Engineering Papers⌕ Search

SEARCH · Engineering Papers

Results for “Positioning Resolution”

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.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 757 records · Page 42
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

High resolution characterization of soil dissolved organic matter with FTICR-MS (Fourier-transform ion cyclotron resonance mass spectrometry) from soil samples in control and warming plots in Blodgett Forest, CA (2014 and 2018)

The pathways of carbon transport and loss through and from soils—soil organic matter (SOM) depolymerization to dissolved organic carbon and mineralization to carbon dioxide (CO2)—are fundamentally driven by microbial activity, which is strongly regulated by environmental conditions. As part of Lawrence Berkeley National Laboratory (LBNL) Terrestrial Ecosystem Science (TES) Belowground Biogeochemistry Science Focus Area (SFA), we have established a novel whole-soil long-term warming experiment at the University of California (UC) Blodgett Forest Research Station (Sierra Nevada) in 2014, where we study the role of biogeochemical, microbial and geochemical process interactions in SOM decomposition and stabilization.This package contains Fourier transform ion cyclotron resonance mass spectrometry (21 Tesla FTICR-MS) data measured in negative and positive ionization mode from water and methanol soil extracts. Soil samples were collected in 2014/06/03 and 2018/06/04 from 3 replicated paired plots that had been subjected to experimental warming since June 2014 to simulate a predicted climate change scenario for northern California. The following files are included: (1) fticr_neg_h2oMeoh_data_raw.csv: raw data from combined water (H2O) and methanol (MeOH) extracts in negative ion mode, (2) fticr_neg_h2oMeoh_data_processed.csv: processed data from combined water (H2O) and methanol (MeOH) extracts in negative ion mode, (3) fticr_neg_metadata.csv: metadata for samples/measurements in negative ion mode, (4) fticr_pos_h2oMeoh_data_raw.csv: raw data from combined water (H2O) and methanol (MeOH) extracts in positive ion mode, (5) fticr_pos_h2oMeoh_data_processed.csv: processed data from combined water (H2O) and methanol (MeOH) extracts in positive ion mode, (6) fticr_pos_metadata.csv: metadata for samples/measurements in positive ion mode.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2026

Identification of a key water molecule involved in the macrophage migration inhibitory factor‐catalyzed tautomerization of para ‐hydroxyphenylpyruvate using neutron crystallography

Abstract Neutron crystallography was used to determine a 2.5‐Å resolution all‐atom structure of macrophage migration inhibitory factor (MIF) interacting with 3‐(4‐hydroxyphenyl)‐pyruvate (HPP). MIF is a pro‐inflammatory, pro‐tumorigenic protein that may be an attractive therapeutic target. MIF catalyzes the interconversion of the keto and enol forms of HPP by a tautomerase reaction. Although HPP is evidently not a physiological substrate of MIF, many compounds that inhibit this activity in enzymatic assays have been found also to inhibit physiological activities of MIF. Therefore, the MIF‐catalyzed HPP tautomerization reaction is used in initial screening of compounds in the search for inhibitors of MIF physiological activity. The neutron diffraction‐derived crystal structure reveals the position of a water molecule involved in the tautomerization reaction, and also confirms the charged state of lysine‐32 in the active site. The structure confirms the previously proposed catalytic mechanism of MIF, with the N‐terminal Pro‐1 abstracting a proton to generate an HPP enolate intermediate which is subsequently protonated. The structure reported herein reveals that this proton is supplied by a neighboring water molecule. Along with the neutron structure, a room‐temperature synchrotron x‐ray crystal structure reveals a covalent adduct between HPP and MIF. While this adduct is a result of radiation‐induced chemistry, its formation confirms the catalytic role of the active site residue because a covalent complex could only form if the reactive carbon of the substrate is correctly positioned by the enzyme.

