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2018 Annual Report Laboratory Directed Research and Development at Pacific Northwest National Laboratory

A national laboratory must establish and maintain an environment in which creativity and innovation are encouraged and supported in order to fulfill its missions and remain viable in the long term. As such, multiprogram laboratories are given discretion to allocate a percentage of their operating budgets to support research and development projects that align to PNNL’s and DOE’s missions and support the missions of other federal agencies, including DHS, DOD, and others. Individual project reports comprise the bulk of this LDRD report. The Laboratory focuses its LDRD research on scientific assets that often address more than one scientific discipline.

96 KNOWLEDGE MANAGEMENT AND PRESERVATION↗

Managing EHS of PV-Related Equipment at the National Renewable Energy Laboratory: Preprint

Managing environment, health, and safety (EHS) risks at a national laboratory, or university, can be intimidating to a researcher who is focused on research results. Laboratory research and development (R&D) operations are often driven by scientists with limited engineering support and lack well-refined equipment development resources. To add to the burden for a researcher, there is a plethora ofcodes, standards, and regulations that govern the safe installation and operation of photovoltaic-related R&D equipment -- especially those involving hazardous production materials. To help guide the researcher through the vast list of requirements, the EHS office at NREL has taken a variety of steps. Organizationally, the office has developed hazard-specific laboratory-level procedures togovern particular activities. These procedures are a distillation of appropriate international codes, fire agencies, SEMI standards, U.S. Department of Energy orders, and other industry standards to those necessary and sufficient to govern the safe operation of a given activity. The EHS office works proactively with researchers after a concept for a new R&D capability is conceived to help guidethe safe design, acquisition, installation, and operation of the equipment. It starts with a safety assessment at the early stages such that requirements are implemented to determine the level of risk and degree of complexity presented by the activity so appropriate controls can be put in place to manage the risk. As the equipment requirements and design are refined, appropriate equipmentstandards are applied. Before the 'to-build' specifications are finalized, a process hazard analysis is performed to ensure that no single-point failure presents an unacceptable risk. Finally, as the tool goes through construction and installation stages, reviews are performed at logical times to ensure that the requisite engineering controls and design are in place and operational.Authorization to operate is not given until adherence to these requirements is fully verified and documented. Operations continue under the conditions defined through this process and are reviewed with changing processes.

14 SOLAR ENERGY↗

Design of the Laboratory-Scale Plutonium Oxide Processing Unit in the Radiochemical Processing Laboratory

This report describes a design for a laboratory-scale capability to produce plutonium oxide (PuO 2 ) for use in identifying and validating nuclear forensics signatures associated with plutonium production, as well as for use as exercise and reference materials. This capability will be located in the Radiochemical Processing Laboratory at the Pacific Northwest National Laboratory. The key unit operations are described, including PuO 2 dissolution, purification of the Pu by ion exchange, precipitation, and re-conversion to PuO 2 by calcination.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

Laboratory-Based Micro-X-ray Computed Tomography of Energy Materials at Idaho National Laboratory

Abstract The Idaho National Laboratory (INL) has implemented laboratory-based micro-X-ray computed tomography in a laboratory equipped for the examination of highly radioactive samples. This capability provides nondestructive three-dimensional volumetric information on samples to inform subsequent traditional destructive examinations as well as real-world inputs for high-fidelity scientific modeling. Samples can be imaged with spatial resolutions ranging from several hundred nm/voxel up to ~ 100 µm/voxel. The best usable spatial resolution achieved to date is 384 nm/voxel with this instrument, while the highest radiological dose rate of a sample imaged is ~ 60 R/h β/γ on contact. Advanced data analysis, including custom tomographic reconstruction and segmentation methods, have also been developed to support this capability. In addition to traditional digital X-ray radiography and tomography, this instrument is also able to visualize in situ tensile and compression testing as well as perform diffraction contrast tomography. This work describes the X-ray computed tomography post-irradiation examination capabilities at INL, as well as detailing a variety of applications this instrument has examined.

