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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 19 records

Binary pseudo-random patterned structures for modulation transfer function calibration and resolution characterization of a full-field transmission soft x-ray microscope

We present a modulation transfer function (MTF) calibration method based on binary pseudo-random (BPR) one-dimensional sequences and two-dimensional arrays as an effective method for spectral characterization in the spatial frequency domain of a broad variety of metrology instrumentation, including interferometric microscopes, scatterometers, phase shifting Fizeau interferometers, scanning and transmission electron microscopes, and at this time, x-ray microscopes. The inherent power spectral density of BPR gratings and arrays, which has a deterministic white-noise-like character, allows a direct determination of the MTF with a uniform sensitivity over the entire spatial frequency range and field of view of an instrument. We demonstrate the MTF calibration and resolution characterization over the full field of a transmission soft x-ray microscope using a BPR multilayer (ML) test sample with 2.8 nm fundamental layer thickness. We show that beyond providing a direct measurement of the microscope’s MTF, tests with the BPRML sample can be used to fine tune the instrument’s focal distance. Our results confirm the universality of the method that makes it applicable to a large variety of metrology instrumentation with spatial wavelength bandwidths from a few nanometers to hundreds of millimeters.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

The National Ignition Facility modular Kirkpatrick-Baez microscope

Current two-dimensional X-ray imaging at the National Ignition Facility (NIF) uses time resolved pinhole cameras with ∼10-25 μm pinholes. This method has limitations in the smallest resolvable features that can be imaged with reasonable photon statistics for inertial confinement fusion (ICF) applications. ICF sources have a broadband self-emission spectrum that causes the pinhole images obtained, through thin foil filters, to contain a similarly broadband spectrum complicating the interpretation of structure in the source. In order to study phenomena on the scale of ∼5 μm, such as dopant mix in the ICF capsule, a narrow energy band, higher spatial resolution microscope system with improved signal/noise has been developed using X-ray optics. Utilizing grazing incidence mirrors in a Kirkpatrick-Baez microscope (KBM) configuration [P. Kirkpatrick and A. V. Baez, J. Opt. Soc. Am. 38, 766–774 (1948)], an X-ray microscope has been designed and fielded on NIF with four imaging channels. The KBM has ∼12 × magnification, <8 μm resolution, and higher throughput in comparison to similar pinhole systems. The first KBM mirrors are coated with a multilayer mirror to allow a “narrow band” energy response at 10.2 keV with ΔE ∼ 3 keV. By adjusting the mirror coating only, the energy response can be matched to the future experimental requirements. Several mirror packs have been commissioned and are interchangeable in the diagnostic snout.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Automated markerless full field hard x-ray microscopic tomography at sub-50nm 3-dimension spatial resolution

A full field transmission x-ray microscope (TXM) has been developed and commissioned at the National Synchrotron Light Source at Brookhaven National Laboratory. The capabilities we developed in auto-tomography, local tomography, and spectroscopic imaging that overcome many of the limitations and difficulties in existing transmission x-ray microscopes are described and experimentally demonstrated. Sub-50 nm resolution in 3-dimension (3D) with markerless automated tomography has been achieved. These capabilities open up scientific opportunities in many research fields.

36 MATERIALS SCIENCE↗

Coupling a nano-particle with isothermal fluctuating hydrodynamics: Coarse-graining from microscopic to mesoscopic dynamics

