generally starting at diameters smaller than 20 nm, and that the distribution of methane density is affected by pressure cycling.

03 NATURAL GAS↗

Water Migration and Swelling in Engineered Barrier Materials for Radioactive Waste Disposal

Deep, underground repositories are needed to isolate radioactive waste from the biosphere. Because bentonite is an integral component of many multibarrier repository systems, information on the hydraulic behavior of bentonite is crucial for modeling the long-term viability of such systems. In this paper the hydraulic behavior of bentonite samples was analyzed as a function of aggregate size, and samples were subjected to hydrothermal treatments involving contact with NaCl, KCl, and deionized water. Neutron and X-ray imaging were used to quantify water sorption into packed bentonite samples and bentonite swelling into the water column. The distance between the original clay-water interface and the wetting front was determined as a function of time. Average water uptake exhibited a square-root-of-time dependence in freshly prepared samples, but more variable rates were observed for samples previously in contact with water. The radiography was supported by small-angle neutron scattering analysis and ultra-small-angle neutron scattering analysis of aggregate size distributions and by inelastic neutron scattering to understand the physicochemical environment of the sorbed water. Results showed that hydrothermal treatment with KCl had the greatest effect of increased water transport in the bentonite, possibly as a result of the interaction of K + with smectite layers in the clay.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