Schröder, Gabriela C. [Department of Molecular and↗
DOE OSTI2024

Structural, biophysical, and biochemical insights into C–S bond cleavage by dimethylsulfone monooxygenase

Sulfur is an essential element for life. Bacteria can obtain sulfur from inorganic sulfate; but in the sulfur starvation–induced response,Pseudomonadsemploy two-component flavin-dependent monooxygenases (TC-FMOs) from themsuandsfnoperons to assimilate sulfur from environmental compounds including alkanesulfonates and dialkylsulfones. Here, we report binding studies of oxidized FMN to enzymes involved within theP. fluorescensenzymatic pathway responsible for converting dimethylsulfone (DMSO 2 ) to sulfite. In this catabolic pathway, SfnG serves as the initial TC-FMO for sulfur assimilation, which is investigated in detail by solving the 2.6-Å resolution crystal structure of unliganded SfnG and the 1.75-Å resolution crystal structure of the SfnG ternary complex containing FMN and DMSO 2 . We find that SfnG adopts a (β/α) 8 barrel fold with a distinct quaternary configuration from other tetrameric class C TC-FMOs. To probe the unexpected tetramer arrangement, structural heterogeneity is assessed by chromatography and light scattering to confirm ligand binding correlates with a tetramer. Binding of FMN and DMSO 2 accompanies ordering of the active site, with DMSO 2 bound on thesi-face of the flavin. A previously unobserved protein backbone conformation is found within the oxygen-binding site on there-face of the flavin. Functional assays and the positioning of ligands with respect to the oxygen-binding site are consistent with use of an N5-(hydro)peroxyflavin pathway. Biochemical endpoint assays and docking studies reveal SfnG breaks the C–S bond of a range of dialkylsulfones.

Science & Technology - Other Topics↗
DOE OSTI2023

Photoaging of phenolic secondary organic aerosol in the aqueous phase: evolution of chemical and optical properties and effects of oxidants

Abstract. While gas-phase reactions are well established to have significant impacts on the mass concentration, chemical composition, and optical properties of secondary organic aerosol (SOA), the aqueous-phase aging of SOA remains poorly understood. In this study, we performed a series of long-duration photochemical aging experiments to investigate the evolution of the composition and light absorption of the aqueous SOA (aqSOA) from guaiacyl acetone (GA), a semivolatile phenolic carbonyl that is common in biomass burning smoke. The aqSOA was produced from reactions of GA with hydroxyl radical (•OH-aqSOA) or a triplet excited state of organic carbon (3C∗-aqSOA) and was then photoaged in water under conditions that simulate sunlight exposure in northern California for up to 48 h. The effects of increasing aqueous-phase •OH or 3C∗ concentration on the photoaging of the aqSOA were also studied. High-resolution aerosol mass spectrometry (HR-AMS) and UV–Vis spectroscopy were utilized to characterize the composition and the light absorptivity of the aqSOA and to track their changes during aging. Compared to •OH-aqSOA, the 3C∗-aqSOA is produced more rapidly and shows less oxidation, a greater abundance of oligomers, and higher light absorption. Prolonged photoaging promotes fragmentation and the formation of more volatile and less light-absorbing products. More than half of the initial aqSOA mass is lost, and substantial photobleaching occurs after 10.5 h of prolonged aging under simulated sunlight illumination for 3C∗-aqSOA and 48 h for •OH-aqSOA. By performing positive matrix factorization (PMF) analysis of the combined HR-AMS and UV–Vis spectral data, we resolved three generations of aqSOA with distinctly different chemical and optical properties. The first-generation aqSOA shows significant oligomer formation and enhanced light absorption at 340–400 nm. The second-generation aqSOA is enriched in functionalized GA species and has the highest mass absorption coefficients in 300–500 nm, while the third-generation aqSOA contains more fragmented products and is the least light absorbing. These results suggest that intermediately aged phenolic aqSOA is more light absorbing than other generations, and that the light absorptivity of phenolic aqSOA results from a competition between brown carbon (BrC) formation and photobleaching, which is dependent on aging time. Although photoaging generally increases the oxidation of aqSOA, a slightly decreased O/C of the •OH-aqSOA is observed after 48 h of prolonged photoaging with additional •OH exposure. This is likely due to greater fragmentation and evaporation of highly oxidized compounds. Increased oxidant concentration accelerates the transformation of aqSOA and promotes the decay of BrC chromophores, leading to faster mass reduction and photobleaching. In addition, compared with •OH, photoaging by 3C∗ produces more low-volatility functionalized products, which counterbalances part of the aqSOA mass loss due to fragmentation and evaporation.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2021

Field validation of an actuated convergent-beam acoustic Doppler profiler for high resolution flow mapping

