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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↗

MP1 Intermediate Characterization Report Summary

Great effort worldwide has been invested in replacing high enriched uranium (HEU) fuel with low enriched uranium (LEU) fuel in nuclear plants. This effort aims in safeguarding nuclear material and promoting the proliferation resistance of current reactors. The United States Department of Energy (DOE), National Nuclear Security Administration's (NNSA) Materials Management and Minimization Reactor Conversion program is actively working to convert civilian research and test reactors from the use of HEU to LEU fuel. To date, DOE NNSA has converted or verified the shutdown of various domestic reactors and also reactors worldwide. The task to develop and test a new LEU fuel while maintaining current performances has been assigned to the High-Performance Research Reactor (USHPRR) program. U alloyed with Mo achieves the goal of high uranium density necessary for the conversion of the high performance research reactors, and has also demonstrated good performance in pile [1]. The alloying process of U with Mo stabilizes the body-centered cubic (bcc) gamma phase (?-U) at room temperature. Without this alloying property enhancement, this phase is only stable at temperatures only above 770 °C. Retaining this isotropic gamma phase within the U-Mo alloy provides swelling and oxidation resistance and desired mechanical properties [2]. Generally 10% w. has been considered sufficient to achieve stabilization. However, local phenomena within the alloy can affect the local Mo content and lead to gamma phase decomposition. Because of this, it has been suggested that controlling gamma phase decomposition is most critical during processing [2-3]. The work detailed in this document is part of the HPPR program and focuses on the characterization of fresh fuel (a.k.a. as fabricated, before reactor testing) in collaboration with other laboratories including PNNL (Pacific Northwest National Laboratory), LANL (Los Alamos National Laboratory) and BWXT (Babcock and Wilcox Technologies). This testing is part of a 4 way validation for which similar samples from master plates were taken and distributed to each laboratory to independently analyze utilizing a standardized set of measurement and analysis procedures. When complete this work will supply a “toolbox” of information for alloying and fabrication parameters with its direct effects on microstructure quantified. Various parameters have been analyzed in this characterization effort (including grain size, quality of the coating layer, composition of the samples, carbide content etc.), based on the direction of the working group in ref.[4]. The final aim of this work is to increase the understanding of the impact of processing conditions on the final fuel microstructure, using fabrication processes that meet “commercial viability” requirements [4]. The strength of this campaign rests on the extent of the samples studied and the variation of the manufacture parameters which will permit to achieve the required understanding. Thus permitting to use these experiments to down-select test samples used to evaluate irradiation performance [4] to be tested in various locations of the Idaho National Laboratory (INL) Advanced Test Reactor (ATR).

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Cask RT-100 Type B(U) Self-Certification for DOT 7A, Type A Nuclear Waste Transportation - 20098

The purpose of this Type A certification is to diversify the use of the RT-100 cask by allowing the end user to transport either Type A or Type B radioactive waste in accordance with the handling procedures for each waste category. The project's scope included the development of a matrix that contains all applicable requirements for a Type A package from the Code of Federal Regulations (CFR), Title 49 for the Department of Transportation (DOT) with a justification for each requirement. Moreover, the scope included the writing of conditions and restrictions list for the transportation of Type A nuclear waste, the writing of a compliance statement, and the design and fabrication of a Type A placard to be permanently placed on the RT-100 cask. Type A packages are self-certified by the end user using one of three methods as permitted by 49 CFR 173.461, either by performance of tests with prototypes or samples of the specimens representing the packaging, or reference to a previous satisfactory demonstration of compliance of a sufficiently similar nature, or calculations or reasoned evaluation using reliable and conservative procedures and parameters. Since the RT-100 cask was licensed by the Nuclear Regulatory Commission (NRC) as a Type B cask, Robatel relied on the method of reference to a previous satisfactory demonstration of compliance of a sufficiently similar nature for Type A certification. This method was determined to be acceptable, since Type B packages are evaluated for more demanding transport conditions than those required for Type A packages. This paper presents Robatel's process for certifying the RT-100 cask for Type A shipments, an overview of the DOT regulations related to Type A packages, and the documents that were generated for the end user. This paper is concluded with a discussion on the advantages of having the option to transport both Type A and Type B nuclear waste, and possible future projects to further improve the operation of the cask when making Type A shipments. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Energy and momentum preserving Coulomb collision model for kinetic Monte Carlo simulations of plasma steady states in toroidal fusion devices