We derive a coarse-grained description of the dynamics of a nanoparticle immersed in an isothermal simple fluid by performing a systematic coarse graining of the underlying microscopic dynamics. As coarse-grained or relevant variables, we select the position of the nanoparticle and the total mass and momentum density field of the fluid, which are locally conserved slow variables because they are defined to include the contribution of the nanoparticle. The theory of coarse graining based on the Zwanzing projection operator leads us to a system of stochastic ordinary differential equations that are closed in the relevant variables. We demonstrate that our discrete coarse-grained equations are consistent with a Petrov-Galerkin finite-element discretization of a system of formal stochastic partial differential equations which resemble previously used phenomenological models based on fluctuating hydrodynamics. Key to this connection between our “bottom-up” and previous “top-down” approaches is the use of the same dual orthogonal set of linear basis functions familiar from finite element methods (FEMs), both as a way to coarse-grain the microscopic degrees of freedom and as a way to discretize the equations of fluctuating hydrodynamics. Another key ingredient is the use of a “linear for spiky” weak approximation which replaces microscopic “fields” with a linear FE interpolant inside expectation values. For the irreversible or dissipative dynamics, we approximate the constrained Green-Kubo expressions for the dissipation coefficients with their equilibrium averages. Under suitable approximations, we obtain closed approximations of the coarse-grained dynamics in a manner which gives them a clear physical interpretation and provides explicit microscopic expressions for all of the coefficients appearing in the closure. Our work leads to a model for dilute nanocolloidal suspensions that can be simulated effectively using feasibly short molecular dynamics simulations as input to a FEM fluctuating hydrodynamic solver.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Microscopic theory of singlet exciton fission. III. Crystalline pentacene

We extend our previous work on singlet exciton fission in isolated dimers to the case of crystalline materials, focusing on pentacene as a canonical and concrete example. We discuss the proper interpretation of the character of low-lying excited states of relevance to singlet fission. In particular, we consider a variety of metrics for measuring charge-transfer character, conclusively demonstrating significant charge-transfer character in the low-lying excited states. The impact of this electronic structure on the subsequent singlet fission dynamics is assessed by performing real-time master-equation calculations involving hundreds of quantum states. We make direct comparisons with experimental absorption spectra and singlet fission rates, finding good quantitative agreement in both cases, and we discuss the mechanistic distinctions that exist between small isolated aggregates and bulk systems.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

An in-vacuum x-ray diffraction microscope for use in the 0.7-2.9 keV range

A dedicated in-vacuum coherent x-ray diffraction microscope was installed at the 2-ID-B beamline of the Advanced Photon Source for use with 0.7-2.9 keV x-rays. The instrument can accommodate three common implementations of diffractive imaging; plane wave illumination; defocused-probe (Fresnel diffractive imaging) and scanning (ptychography) using either a pinhole, focused or defocused probe. The microscope design includes active feedback to limit motion of the optics with respect to the sample. Upper bounds on the relative optics-to-sample displacement have been measured to be 5.8 nm(v) and 4.4 nm(h) rms/h using capacitance micrometry and 27 nm/h using x-ray point projection imaging. The stability of the measurement platform and in-vacuum operation allows for long exposure times, high signal-to-noise and large dynamic range two-dimensional intensity measurements to be acquired. Finally, we illustrate the microscope's stability with a recent experimental result.

43 PARTICLE ACCELERATORS↗

Quantitative Defect Analysis of Ablator Capsule Surfaces Using a Leica Confocal Microscope and a High-Density Atomic Force Microscope

High-density carbon (HDC) is being evaluated as an alternative to the current National Ignition Facility (NIF) point-design ablator material (glow discharge plasma, or GDP, plastic) due to its high density and optimal opacity, which leads to a higher implosion velocity. Chemical-vapor-deposition-coated HDC capsules have a near perfect surface figure but a microscopically rough surface. After polishing, the surface becomes smooth at nanometer scales but has numerous micron-sized surface pits, whose volumes, morphology, and distribution must be quantified to guide NIF target selection. Traditional metrology tools for GDP surface defects, such as the atomic force microscope (AFM) based Spheremapper and a phase-shifting differential interferometer, lack the resolution to characterize these localized features. In this paper, we describe how this metrology challenge is met by developing automated surface metrology solutions based on a high-density (HD) AFM and a Leica confocal microscope. Furthermore, these tools are complementary in nature. HD-AFM has a 0.1-μm spatial resolution and determines the overall shape distortion and pit statistics by tracing great circles on a capsule with high throughput.