Abstract Energetic river and tidal flow environments feature complex hydrodynamic conditions. Conventional acoustic Doppler profiling instrumentation typically requires assumptions of flow homogeneity over the spatial scales of the divergent beam separation. This removes the ability to measure spatio-temporal variability within the flow. However, velocity variability within these spatial scales is often important in the design of structures and devices exposed to such flow, informing dynamic and peak hydrodynamic load predictions. The research presented outlines the development and testing of a flow measurement instrument consisting of multiple spatially-separated single beam acoustic Doppler profilers converging on a remote focal point, the location of which can be programmatically adjusted through actuation. This increases the spatial resolution at which remote field measurements can be made in energetic flow environments. Field testing of the instrument was conducted in a tidal channel at Sequim Bay Inlet, WA, USA. Results are compared with independent reference measurements made by a co-located, motion-corrected acoustic Doppler velocimeter. This comparison, across tidal velocities of 0.4–0.7 m s −1 , showed a mean velocity error of 0.5%–13.2% across nine sample locations within a 3.00 m × 2.25 m plane. To the authors’ knowledge, this is the first publication of flow velocity results from non-intrusive acoustic measurements at an off-axis, focal point location that features 3D positional control.

13 HYDRO ENERGY↗
DOE OSTI2021

Negative Index Metamaterial Lens for Subwavelength Microwave Detection

Metamaterials are engineered periodic structures designed to have unique properties not encountered in naturally occurring materials. One such unusual property of metamaterials is the ability to exhibit negative refractive index over a prescribed range of frequencies. A lens made of negative refractive index metamaterials can achieve resolution beyond the diffraction limit. This paper presents the design of a metamaterial lens and its use in far-field microwave imaging for subwavelength defect detection in nondestructive evaluation (NDE). Theoretical formulation and numerical studies of the metamaterial lens design are presented followed by experimental demonstration and characterization of metamaterial behavior. Finally, a microwave homodyne receiver-based system is used in conjunction with the metamaterial lens to develop a far-field microwave NDE sensor system. A subwavelength focal spot of size 0.82λ was obtained. The system is shown to be sensitive to a defect of size 0.17λ × 0.06λ in a Teflon sample. Consecutive positions of the defect with a separation of 0.23λ was resolvable using the proposed system.

47 OTHER INSTRUMENTATION↗
DOE OSTI2023

Mapping Glacier Basal Sliding Applying Machine Learning

During the RESOLVE project (“High-resolution imaging in subsurface geophysics: development of a multi-instrument platform for interdisciplinary research”), continuous surface displacement and seismic array observations were obtained on Glacier d’Argentière in the French Alps for 35 days in May 2018. The data set is used to perform a detailed study of targeted processes within the highly dynamic cryospheric environment. In particular, the physical processes controlling glacial basal motion are poorly understood and remain challenging to observe directly. Especially in the Alpine region for temperate based glaciers where the ice rapidly responds to changing climatic conditions and thus, processes are strongly intermittent in time and heterogeneous in space. Spatially dense seismic and Global Positioning System (GPS) measurements are analyzed applying machine learning to gain insight into the processes controlling glacial motions of Glacier d’Argentière. Using multiple bandpass-filtered copies of the continuous seismic waveforms, we compute energy-based features, develop a matched field beamforming catalog and include meteorological observations. Features describing the data are analyzed with a gradient boosting decision tree model to directly estimate the GPS displacements from the seismic noise. We posit that features of the seismic noise provide direct access to the dominant parameters that drive displacement on the highly variable and unsteady surface of the glacier. The machine learning model infers daily fluctuations and longer term trends. The results show on-ice displacement rates are strongly modulated by activity at the base of the glacier. The techniques presented provide a new approach to study glacial basal sliding and discover its full complexity.