A kinetic Monte Carlo model suited for self-consistent transport studies is proposed and tested. The Monte Carlo collision operator is based on a widely used model of Coulomb scattering by a drifting Maxwellian and a new algorithm enforcing the momentum and energy conservation laws. The difference to other approaches consists in a specific procedure of calculating the background Maxwellian parameters, which does not require ensemble averaging and, therefore, allows for the use of single-particle algorithms. This possibility is useful in transport balance (steady state) problems with a phenomenological diffusive ansatz for the turbulent transport, because it allows a direct use of variance reduction methods well suited for single particle algorithms. In addition, a method for the self-consistent calculation of the electric field is discussed. Results of testing of the new collision operator using a set of 1D examples, and preliminary results of 2D modelling in realistic tokamak geometry, are presented.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Beam Commissioning Results from the CBETA Fractional Arc Test (CBETA Note 030)

This work describes first commissioning results from the Cornell Brookhaven ERL Test Accelerator fractional arc test. These include the recommissioning of the Cornell photoinjector, the first full energy operation of the main linac with beam, as well as commissioning of the lowest energy matching beamline (splitter) and a partial section of the Fixed Field Alternating gradient (FFA) return loop featuring first production Halbach style permanent magnets. Achieving these tasks required characterization of the injection beam, calibration and phasing of the main linac cavities, demonstration of the required 36 MeV energy gain, and measurement of the splitter line horizontal dispersion and R 56 at the nominal 42 MeV. In addition, a procedure for determining the BPM offsets, as well as the tune per cell in the FFA section via scanning the linac energy and inducing betatron oscillations around the periodic orbit in the fractional arc was developed and tested. A detailed comparison of these measurements to simulation is discussed.

43 PARTICLE ACCELERATORS↗

A test on reactive force fields for the study of silica dimerization reactions

We studied silica dimerization reactions in the gas and aqueous phase by density functional theory (DFT) and reactive force fields based on two parameterizations of ReaxFF. For each method (both ReaxFF force fields and DFT), we performed constrained geometry optimizations, which were subsequently evaluated in single point energy calculations using the other two methods. Standard fitting procedures typically compare the force field energies and geometries with those from quantum mechanical data after a geometry optimization. The initial configurations for the force field optimization are usually the minimum energy structures of the ab initio database. Hence, the ab initio method dictates which structures are being examined and force field parameters are being adjusted in order to minimize the differences with the ab initio data. As a result, this approach will not exclude the possibility that the force field predicts stable geometries or low transition states which are realistically very high in energy and, therefore, never considered by the ab initio method. Our analysis reveals the existence of such unphysical geometries even at unreactive conditions where the distance between the reactants is large. To test the effect of these discrepancies, we launched molecular dynamics simulations using DFT and ReaxFF and observed spurious reactions for both ReaxFF force fields. Our results suggest that the standard procedures for parameter fitting need to be improved by a mutual comparative method.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Modeling of Environmental-Economic Indicators of Regional Development

One of the current topical problems is the prediction of climate change and mitigation of its consequences. All-sided analysis of ecological, economic, and social aspects of climate issues relies on interdisciplinary assessment models. This article adapts the MERGE optimization model to the current state of the world economy and introduces into the model a new component that implements a simplified procedure of “green” GDP calculation (“green” GDP, or GGDP, provides information about the efficiency of use of environmental resources). The objective of our numerical simulations is to tests the consequences of Russia’s hypothetical participation in the program for reducing greenhouse gas (GHG) emissions and to analyze the environmental indicators of Russia’s GDP. The input data are mainly provided by the project of scenario conditions and main macroeconomic parameters for the forecasting of socio-economic development in Russia in the near future implemented by the Ministry of Economic Development of the Russian Federation. The calculations reveal the existence of reserves for Russia’s “painless” participation in environment-preserving initiatives that call for not exceeding the 1990 emission level in 2020–2025. At the same time, increasing the environmental efficiency of Russia’s GDP is a relevant task that requires immediate attention.

