Whither Mn Oxidation in Mn-Rich Alkali-Excess Cathodes?
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99 GENERAL AND MISCELLANEOUS↗
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Results for “Diffraction systems”
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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Physical and Electrochemical Characterization of Aluminum Electrodes during Electrocoagulation
Electrocoagulation (EC) of synthetic groundwater was conducted using a sacrificial aluminum electrode in a flow-through EC reactor with short retention times (<1 min) under varying hydrodynamic and electrochemical conditions. The treated water was allowed to settle for 24 h and achieved silicate removal of up to 50 ± 4%, and hardness removal of 11 ± 1%. Physical, chemical, and electrochemical characterization was performed to explore changes in electrode surface morphology and composition. Electrochemical impedance spectroscopy (EIS) showed that chemical reactions at the electrode/water interface are sensitive to changes in the immediate chemical environment. We demonstrate that the most energy-intensive step in EC is aluminum dissolution at the anode, which remained fairly constant due to the continuous renewal of the anode’s surface, a result of aluminum dissolution. At the cathode, a structural change in the oxide layer, from γ-Al 2 O 3 to gibbsite, was detected by grazing-incidence X-ray diffraction, which decreased the resistance to charge transfer at the cathode surface, resulting in decreased electrode resistance. The high flow rate in the system minimized the accumulation of aluminum hydroxide solids and aluminum ions at the electrode/water interface, which minimized the formation of thick scalants and amorphous Al(OH) 3 on the cathode and anode, respectively. In conclusion, it was further demonstrated by EIS that under these conditions the resistance to charge transfer was constant throughout the duration of the experiment.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Direct visualization of polaron formation in the thermoelectric SnSe
SnSe is a layered material that currently holds the record for bulk thermoelectric efficiency. The primary determinant of this high efficiency is thought to be the anomalously low thermal conductivity resulting from strong anharmonic coupling within the phonon system. Here we show that the nature of the carrier system in SnSe is also determined by strong coupling to phonons by directly visualizing polaron formation in the material. We employ ultrafast electron diffraction and diffuse scattering to track the response of phonons in both momentum and time to the photodoping of free carriers across the bandgap, observing the bimodal and anisotropic lattice distortions that drive carrier localization. Relatively large (18.7 Å), quasi-one-dimensional (1D) polarons are formed on the 300-fs timescale with smaller (4.2 Å) 3D polarons taking an order of magnitude longer (4 ps) to form. This difference appears to be a consequence of the profoundly anisotropic electron–phonon coupling in SnSe, with strong Fröhlich coupling only to zone-center polar optical phonons. These results demonstrate a high density of polarons in SnSe at optimal doping levels. Strong electron-phonon coupling is critical to the thermoelectric performance of this benchmark material and, potentially, high performance thermoelectrics more generally.
36 MATERIALS SCIENCE↗
Structural properties of PbTe quantum dots revealed by high-energy x-ray diffraction
High-energy x-ray diffraction (HE-XRD) experiments combined with an analysis based on atomic-pair-distribution functions can be an effective tool for probing low-dimensional materials. Here, we show how such an analysis can be used to gain insight into structural properties of PbTe nanoparticles (NPs). Here we interpret our HE-XRD data using an orthorhombic Pnma phase of PbTe, which is an orthorhombic distortion of the rocksalt phase. Although local crystal geometry can vary substantially with particle size at scales below 10 nm, and for very small NPs the particle size itself influences x-ray diffraction patterns, our study shows that HE-XRD can provide a unique nano-characterization tool for unraveling structural properties of nanoscale systems.