58 GEOSCIENCES↗
DOE OSTI2022

Inferring small-sample-reactivity worth from oscillation experiment with auto-corrected local flux

To estimate reactivity changes as a function of time from the signal of detectors count rates, one usually uses point kinetic equations. However, when detectors are located inside the core, it is often necessary to compute a correction factor to account for the flux-shape deformation (i.e. the change of detector efficiency that may have been induced by neutron absorbers movements). Various simulation methods have been developed depending on transients observed. They range from the resolution of static equations up to full-time-dependent neutron transport in 3D. However, those methods require high computational-cost calculations of local reaction rates that rely on nuclear data evaluations. Therefore, a 'measured' reactivity is never determined through pure measurements. Taking advantage of the known oscillation movement of a small sample at the center of the MINERVE reactor, the innovative algorithm presented in this paper derives the correction factor needed to get no time drift on reactivity steps. Derived correction factors are in good agreement with those obtained independently with TRIPOLI-4 through sensitivity analysis. Low sensitivity to the sample composition and moderate sensitivity to the detectors position reinforce the reliability of those results. This application paves the way to almost pure nuclear data reactivity measurements. (authors)

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗
DOE OSTI2021

Effect of photon counting shot noise on total internal reflection microscopy

Total internal reflection microscopy (TIRM) measures changes in the distance between a colloidal particle and a transparent substrate by measuring the scattering intensity of the particle illuminated by an evanescent wave. From the distribution of the recorded separation distances, the height-dependent effective potential φ(z) between the colloidal particle and the substrate can be measured. In this work, we show that spatial resolution with which TIRM can measure φ(z) is limited by the photon counting statistics of the scattered laser light. Here, we develop a model to evaluate the effect of photon counting statistics on different potential profiles using Brownian dynamics simulations and experiments. Our results show that the effect of photon counting statistics depends on spatial gradients ∂φ/∂z of the potential, with the result that sharp features tend to be significantly blurred. We further establish the critical role of photon counting statistics and the intensity integration time τ in TIRM measurements, which is a trade-off between narrowing the width of the photon counting distribution and capturing the instantaneous position of the probe particle.

47 OTHER INSTRUMENTATION↗
DOE OSTI2024

The crystal structure of Grindelia robusta 7,13-copalyl diphosphate synthase reveals active site features controlling catalytic specificity

Diterpenoid natural products serve critical functions in plant development and ecological adaptation and many diterpenoids have economic value as bioproducts. The family of class II diterpene synthases catalyzes the committed reactions in diterpenoid biosynthesis, converting a common geranylgeranyl diphosphate precursor into different bicyclic prenyl diphosphate scaffolds. Enzymatic rearrangement and modification of these precursors generate the diversity of bioactive diterpenoids. We report the crystal structure of Grindelia robusta 7,13-copalyl diphosphate synthase, GrTPS2, at 2.1 Å of resolution. GrTPS2 catalyzes the committed reaction in the biosynthesis of grindelic acid, which represents the signature metabolite in species of gumweed (Grindelia spp., Asteraceae). Grindelic acid has been explored as a potential source for drug leads and biofuel production. The GrTPS2 crystal structure adopts the conserved three-domain fold of class II diterpene synthases featuring a functional active site in the γβ-domain and a vestigial α-domain. Substrate docking into the active site of the GrTPS2 apo protein structure predicted catalytic amino acids. Biochemical characterization of protein variants identified residues with impact on enzyme activity and catalytic specificity. Specifically, mutagenesis of Y457 provided mechanistic insight into the position-specific deprotonation of the intermediary carbocation to form the characteristic 7,13 double bond of 7,13-copalyl diphosphate.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Insights into the molecular mechanism of translation inhibition by the ribosome-targeting antibiotic thermorubin

Thermorubin (THR) is an aromatic anthracenopyranone antibiotic active against both Gram-positive and Gram-negative bacteria. It is known to bind to the 70S ribosome at the intersubunit bridge B2a and was thought to inhibit factor-dependent initiation of translation and obstruct the accommodation of tRNAs into the A site. Here, we show that thermorubin causes ribosomes to stall in vivo and in vitro at internal and termination codons, thereby allowing the ribosome to initiate protein synthesis and translate at least a few codons before stalling. Our biochemical data show that THR affects multiple steps of translation elongation with a significant impact on the binding stability of the tRNA in the A site, explaining premature cessation of translation. Our high-resolution crystal and cryo-EM structures of the 70S-THR complex show that THR can co-exist with P- and A-site tRNAs, explaining how ribosomes can elongate in the presence of the drug. Remarkable is the ability of THR to arrest ribosomes at the stop codons. Our data suggest that by causing structural re-arrangements in the decoding center, THR interferes with the accommodation of tRNAs or release factors into the ribosomal A site.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2025