29 ENERGY PLANNING, POLICY, AND ECONOMY↗

Finite element model for piles in liquefiable ground

This paper develops a three dimensional finite element modelling method for piles in liquefiable ground and applies it to the analysis of seismic pile responses. A unified plasticity model for large post-liquefaction shear deformation of sand provides the basis for the effective and efficient modelling of liquefiable ground. Special attention is dedicated towards the modelling of piles and soil-pile interface to accurately reflect the behaviour of piles. A staged modelling procedure is adopted to appropriately generate the initial conditions for the soil and piles and achieve hydrostatic pore pressure prior to seismic loading. Three centrifuge shaking table tests on single piles, both with and without pile cap and superstructure, in level and inclined liquefiable ground are conducted and simulated in validation and application of the proposed method. Further studies to investigate the effects of pile cap, lateral spreading, and non-liquefiable surface layer are undertaken numerically using the validated method. The results show these aforementioned factors to be influential in the dynamic and residual response of piles in liquefiable ground.

Centrifuge test↗

Survey of Surveys: I. The largest compilation of radial velocities for the Galaxy

In the present-day panorama of large spectroscopic surveys, the amount, diversity, and complexity of the available data continuously increase. The overarching goal of studying the formation and evolution of our Galaxy is hampered by the heterogeneity of instruments, selection functions, analysis methods, and measured quantities. Here, we present a comprehensive catalogue, the Survey of Surveys (SoS), built by homogeneously merging the radial velocity (RV) determinations of the largest ground-based spectroscopic surveys to date, such as APOGEE, GALAH, Gaia-ESO, RAVE, and LAMOST, using Gaia as a reference. This pilot study serves to prove the concept and to test the methodology that we plan to apply in the future to the stellar parameters and abundance ratios as well. We have devised a multi-staged procedure that includes: (i) the cross match between Gaia and the spectroscopic surveys using the official Gaia cross-match algorithm, (ii) the normalisation of uncertainties using repeated measurements or the three-cornered hat method, (iii) the cross calibration of the RVs as a function of the main parameters on which depend (magnitude, effective temperature, surface gravity, metallicity, and signal-to-noise ratio) to remove trends and zero point offsets, and (iv) the comparison with external high-resolution samples, such as the Gaia RV standards and the Geneva-Copenhagen survey, to validate the homogenisation procedure and to calibrate the RV zero-point of the SoS catalogue. We provide the largest homogenised RV catalogue to date, containing almost 11 million stars, of which about half come exclusively from Gaia and half in combination with the ground-based surveys. We estimate the accuracy of the RV zero-point to be about 0.16–0.31 km s –1 and the RV precision to be in the range 0.05–1.50 km s –1 depending on the type of star and on its survey provenance. We validate the SoS RVs with open clusters from a high resolution homogeneous samples and provide the systemic velocity of 55 individual open clusters. Additionally, we provide median RVs for 532 clusters recently discovered by Gaia data. The SoS is publicly available and ready to be applied to various research projects, such as the study of star clusters, Galactic archaeology, stellar streams, or the characterisation of planet-hosting stars, to name a few. We also plan to include survey updates and more data sources in future versions of the SoS.

79 ASTRONOMY AND ASTROPHYSICS↗

The DES Science Verification weak lensing shear catalogues

Here, we present weak lensing shear catalogues for 139 square degrees of data taken during the Science Verification (SV) time for the new Dark Energy Camera (DECam) being used for the Dark Energy Survey (DES). We also describe our object selection, point spread function estimation and shear measurement procedures using two independent shear pipelines, IM3SHAPE and NGMIX, which produce catalogues of 2.12 million and 3.44 million galaxies, respectively. Furthermore, we detail a set of null tests for the shear measurements and find that they pass the requirements for systematic errors at the level necessary for weak lensing science applications using the SV data. Finally, we discuss some of the planned algorithmic improvements that will be necessary to produce sufficiently accurate shear catalogues for the full 5-yr DES, which is expected to cover 5000 square degrees.

79 ASTRONOMY AND ASTROPHYSICS↗

Evaluation Of Year 2020 IEEE RTS Generation Reliability Indices

A new IEEE Reliability Test System (2017 update) with wind and solar sources modeling 2020 has been created by NREL and posted on the GitHub RTS-GMLC repository. A simple procedure duplicates the 1979 RTS 'exact' indices and calculates indices for the 1996 RTS and the new 2020 Model RTS 'exact' indices. Extremely fast execution is realized by simply 'looking up' the exact LOLPs each hour from a COPT. Wind and solar are treated as hourly demand reducers. Computer program codes are included.