71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
Characterization of groove density variation of VLS gratings with ALS XROL LTP-II in different operation modes
The long trace profiler, LTP-II, available at the Advanced Light Source (ALS) X-ray Optics Laboratory (XROL), was recently upgraded by replacing a multimode diode laser light source with a single-mode, wavelength-stabilized, fibercoupled diode laser system. The upgrade enables us to reliably characterize the lateral variation of groove density of variable-line-spacing (VLS) x-ray diffraction gratings. Here, we discuss the LTP-II performance with an example of measurements with a VLS grating with the groove density at the grating center of 300 lines/mm. For the measurements, we use the LTP-II in two different operation arrangements, the single Gaussian beam and the pencil beam interferometer arrangements. For each operation arrangement, we apply two data processing algorithms: with calculating the centroid position and with determining the position of a characteristic features of the detected beam intensity distributions. Additionally, we discuss the observed strong correlation between the LTP-II modes of operation and the resulted (extracted) groove density variations. We also speculate on possible origin of the correlation.
42 ENGINEERING↗
Serial femtosecond and serial synchrotron crystallography can yield data of equivalent quality: A systematic comparison
For the two proteins myoglobin and fluoroacetate dehalogenase, we present a systematic comparison of crystallographic diffraction data collected by serial femtosecond (SFX) and serial synchrotron crystallography (SSX). To maximize comparability, we used the same batch of micron-sized crystals, the same sample delivery device, and the same data analysis software. Overall figures of merit indicate that the data of both radiation sources are of equivalent quality. For both proteins, reasonable data statistics can be obtained with approximately 5000 room-temperature diffraction images irrespective of the radiation source. The direct comparability of SSX and SFX data indicates that the quality of diffraction data obtained from these samples is linked to the properties of the crystals rather than to the radiation source. Therefore, for other systems with similar properties, time-resolved experiments can be conducted at the radiation source that best matches the desired time resolution.
59 BASIC BIOLOGICAL SCIENCES↗
Microwave-Assisted Production of Polycarbonate Diols using Carbon Dioxide
Carbon dioxide (CO2) is a cheap and readily available resource that can be converted to value-added chemicals including fuels, polymers, and other products. One lucrative option is polycarbonate diols, which are the precursor to polyurethanes that find wide applications in automotive and aerospace industries. The traditional process for the synthesis of polycarbonate diols involves using hazardous phosgene and alcohols in a strongly basic medium that generates significant amounts of salt. Alternately, CO2 can be reacted with alkanediols over CeO2 catalysts to produce polycarbonate diols. For the current work, a microwave-assisted atmospheric flow system was investigated for converting CO2 into polycarbonate diols and was compared against a thermal system. Various parameters such as type and ratio of solvents, and the addition of dehydrating agents for the microwave system was tested. The different CeO2 catalysts used were characterized using Brunauer–Emmett–Teller (BET) surface area analysis, Raman spectroscopy, X-ray diffraction, and temperature programmed desorption (NH3-TPD and CO2-TPD).
CO2 utilization↗
SCExAO/MEC and CHARIS Discovery of a Low-mass, 6 au Separation Companion to HIP 109427 Using Stochastic Speckle Discrimination and High-contrast Spectroscopy
We report the direct imaging discovery of a low-mass companion to the nearby accelerating A star, HIP 109427, with the Subaru Coronagraphic Extreme Adaptive Optics (SCExAO) instrument coupled with the Microwave Kinetic Inductance Detector Exoplanet Camera (MEC) and CHARIS integral field spectrograph. CHARIS data reduced with reference star point spread function (PSF) subtraction yield 1.1–2.4 μm spectra. MEC reveals the companion in Y and J band at a comparable signal-to-noise ratio using stochastic speckle discrimination, with no PSF subtraction techniques. Combined with complementary follow-up L {sub p} photometry from Keck/NIRC2, the SCExAO data favors a spectral type, effective temperature, and luminosity of M4–M5.5, 3000–3200 K, and log{sub 10}(L/L{sub ⊙})=−2.28{sub −0.04}{sup +0.04}, respectively. Relative astrometry of HIP 109427 B from SCExAO/CHARIS and Keck/NIRC2, and complementary Gaia–Hipparcos absolute astrometry of the primary favor a semimajor axis of 6.55{sup +3.0} {sub −0.48} au, an eccentricity of 0.54{sub −0.15}{sup +0.28}, an inclination of 66.7{sub −14}{sup +8.5} degrees, and a dynamical mass of 0.280{sub −0.059}{sup +0.18} M {sub ⊙}. This work shows the potential for extreme AO systems to utilize speckle statistics in addition to widely used postprocessing methods to directly image faint companions to nearby stars near the telescope diffraction limit.