Probing the local structure of Bi 2 O 3 chemical derivatives: the neglected cation sublattice

High-resolution synchrotron X-ray diffraction data confirm the stabilization of the average structure at ambient temperatures as a defect fluorite structure in ternary and quaternary oxides of Bi 2 O 3 , where some Bi cations are replaced with Dy 3+ and/or Er 3+ , Nb 5+ and W 6+ . Rietveld refinement of the diffraction data indicates that when the larger cation Er 3+ (0.89 Å) is replaced with smaller cations W 6+ (0.42 Å) and/or Nb 5+ (0.48 Å), the unit-cell parameter a, based on the relative ionic radii of the substituents, counterintuitively increases. Total scattering data show that the identity of the cation substituent is important in determining the positions of some Bi cations in the defect fluorite structure. Er 3+ and Dy 3+ cations induce monoclinic-like distortions that extend only locally in the Bi 3+ sublattice. X-ray absorption spectroscopy provides evidence that some Dy cations, in the δ phases, prefer to keep a similar local environment to that in the parent Dy 2 O 3 . W cations are found to be predominantly tetrahedrally coordinated in the δ phases explored in this work.

36 MATERIALS SCIENCE↗
DOE OSTI2021

New Fracture Diagnostic Tool for Unconventionals: High-Resolution Distributed Strain Sensing via Rayleigh Frequency Shift during Production in Hydraulic Fracture Test 2

Fiber Optic monitoring in unconventional reservoirs has proven to be an invaluable diagnostic tool for assessing both near-wellbore stimulation effectiveness and to help describe the far-field frac geometries created by hydraulic fracture stimulation. Unfortunately, gaining any detailed qualitative and quantitative understanding of the near-wellbore frac geometry or cluster/stage productivity during production via Fiber Optic (FO) has proven to be more difficult, particularly in wells producing liquids. A new FO diagnostic method, Distributed Strain Sensing based on Rayleigh Frequency Shift (DSS-RFS), first demonstrated for oil and gas applications in the Hydraulic Test Site 2 (HFTS2) provides new insights about the characteristics of near-wellbore-region (NWR) during production. DSS-RFS is different from other FO strain measurements because it relies on accurate measurement of frequency shifts of Rayleigh backscattered spectrum obtained by scanning the fiber with a coherent optical time-domain reflectometer with a range of laser frequencies using a tunable-wavelength laser system. Changes in strain are measured with an extremely high spatial resolution of 20 cm and with high signal-to-noise ratios over long distances. In HFTS2, strain changes for the entire wellbore have been measured twice during scheduled shut-in and reopening operations (February 2020 and September 2020). After removing temperature effects, consistent strain changes have been observed at the location of most perforation clusters. These are caused by near wellbore fracture aperture changes due to pressure increases during shut-in within the near-wellbore fracture network. The strain-change patterns from the DSS-RFS during shut-in correlate very well with the location of clusters and allow for the definition of extending intervals with positive strain signals at each cluster and slightly compressing intervals with negative strain signals between the clusters and in the non stimulated intervals. The locations of the measured positive strain peaks also show good correspondence to DAS acoustic intensity measurements acquired during the stimulation. The geometry and magnitude of the strain changes differ significantly between the two tested completion designs in the same well. During shut in and reopening each cluster exhibit its own strain-change / pressure path. In addition, the September 2020 dataset also revealed the existence of small but measurable strain changes as consequence of pressure decline during production. These strain changes also correlate well with the presence of producing clusters, but the strain-rate signals are opposite to that obtained during shut-in and reopening operations. Although Downloaded from http://onepetro.org/URTECONF/proceedings-pdf/21URTC/2-21URTC/D021S031R002/2477551/urtec-2021-5408-ms.pdf/1 by Carol Worster on 28 February 2022 URTeC 5408 2 we are still in the early stages of exploring the potential of this novel FO technique, we believe that the highly detailed information contained in the measurement of strain changes using DSS-RFS during production can significantly improve our understanding of near-wellbore hydraulic fracture characteristics and the relationships between stimulation and production from unconventional oil and gas wells.