29 ENERGY PLANNING, POLICY, AND ECONOMY↗

Status and Challenges in the MQXFB Nb 3 Sn Quadrupoles for the HL-LHC

The inner triplet (or low-β) quadrupole magnets are among the components to be upgraded in LHC interaction regions for the HL-LHC project. The new quadrupole magnets, called MQXF, are based on Nb 3 Sn superconducting magnet technology, with a conductor peak field of 11.3 T. CERN is in charge of the fabrication of the MQXFB variant, the longest Nb 3 Sn accelerator magnets designed and manufactured up to now, with a magnetic length of 7.2 m. Two magnets, MQXFBP3 and MQXFB02, reached the HL-LHC project requirements. However, they still exhibited a limitation at 4.5 K with a phenomenology similar to the one observed on the first two prototypes. After improvements on the cold mass (longitudinal welding) and magnet assembly (elimination of overstress on the conductor during loading) procedures, a series of modifications were implemented in MQXFB03 at the level of the coil fabrication to address and/or reduce weaknesses in the coils. The magnet was tested and was the first to achieve performance requirements at both 1.9 K and 4.5 K, with no signs of conductor limitation at 4.5 K. MQXFB is now in the series production phase, with around 2/3 of the coils completed and half of the magnets assembled. We provide in this paper an overview of the MQXFB program, with a summary of the main recent achievements and an overall status of the fabrication.

43 PARTICLE ACCELERATORS↗

PCB-on-DBC GaN Power Module Design with High-Density Integration and Double-Sided Cooling

Lateral gallium nitride (GaN) high-electron-mobility transistors (HEMTs) present better electrical characteristics compared to silicon or silicon carbide devices such as high switching speed and low gate charge, but also present additional challenges on the module design. Here, this paper discusses a high-density GaN power module with double-sided cooling, low inductance, on-package decoupling capacitors, and integrated gate drivers. The GaN dies as well as the gate drive are sandwiched between the printed circuit board (PCB) and direct bonded copper (DBC) substrate to achieve compact loop and double-sided cooling effect. Design considerations and thermal performance are analyzed. A module assembly procedure is presented utilizing the layer-by-layer attachment process. Finally, a 2.7 cm x 1.8 cm half-bridge GaN power module is fabricated and tested, achieving a low power-loop inductance of 1.03 nH, and the overshoot voltage of the switching waveform is less than 5% under a 400-V/25-A double-pulse test. The thermal resistance is 0.32 K/W, verified by simulation and experimental results. The design and assembly process can be generalized and applied to high power applications to achieve high power density and high performance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Mechanical Characterization Study of Sintered Silver Pastes Bonded in a Double-Lap Configuration

Sintered silver-based bonded interfaces are a critical enabling technology for high-temperature, compact, high-performance, and reliable wide-bandgap packages and components. High-pressure (~40 MPa) sintered silver interfaces have been implemented commercially, most notably the commercial products offered by Semikron. To reduce manufacturing complexity, there is significant industry interest in pressure-less sintered silver interfaces. To this end, current formulations of sintered silver paste are comprised of purely nano-sized silver particles or a combination of nano- and micro-sized silver particles/flakes. It is essential to quantify the mechanical properties and determine the reliability of these interfaces prior to use in automotive power electronics applications. In this paper, research efforts at the National Renewable Energy Laboratory, in collaboration with Virginia Polytechnic Institute and State University and an industry partner, in optimizing the synthesis procedure and mechanical characterization of sintered silver double-lap samples are described. These double-lap samples were synthesized using pressure-less sintering techniques. Shear testing was conducted at multiple temperatures and displacement rates on these samples sintered using two types of sintered sintered silver pastes, one of them consisting of nano-silver particles and the other a hybrid paste or a combination of nano- and micron-sized silver flakes, employed in a double-lap configuration. Maximum values of shear stress obtained from the characterization study are reported.