36 MATERIALS SCIENCE↗

Refined tip preparation by electrochemical etching and ultrahigh vacuum treatment to obtain atomically sharp tips for scanning tunneling microscope and atomic force microscope

A modification of the common electrochemical etching setup is presented. The described method reproducibly yields sharp tungsten tips for usage in the scanning tunneling microscope and tuning fork atomic force microscope. In situ treatment under ultrahigh vacuum (p {<=}10{sup -10} mbar) conditions for cleaning and fine sharpening with minimal blunting is described. The structure of the microscopic apex of these tips is atomically resolved with field ion microscopy and cross checked with field emission.

36 MATERIALS SCIENCE↗

Electron Microscopic Evaluation and Fission Product Identification of Irradiated TRISO Coated Particles from the AGR-1 Experiment: A Preliminary Review

Post-irradiation examination of coated particle fuel from the AGR-1 experiment is in progress at Idaho National Laboratory and Oak Ridge National Laboratory. In this paper a brief summary of results from characterization of microstructures in the coating layers of selected irradiated fuel particles with burnup of 11.3% and 19.3% FIMA will be given. The main objectives of the characterization were to study irradiation effects, fuel kernel porosity, layer debonding, layer degradation or corrosion, fission-product precipitation, grain sizes, and transport of fission products from the kernels across the TRISO layers. Characterization techniques such as scanning electron microscopy, transmission electron microscopy, energy dispersive spectroscopy, and wavelength dispersive spectroscopy were used. A new approach to microscopic quantification of fission-product precipitates is also briefly demonstrated. Microstructural characterization focused on fission-product precipitates in the SiC-IPyC interface, the SiC layer and the fuel-buffer interlayer. The results provide significant new insights into mechanisms of fission-product transport. Although Pd-rich precipitates were identified at the SiC-IPyC interlayer, no significant SiC-layer thinning was observed for the particles investigated. Characterization of these precipitates highlighted the difficulty of measuring low concentrations of Ag in precipitates with significantly higher concentrations of Pd and U. Different approaches to resolving this problem are discussed. An initial hypothesis is provided to explain fission-product precipitate compositions and locations. No SiC phase transformations were observed and no debonding of the SiC-IPyC interlayer as a result of irradiation was observed for the samples investigated. Lessons learned from the post-irradiation examination are described and future actions are recommended.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Performance and characterization of the prototype nm-scale spatial resolution scanning multilayer Laue lenses microscope

Synchrotron based x-ray microscopy established itself as a prominent tool for noninvasive investigations in many areas of science and technology. Many facilities around the world routinely achieve sub-micrometer resolution with a few instruments capable of imaging with the spatial resolution better than 100 nm. With an ongoing effort to push the 2D/3D resolution down to 10 nm in the hard x-ray regime both fabrication of the nano-focusing optics and stability of a microscope become extremely challenging. In this work we present our approach to overcome technical challenges on the path towards high spatial resolution hard x-ray microscopy and demonstrate the performance of a scanning fluorescence microscope equipped with the multilayer Laue lenses focusing optics.

36 MATERIALS SCIENCE↗

Probing the limits of Si:P δ -doped devices patterned by a scanning tunneling microscope in a field-emission mode

Recently, a single atom transistor was deterministically fabricated using phosphorus in Si by H-desorption lithography with a scanning tunneling microscope (STM). This milestone in precision, achieved by operating the STM in the conventional tunneling mode, typically utilizes slow (∼102 nm2/s) patterning speeds. By contrast, using the STM in a high-voltage (>10 V) field-emission mode, patterning speeds can be increased by orders of magnitude to ≳104 nm2/s. We show that the rapid patterning negligibly affects the functionality of relatively large micron-sized features, which act as contacting pads for these devices. For nanoscale structures, we show that the resulting electrical transport is consistent with the donor incorporation chemistry constraining the electrical dimensions to a scale of 10 nm even though the pattering spot size is 40 nm.

Rudolph, M.↗