04 OIL SHALES AND TAR SANDS↗
DOE OSTI2024

Chemical properties and single-particle mixing state of soot aerosol in Houston during the TRACER campaign

Abstract. A high-resolution soot particle aerosol mass spectrometer (SP-AMS) was used to selectively measure refractory black carbon (rBC) and its associated coating material using both the ensemble size-resolved mass spectral mode and the event trigger single particle (ETSP) mode in Houston, Texas, in summer 2022. This study was conducted as part of the Department of Energy Atmospheric Radiation Measurement (ARM) program's TRacking Aerosol Convection interactions ExpeRiment (TRACER) field campaign. The study revealed an average (±1σ) rBC concentration of 103 ± 176 ng m−3. Additionally, the coatings on the BC particles were primarily composed of organics (59 %; 219 ± 260 ng m−3) and sulfate (26 %; 94 ± 55 ng m−3). Positive matrix factorization (PMF) analysis of the ensemble mass spectra of BC-containing particles resolved four distinct types of soot aerosol, including an oxidized organic aerosol (OOABC,PMF) factor associated with processed primary organic aerosol, an inorganic sulfate factor (SO4,BC,PMF), an oxidized rBC factor (O-BCPMF), and a mixed mineral dust–biomass burning aerosol factor with significant contribution from potassium (K-BBBC,PMF). Additionally, K-means clustering analysis of the single-particle mass spectra identified eight different clusters, including soot particles enriched in hydrocarbon-like organic aerosol (HOABC,ETSP), sulfate (SO4,BC,ETSP), two types of rBC, OOA (OOABC,ETSP), chloride (ClBC,ETSP), and nitrate (NO3,BC,ETSP). The single-particle measurements demonstrate substantial variation in BC coating thickness with coating-to-rBC mass ratios ranging from 0.1 to 100. The mixing state index (χ), which denotes the degree of homogeneity of the soot aerosol, varied from 4 % to 94 % with a median of 40 %, indicating that the aerosol population lies in between internal and external mixing but has large temporal and source type variability. In addition, a significant fraction of BC-containing particles, a majority enriched with oxidized organics and sulfate, exhibit sufficiently high κ values and diameters conducive to activation as cloud nuclei under atmospherically relevant supersaturation conditions. This finding bears significance in comprehending the aging processes of rBC-containing particles and their activation into cloud droplets. Our analysis highlights the complex nature of soot aerosol and underscores the need to comprehend its variability across different environments for accurate assessment of climate change.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2024

Present understanding of ignition and gain using indirect-drive inertial confinement fusion target designs on the U.S. National Ignition Facility

For many decades, the running joke in fusion research has been that 'fusion' is thirty years away and always will be. Yet, these past few years we find ourselves in a position where we can now talk about the milestones of burning plasmas, fusion ignition, and target energy gain greater than unity (scientific breakeven) in the past tense. Fusion is no longer a joke! Yet getting to fusion ignition, the tipping-point of thermonuclear instability resulting in an explosive increase in ion thermal temperature and fusion reaction-rate, and scientific breakeven (target gain, $G_{target} =$ fusion yield/deposited laser energy >1, in the laser-driven inertial confinement fusion context) has not been easy. Here, in this publication, we discuss our present understanding of the physics and technological challenges surrounding ignition and Gain as well as highlight some outstanding problems that still need resolution.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2020

Characterization of Partial Charge Collection Induced by Neutron Damage in High-Purity Germanium Detectors

This paper investigates the correlation of damage induced by neutron interactions and degradation in the spectra of HPGe detectors. As neutrons kinetically interact with germanium crystals, they create interstitial and vacancy defects within the lattice. These defects then interfere with the charge migration of electron-hole pairs and reduce resolution in the observed energy spectrum. The partial charge collection produces observable spectral changes by increasing the peak width and reducing resolution (full width half maximum). A detailed characterization using various check sources was performed before and after iterations of neutron exposure in order to observe the effects of the neutron damage. An additional set of measurements was performed along with characterizations to show the detector’s response at discrete locations on the HPGe crystal. This was done to observe how the spectrum changes when the gamma rays are isolated to regions of various thicknesses of germanium. In order to impart damage, the detector was placed inside a californium shuffler with the face of the detector against the guide tube for the 252 Cf source. For irradiation of the HPGe, the source was then positioned in front of the face of the detector using the stepper motor of the shuffler. The neutron exposure time intervals were recorded and increased based on the initial damage observed. An MCNP simulation was performed to estimate the amount of interactions that occurred in the germanium crystal to ensure enough damage had occurred. Studying the effects that neutron damage imparts on a bullet-type HPGe detector can help provide necessary data to estimate total neutron exposure limits, reduce the likelihood of decisions made on suspect data, and aid in diagnostics of a damaged detector.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Oil-Pressure Based Apparatus for In-Situ High-Energy Synchrotron X-Ray Diffraction Studies During Biaxial Deformation