36 MATERIALS SCIENCE↗

Acoustic Energy Release During the Laboratory Seismic Cycle: Insights on Laboratory Earthquake Precursors and Prediction

Abstract Machine learning can predict the timing and magnitude of laboratory earthquakes using statistics of acoustic emissions. The evolution of acoustic energy is critical for lab earthquake prediction; however, the connections between acoustic energy and fault zone processes leading to failure are poorly understood. Here, we document in detail the temporal evolution of acoustic energy during the laboratory seismic cycle. We report on friction experiments for a range of shearing velocities, normal stresses, and granular particle sizes. Acoustic emission data are recorded continuously throughout shear using broadband piezo‐ceramic sensors. The coseismic acoustic energy release scales directly with stress drop and is consistent with concepts of frictional contact mechanics and time‐dependent fault healing. Experiments conducted with larger grains (10.5 μm) show that the temporal evolution of acoustic energy scales directly with fault slip rate. In particular, the acoustic energy is low when the fault is locked and increases to a maximum during coseismic failure. Data from traditional slide‐hold‐slide friction tests confirm that acoustic energy release is closely linked to fault slip rate. Furthermore, variations in the true contact area of fault zone particles play a key role in the generation of acoustic energy. Our data show that acoustic radiation is related primarily to breaking/sliding of frictional contact junctions, which suggests that machine learning‐based laboratory earthquake prediction derives from frictional weakening processes that begin very early in the seismic cycle and well before macroscopic failure.

58 GEOSCIENCES↗

Inter-laboratory testing of the effect of DNA blocking reagent G2 on DNA extraction from low-biomass clay samples [Inter-laboratory testing of the effect of DNA blocking reagent G2 on DNA extraction from low-biomass clay subsoil]

Here we show that a commercial blocking reagent (G2) based on modified eukaryotic DNA significantly improved DNA extraction efficiency. We subjected G2 to an inter-laboratory testing, where DNA was extracted from the same clay subsoil using the same batch of kits. The inter-laboratory extraction campaign revealed large variation among the participating laboratories, but the reagent increased the number of PCR-amplified16S rRNA genes recovered from biomass naturally present in the soils by one log unit. Furthermore, an extensive sequencing approach demonstrated that the blocking reagent was free of contaminating DNA, and may therefore also be used in metagenomics studies that require direct sequencing.

59 BASIC BIOLOGICAL SCIENCES↗

A practical superconducting-microcalorimeter X-ray spectrometer for beamline and laboratory science

We describe a series of microcalorimeter X-ray spectrometers designed for a broad suite of measurement applications. The chief advantage of this type of spectrometer is that it can be orders of magnitude more efficient at collecting X-rays than more traditional high-resolution spectrometers that rely on wavelength-dispersive techniques. This advantage is most useful in applications that are traditionally photon-starved and/or involve radiation-sensitive samples. Each energy-dispersive spectrometer is built around an array of several hundred transition-edge sensors (TESs). TESs are superconducting thin films that are biased into their superconducting-to-normal-metal transitions. The spectrometers share a common readout architecture and many design elements, such as a compact, 65 mK detector package, 8-column time-division-multiplexed superconducting quantum-interference device readout, and a liquid-cryogen-free cryogenic system that is a two-stage adiabatic-demagnetization refrigerator backed by a pulse-tube cryocooler. We have adapted this flexible architecture to mate to a variety of sample chambers and measurement systems that encompass a range of observing geometries. There are two different types of TES pixels employed. The first, designed for X-ray energies below 10 keV, has a best demonstrated energy resolution of 2.1 eV (full-width-at-half-maximum or FWHM) at 5.9 keV. The second, designed for X-ray energies below 2 keV, has a best demonstrated resolution of 1.0 eV (FWHM) at 500 eV. Our team has now deployed seven of these X-ray spectrometers to a variety of light sources, accelerator facilities, and laboratory-scale experiments; these seven spectrometers have already performed measurements related to their applications. Another five of these spectrometers will come online in the near future. We have applied our TES spectrometers to the following measurement applications: synchrotron-based absorption and emission spectroscopy and energy-resolved scattering; accelerator-based spectroscopy of hadronic atoms and particle-induced-emission spectroscopy; laboratory-based time-resolved absorption and emission spectroscopy with a tabletop, broadband source; and laboratory-based metrology of X-ray-emission lines. Here, we discuss the design, construction, and operation of our TES spectrometers and show first-light measurements from the various systems. Finally, because X-ray-TES technology continues to mature, we discuss improvements to array size, energy resolution, and counting speed that we anticipate in our next generation of TES-X-ray spectrometers and beyond.