46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
Thermodynamic investigation of the NaCl-KCl salt system from 25 to 950 °C
NaCl-KCl molten salt system has been proposed as a primary component of several promising heat transfer eutectics and fuel host for Generation IV molten salt reactors (MSR). In this work, several key thermodynamic parameters, including high temperature enthalpies, isobaric heat capacities (C p ) and molar enthalpies of mixing (ΔH mix ), of the NaCl -KCl system (NaCl, 75mol% NaCl – 25mol% KCl, 51mol% NaCl – 49mol% KCl, 25mol% NaCl – 75mol% KCl, and KCl) were measured by high temperature drop calorimetry (HTDC) utilizing laser sealed nickel and aluminum crucibles. Salts were checked for phase purity by X-ray diffraction (XRD), and water content by Karl Fischer coulometric titrimetry and thermogravimetric analysis (TGA). Thermo-mechanical analysis (TMA) utilizing custom-built boron nitride (BN) crucibles was employed to determine temperatures of phase transitions (solid $\rightarrow$ liquid) for the salts and plotted against the pseudobinary phase diagram for the NaCl-KCl system. Small deviations (3-10 %) were found among C p values obtained from HTDC, differential scanning calorimetry (DSC), and NIST, comparable to the average uncertainty based on two standard deviations of measured data that are ~6% for DSC and ~3% for HTDC. Additionally, the measured enthalpies and C p values of mixed NaCl-KCl salts (e.g., 51mol% NaCl – 49mol% KCl eutectic) were shown to behave as statistical mixtures of its pure endmembers, consistent with ΔH mix = ~ 0 kJ/mol at 800 °C, and a regular interaction parameter of Ω = 1.20 ± 0.76 kJ/mol. In conclusion, this study represents a step towards improved accuracy and precision in determinations of thermodynamic parameters of molten salts by using DSC, TMA, and HTDC, in completion of the Molten Salt Thermal Properties Database (MSTDB).
11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
Ta–Zr carbides: Synthesis advances via carbothermal reduction and defect evolution observed through transmission electron microscopy ion irradiation
The thermodynamic stability of six distinct compositions within the Zr—Ta—C ternary system is investigated in this study, marking the first report of their synthesis through carbothermic reduction in vacuum. A prolonged annealing process at 2200°C enabled high densification and phase equilibrium. Detailed phase identification and microstructural characterization through microscopy and X-ray diffraction techniques revealed clear compositional trends and stable phase formations. Two compositions ((Ta 0.2 Zr 0.8 )C 0.6 and (Ta 0.5 Zr 0.5 )C 1 ) were selected for ion irradiation experiments using 200 keV Kr + at 600°C—representing the first-ever irradiation study on the Zr—Ta—C system. The findings indicated defect accumulation and nanoscale cavity formation without any evidence of amorphization, highlighting the system's structural stability under irradiation. Together, the synthesis and irradiation results provide a basis for further investigation of the system and suggest its relevance for applications under extreme environments.
36 MATERIALS SCIENCE↗
10 Boron-film-based gas detectors at ESS
The development of detectors for the European Spallation Source is an important parallel element to the effort put into the design and construction of the neutron source and instruments. The 10Boron-film-based detector developments that started over a decade ago as basic detector concepts have now reached technical maturity after intense prototyping work and numerous testing campaigns. Several of the ESS beamlines that will soon enter the commissioning phase started welcoming the detector systems built with the 10 B-film converter technology. The real-size demonstrators evolved in the last 2–3 years into a diverse suite of gas proportional counters for use in diffraction, reflectometry and small-angle scattering studies in spite of the operational complexity posed by the requirements for large-area coverage, low material budget and robustness for operation in the high-flux and high-radiation environment of ESS. The detectors are now being shipped to ESS or undergoing the last performance and calibration tests before being handed over to the instrument teams for installation in the host beamlines. A common feature of these detector systems is the very large number of readout channels that they are instrumented with in order to fulfill the demanding requirements for sensitivity, spatial resolution and count-rate capability. Across all of the detector types that will operate at ESS, the integration, testing and commissioning of the read-out technologies and software tools for data reduction, calibration and analysis are the focus of the detector and integration teams. These will yield a wealth of knowledge about their operation as well as initial results on the in-situ performance, a very important asset to ensure rapid commissioning of the detectors when neutrons from the ESS source become available. In this paper we will give an overview of the 10 B-film-based detector technologies included in the ESS detector suite that are currently facing the transition from the production phase to installation and integration with the other beamline components, which comes with its own specific challenges of both organizational and technical nature.