33 ADVANCED PROPULSION SYSTEMS↗

Correction of Dual-PRF Doppler Velocity Outliers in the Presence of Aliasing

Abstract In Doppler weather radars, the presence of unfolding errors or outliers is a well-known quality issue for radial velocity fields estimated using the dual–pulse repetition frequency (PRF) technique. Postprocessing methods have been developed to correct dual-PRF outliers, but these need prior application of a dealiasing algorithm for an adequate correction. This paper presents an alternative procedure based on circular statistics that corrects dual-PRF errors in the presence of extended Nyquist aliasing. The correction potential of the proposed method is quantitatively tested by means of velocity field simulations and is exemplified in the application to real cases, including severe storm events. The comparison with two other existing correction methods indicates an improved performance in the correction of clustered outliers. The technique proposed is well suited for real-time applications requiring high-quality Doppler radar velocity fields, such as wind shear and mesocyclone detection algorithms, or assimilation in numerical weather prediction models.

58 GEOSCIENCES↗

Benchmark Analysis

Tremendous progress has been achieved in the development of land models and their inclusion in Earth system models (ESMs). However, we still have very limited knowledge on the performance skills of these land models. This chapter introduces benchmark analysis, which is a procedure to measure performance of models against a set of defined standards. The benchmark analysis includes: (1) defining targeted aspects of model performance to be evaluated; (2) testing model performance in comparison with a set of benchmarks; (3) measuring model performance skill through quantitative metrics; and (4) evaluating model performance and offering suggestions for future model improvement.

Luo, Yiqi↗

Direct Utilization of Coal Syngas in High Temperature Fuel Cells

This EPSCoR project had two primary goals: (i) to build infrastructure and work force at WVU to support long-term research in the area of fuel cells and related sciences; (ii) study effects of various impurities found in coal-syngas on performance of Solid Oxide Fuel Cells (SOFC). As detailed in this report the WVU research team has made significant accomplishments in both of these areas. What follows is a brief summary of these accomplishments: State-of-the-art test facilities and diagnostic tools have been built and put into use. These include cell manufacturing, half-cell and full-cell test benches, XPS, XRD, TEM, Raman, EDAX, SEM, EIS, and ESEM equipment, unique in-situ measurement techniques and test benches (Environmental EM, Transient Mass-Spectrometer-MS, and IR Optical Temperature measurements). In addition, computational capabilities have been developed culminating in a multi-scale multi-physics fuel cell simulation code, DREAM-SOFC, as well as a Beowulf cluster with 64 CPU units. We have trained 16 graduate students, 10 postdoctoral fellows, and recruited 4 new young faculty members who have actively participated in the EPSCoR project. All four of these faculty members have already been promoted to the tenured associate professor level. With the help of these faculty and students, we were able to secure 14 research awards/contracts amounting to a total of circa $5.0 Million external funding in closely related areas of research. Using the facilities mentioned above, the effects of PH3, HCl, Cl2, and H2S on cell performance have been studied in detail, mechanisms have been identified, and also remedies have been proposed and demonstrated in the laboratory. For example, it has been determined that PH3 reacts rapidly with Ni to from secondary compounds which may become softer or even melt at high temperature and then induce Ni migration to the surface of the cell changing the material and micro-structural properties of the cell drastically. It is found that the extent of steam and current load accelerate the degradation caused by PH3. A unique filtering technique has been proposed to reduce the effect of PH3. In addition, various cell materials have been proposed to reduce the rate of degradation caused by H2S. Furthermore, a three-dimensional, transient multi-physics model has been formulated to describe primary transport processes and electro-chemical reactions occurring within the cell. This model has been validated using data gathered from accelerated tests. The validated model then has been used to study the degradation rates under a range of operating conditions and impurity levels. This has resulted in a procedure that uses both experiments and simulations to predict the life-time of a cell operating with syngas with known concentration of trace impurities. Finally all the experience and knowledge gained has been disseminated via 39 journal papers and 43 presentations/posters/conference papers.

01 COAL, LIGNITE, AND PEAT↗

Report on the FY18 creep rupture and creep-fatigue tests on the first commercial heat of Alloy 709

Creep, fatigue and creep-fatigue tests were performed on the Carlson plate of Alloy 709 (ID 58776). The plate, which is the first of the commercial heats tested, was divided into several sections, each undergoing different processing conditions. The effects of processing method and solution annealing temperature were studied in FY18 to inform best procedures for the second heat. The solution annealing temperature of 1050°C was found to be unacceptable due to the grain size being smaller than allowed by the specifications, as well as generally having poor creep properties. Both argon oxygen decarburization AOD and electro-slag remeltin ESR were found to have desirable properties, and the homogenization heat treatment was found to not significantly improve the mechanical properties.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