47 OTHER INSTRUMENTATION↗

Tritium Laboratory Karlsruhe: administrative and technical framework for isotope laboratory operation

Originally licensed in 1993 the Tritium Laboratory Karlsruhe (TLK) is a unique pilot scale isotope laboratory focused on tritium handling and processing to conduct a variety of scientific experiments and development tasks in view of future fusion power plants. TLK currently operates 15 glove boxes of 125 m{sup 3} total volume in an experimental hall measuring nearly 1500 m{sup 2}. The tritium infrastructure, comprising of the tritium storage system, the tritium transfer system and the isotope separation system, is integrated into TLK as a closed loop system to supply tritium to the experiments. Having a license for handling of up to 40 g of tritium and a closed tritium processing loop, TLK is a unique institute in non-military tritium research. In order to fulfil all requirements regarding the license, a framework of regulations is applied as a basis for the operation of TLK, as well as the setup of new experiments and the design of components. This paper will give an overview on the framework of operation in view of licensing issues, as well as administrative and technical regulations mandatory to legally and reliably operate an isotope laboratory of this scale.

07 ISOTOPE AND RADIATION SOURCES↗

Argonne National Laboratory Annual Report of Laboratory Directed Research and Development program activities FY 2010.

As a national laboratory Argonne concentrates on scientific and technological challenges that can only be addressed through a sustained, interdisciplinary focus at a national scale. Argonne's eight major initiatives, as enumerated in its strategic plan, are Hard X-ray Sciences, Leadership Computing, Materials and Molecular Design and Discovery, Energy Storage, Alternative Energy and Efficiency, Nuclear Energy, Biological and Environmental Systems, and National Security. The purposes of Argonne's Laboratory Directed Research and Development (LDRD) Program are to encourage the development of novel technical concepts, enhance the Laboratory's research and development (R and D) capabilities, and pursue its strategic goals. projects are selected from proposals for creative and innovative R and D studies that require advance exploration before they are considered to be sufficiently developed to obtain support through normal programmatic channels. Among the aims of the projects supported by the LDRD Program are the following: establishment of engineering proof of principle, assessment of design feasibility for prospective facilities, development of instrumentation or computational methods or systems, and discoveries in fundamental science and exploratory development.

99 GENERAL AND MISCELLANEOUS↗

Argonne National Laboratory Annual Report of Laboratory Directed Research and Development program activities FY 2011.

As a national laboratory Argonne concentrates on scientific and technological challenges that can only be addressed through a sustained, interdisciplinary focus at a national scale. Argonne's eight major initiatives, as enumerated in its strategic plan, are Hard X-ray Sciences, Leadership Computing, Materials and Molecular Design and Discovery, Energy Storage, Alternative Energy and Efficiency, Nuclear Energy, Biological and Environmental Systems, and National Security. The purposes of Argonne's Laboratory Directed Research and Development (LDRD) Program are to encourage the development of novel technical concepts, enhance the Laboratory's research and development (R and D) capabilities, and pursue its strategic goals. projects are selected from proposals for creative and innovative R and D studies that require advance exploration before they are considered to be sufficiently developed to obtain support through normal programmatic channels. Among the aims of the projects supported by the LDRD Program are the following: establishment of engineering proof of principle, assessment of design feasibility for prospective facilities, development of instrumentation or computational methods or systems, and discoveries in fundamental science and exploratory development.