47 OTHER INSTRUMENTATION↗
Exotic Long-Range Surface Reconstruction on La 0.7 Sr 0.3 MnO 3 Thin Films
Due to an extremely diverse phase space, La 1–x Sr x MnO 3 , as with other manganites, offers a wide range of tunability and applications including colossal magnetoresistance and use as spin-polarized electrodes. Here, we study an unprecedented, exotic surface reconstruction (6 × 6) in La 1–x Sr x MnO 3 (x = 0.3) observed via low-energy electron diffraction (LEED). Scanning tunneling microscopy (STM) shows the surface is relatively flat, with unit-cell step heights, and X-ray photoelectron spectroscopy (XPS) reveals a strong degree of Sr segregation at the surface. By combining electron diffraction and first-principles computations, we propose that the long-range surface reconstruction consists of a Sr-segregated surface with La (6 × 6) ordering. This study expands our understanding of manganite systems and underscores their ability to form interesting surface reconstructions, driven largely by cation segregation that can potentially be controlled for tuning surface ordering.
36 MATERIALS SCIENCE↗
The intrinsic mechanical properties of hydromagnesite, Mg 5 (CO 3 ) 4 (OH) 2 ·4H 2 O, a key phase of reactive MgO carbonate cement
To potentially enable CO 2 sequestration, reactive MgO carbonate cement is emerging as an alternative binder to Portland cement. Understanding the mechanical properties of its binding phase is critical for understanding the strength development and performing materials design for reactive MgO cement systems; however, the intrinsic mechanical properties of hydromagnesite (Mg 5 (CO 3 ) 4 (OH) 2 ·4H 2 O), a key binding phase, remain unexplored. Here the present study utilized synchrotron-based high-pressure X-ray diffraction to determine the unit cell-scale, intrinsic mechanical properties of hydromagnesite for the first time. Up to hydrostatic loading of 7.7 GPa, the bulk modulus of hydromagnesite was determined as 59 GPa or 71 GPa fitted using the second-order or third-order Birch-Murnaghan equation of state, which we contextualize with binding phases in various cement systems. The experiment results are applicable in materials design of low-carbon concrete and valuable for the validation and calibration of atomistic models.