Background: Understanding biaxial loading response at the microstructural level is crucial in helping better design sheet manufacturing processes and calibrate/validate material deformation models. Objective: The objective of this work was to develop a low-cost testing apparatus to probe, with sufficient spatial resolution, the micro-mechanical response of a sheet material in-situ under biaxial loading conditions. Methods: The testing apparatus fabricated as a part of this study operates in a similar fashion to a standard bulge test and uses oil pressure to generate biaxial loading conditions. This biaxial testing apparatus was operated within a synchrotron beamline to characterize the mechanical response of a flash-processed steel sheet using in-situ high-energy X-ray diffraction (XRD) measurements. Further, the GSAS-II package was utilized to develop a workflow for the analysis of the large volume of diffraction data acquired. The workflow was then used to extract the peak position, width, and integrated intensity of the XRD peaks corresponding to the major body-centered cubic phase. Results: The equi-biaxial nature of the loading in the measured area was independently corroborated using experimental (XRD) and simulation (finite element analysis) methods. Furthermore, we discuss the evolution of elastic strain in the major body-centered cubic phase as a function of applied oil pressure and location on the steel sheet. Conclusions: A key advantage of the biaxial apparatus fabricated in this synchrotron study is demonstrated using the results obtained for the flash-processed steel sheet – i.e., mapping the lattice plane-dependent response to biaxial loading for a relatively large sample area in a spatially resolved manner.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Application of sulfur SAD to small crystals with a large asymmetric unit and anomalous substructure

The application of sulfur single-wavelength anomalous dispersion (S-SAD) to determine the crystal structures of macromolecules can be challenging if the asymmetric unit is large, the crystals are small, the size of the anomalously scattering sulfur structure is large and the resolution at which the anomalous signals can be accurately measured is modest. Here, as a study of such a case, approaches to the SAD phasing of orthorhombic Ric-8A crystals are described. The structure of Ric-8A was published with only a brief description of the phasing process [Zeng et al. (2019), Structure , 27 , 1137–1141]. Here, alternative approaches to determining the 40-atom sulfur substructure of the 103 kDa Ric-8A dimer that composes the asymmetric unit are explored. At the data-collection wavelength of 1.77 Å measured at the Frontier micro-focusing Macromolecular Crystallography (FMX) beamline at National Synchrotron Light Source II, the sulfur anomalous signal strength, |Δ ano |/σΔ ano ( d ′′/sig), approaches 1.4 at 3.4 Å resolution. The highly redundant, 11 000 000-reflection data set measured from 18 crystals was segmented into isomorphous clusters using BLEND in the CCP 4 program suite. Data sets within clusters or sets of clusters were scaled and merged using AIMLESS from CCP 4 or, alternatively, the phenix.scale_and_merge tool from the Phenix suite. The latter proved to be the more effective in extracting anomalous signals. The HySS tool in Phenix , SHELXC / D and PRASA as implemented in the CRANK 2 program suite were each employed to determine the sulfur substructure. All of these approaches were effective, although HySS , as a component of the phenix.autosol tool, required data from all crystals to find the positions of the sulfur atoms. Critical contributors in this case study to successful phase determination by SAD included (i) the high-flux FMX beamline, featuring helical-mode data collection and a helium-filled beam path, (ii) as recognized by many authors, a very highly redundant, multiple-crystal data set and (iii) the inclusion within that data set of data from crystals that were scanned over large ω ranges, yielding highly isomorphous and highly redundant intensity measurements.

59 BASIC BIOLOGICAL SCIENCES↗