99 GENERAL AND MISCELLANEOUS↗

LBNL 2011 Inter-Laboratory Comparison for Laboratories Submitting Specular Data to the International Glazings Database (IGDB)

Laboratories that submit data to the International Glazings Database (IGDB) have to participate in an inter-laboratory comparison (ILC) every four years. This is a procedure that allow both contributors and database maintainers to confirm that the measurement capabilities of the laboratories are of high quality. All laminate and applied film samples are manufactured using the same batch of clear glass to allow for an investigation of the accuracy in the Optics 5 laminate deconstruction process. The IGDB contains optical information in the wavelength region between 300-2500 nm where transmittance as well as reflectance for both the front and the back surface is recorded. In addition to that emissivity, obtained through measurement of reflectance between 5 and 25 m, is recorded for both the front and back surface. The goal for submitters is to pass within the tolerances dictated by NFRC document 302 which states that transmittances should be within 1% and reflectance/emissivity withing 2%. As an organizing entity LBNL aims to educate and help submitters troubleshoot any issues that give rise to systematic errors. The ILC is a living ILC and does not necessarily contain the first result submitted by a lab. As errors are found submitters are encouraged to correct procedures or update equipment so that they are allowed to submit data to the IGDB. The risk of this practice is that if any of the recommended solutions introduces new systematic errors this will start to influence the average. Therefore this report tries to highlight the recommendations made so that they can be challenged.

29 ENERGY PLANNING, POLICY, AND ECONOMY↗

Lawrence Livermore National Laboratory (LLNL) Laboratory Directed Research and Development (LDRD) Annual Report (FY 2023)

As Lawrence Livermore National Laboratory’s most significant resource for supporting internally directed research and development, the LDRD Program provides investments in cutting-edge science and technology that allow the Laboratory to attract and retain the world’s most talented scientists and engineers and enables them to expand the frontiers of knowledge and anticipate emerging national security challenges. In this annual report, we summarize how Lawrence Livermore National Laboratory (LLNL) uses LDRD investments to advance our knowledge in strategic science and technology domains, develop our world-class workforce, and foster innovation in key programmatic areas.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

The Italian Summer Students Program at the Fermi National Accelerator Laboratory and other US Laboratories

Since 1984 INFN scientists performing experiments at Fermilab have been running a two-month summer training program for Italian students at the lab. In 1984 the program involved only a few physics students from the Pisa group, but it was later extended to other groups and to engineering students. Since 2004 the program has been supported in part by DOE in the frame of an exchange agreement with INFN and has been run by the Cultural Association of Italians at Fermilab (CAIF). In 2007 the Sant’Anna School of Advanced Studies (Pisa) established an agreement with Fermilab to share the cost of four engineering students each year. In the 34 years of its history, the program has hosted at Fermilab approximately 530 Italian students from more than 20 Italian universities and from some non-Italian universities . In addition, in the years 2010-2018, with the support of INAF, ASI, and CAIF, 25 students were hosted in other US laboratories and universities. The Fermilab training programs spanned from data analysis to design and construction of particle detectors and accelerator components, R/D on superconductive elements, theory of accelerators, and analysis of astrophysical data. At the other US laboratories the offered training was on Space Science. In 2015 the University of Pisa endorsed the program as one of his own Summer Schools. The interns are enrolled as Pisa students for the duration of the internship. They are required to write summary reports published in the Fermilab and University of Pisa web pages. Upon positive evaluation by a University board, students are acknowledged 6 ECTS credits. In 2017 a new initiative of the Oxford Summer School "MovingKnowledge17" allowed three Fermilab summer students to be trained in neutrino physics to spend the month of July at Oxford to follow an advanced course on HEP.The entire program is expected to expand further under CAIF management. An agreement has been signed between ASI and CAIF, for ASI to support yearly three two-months fellowships in US space science laboratories. The program is also part of the Outreach of the European Projects MUSE (H2020-MSCA-RISE-2015, GA 690835), NEWS (H2020-MSCA-RISE-2016, GA 734303) and INTENSE (H2020-MSCA-RISE-2018, GA 822185 in preparation).

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

Zero-gravity cloud physics laboratory: Experiment program definition and preliminary laboratory concept studies

The experiment program definition and preliminary laboratory concept studies on the zero G cloud physics laboratory are reported. This program involves the definition and development of an atmospheric cloud physics laboratory and the selection and delineations of a set of candidate experiments that must utilize the unique environment of zero gravity or near zero gravity.

Eaton, L. R.↗