36 MATERIALS SCIENCE↗
Experimental X-ray Charge-Density Studies–A Suitable Probe for Superconductivity? A Case Study on MgB 2
Case studies of 1T-TiSe 2 and YBa 2 Cu 3 O 7-δ have demonstrated that X-ray diffraction (XRD) studies can be used to trace even subtle structural phase transitions which are inherently connected with the onset of superconductivity in these benchmark systems. However, the utility of XRD in the investigation of superconductors like MgB 2 lacking an additional symmetry-breaking structural phase transition is not immediately evident. Nevertheless, high-resolution powder XRD experiments on MgB 2 in combination with maximum entropy method analyses hinted at differences between the electron density distributions at room temperature and 15 K, that is, below the T c of approx. 39 K. The high-resolution single-crystal XRD experiments in combination with multipolar refinements presented here can reproduce these results but show that the observed temperature-dependent density changes are almost entirely due to a decrease of atomic displacement parameters as a natural consequence of a reduced thermal vibration amplitude with decreasing temperature. Our investigations also shed new light on the presence or absence of magnesium vacancies in MgB 2 samples–a defect type claimed to control the superconducting properties of the compound. Here, we propose that previous reports on the tendency of MgB 2 to form non-stoichiometric Mg 1–x B 2 phases (1 – x ~ 0.95) during high-temperature (HT) synthesis might result from the interpretation of XRD data of insufficient resolution and/or usage of inflexible refinement models. Indeed, advanced refinements based on an Extended Hansen–Coppens multipolar model and high-resolution X-ray data, which consider explicitly the contraction of core and valence shells of the magnesium cations, do not provide any significant evidence for the formation of non-stoichiometric Mg 1–x B 2 phases during HT synthesis.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Phase Transitions in Metal–Organic Frameworks Directly Monitored through In Situ Variable Temperature Liquid-Cell Transmission Electron Microscopy and In Situ X-ray Diffraction
Zr 6 -based metal–organic frameworks (MOFs) with tetratopic organic linkers have been extensively investigated owing to their versatile structural tunability. While diverse topologies and polymorphism in the resulting MOFs are often encountered with tetratopic linkers and Zr 6 nodes, reports on phase transitions within these systems are rare. Thus, we have a limited understanding of polymorph transformations, hindering the rational development of pure phase materials. In this study, a phase transition from a microporous MOF, scu-NU-906, to a mesoporous MOF, csq-NU-1008, was discovered and monitored through in situ variable temperature liquid-cell transmission electron microscopy (VT-LCTEM), high-resolution transmission electron microscopy (HRTEM), and in situ variable temperature powder X-ray diffraction (VT-PXRD). Furthermore, it was found that the microporous- to-mesoporous transformation in the presence of formic acid occurs via a concomitant dissolution–reprecipitation process.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Measurement of differential cross sections for single diffractive dissociation in root s=8 TeV pp collisions using the ATLAS ALFA spectrometer
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72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
Utah FORGE: Well 16A(78)-32 Core Analysis Results
This dataset features petrographic, X-Ray Diffraction (XRD), and Scanning Electron Microscopy Analyses of core samples from well 16A(78)-32, which serves as the injection well for the Utah FORGE Enhanced Geothermal System (EGS) project. In addition to an overview of the analysis, the following items have been included here: images of 21 entire thin sections in plane-polarized and cross-polarized light from 16 depths, scanning electron microscope back scatter electron photomosaic maps of 21 thin sections from 16 depths, bulk XRD data from 16 depths, clay-sized XRD patterns from 16 depths, an optical petrography report, and scanning electron microscopy and energy dispersive spectroscopy analyses of eight selected samples.
15 GEOTHERMAL ENERGY↗
Avoiding CO 2 Improves Thermal Stability at the Interface of Li 7 La 3 Zr 2 O 12 Electrolyte with Layered Oxide Cathodes
Abstract Solid‐state batteries promise higher energy densities and better safety than Li‐ion batteries with liquid electrolytes. However, the interface between solid electrolyte and cathode is unstable at the elevated temperatures that are needed while sintering to achieve good bonding between ceramic components. Here, the hypothesis is that, the gas environment, especially the presence of CO 2, is critical in determining the stability of the solid electrolyte–cathode interface. The effect of gas species on the interface is systematically probed, by a using Li 7 La 3 Zr 2 O 12 (LLZO) solid electrolyte with a thin film LiNi 0.6 Mn 0.2 Co 0.2 O 2 cathode as a model system to enable interface sensitivity. Detrimental phases formed at the interface and their onset conditions are identified by X‐ray absorption spectroscopy, X‐ray diffraction, and Gibbs free energy analysis. As a result, removing CO 2 and minimizing H 2 O(g) during sintering is necessary to obtain good contact at the LLZO|cathode interface without forming secondary phases. Sintering in O 2 is ideal, yielding excellent chemical stability and low interfacial resistance. Secondary phases also do not form in N 2, but oxygen loss occurs at elevated temperatures. The interfacial resistance obtained upon sintering in pure O 2 is comparable to the lowest values at LLZO interfaces with protective coatings, but here without the need for interface coatings.
25 ENERGY STORAGE↗