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At least 361 records · Page 20

Review—Fundamental Uranium Electrochemistry and Spectroscopy in Molten Salt Systems

Uranium is a key element used for nuclear energy production. Some advanced reactor designs, specifically molten salt reactors, will continue to use uranium as the fissile material for energy production. These new technologies require an intimate understanding of uranium chemistry during and after energy production. This review covers contemporary research on the coordination chemistry and behavior of uranium with the coolant and pyroprocessing salts as proposed for use in future reactor designs. Discussed topics include the nature of U redox reactions involving the reduction of U(III) to U metal and oxidation of U(III) to U(IV). These systems have been interrogated using cyclic voltammetry, chronopotentiometry, and optical and X-ray absorption spectroscopies. Insights obtained into the electrode potentials, the uranium species, and their diffusion coefficients in alkali halide melts from decades of research are summarized selectively. Further, perspectives are provided on the importance of unifying studies for comparison across multiple institutions. The application of synchrotron radiation research and multimodal approaches involving two (or more) probes, such as the widespread combination of UV–visible spectroscopy and electroanalysis known as spectroelectrochemistry, can provide new knowledge about the main process of uranium electrorefining—diffusion, as will be demonstrated in this review through the lack of comparable results.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

The massive survey. IV. The X-ray halos of the most massive early-type galaxies in the nearby universe

Studies of the physical properties of local elliptical galaxies are shedding new light on galaxy formation. Here we present the hot-gas properties of 33 early-type systems within the MASSIVE galaxy survey that have archival Chandra X-ray observations, and we use these data to derive X-ray luminosities (L{sub X,gas}) and plasma temperatures (T{sub gas}) for the diffuse gas components. We combine this with the ATLAS{sup 3D} survey to investigate the X-ray–optical properties of a statistically significant sample of early-type galaxies across a wide range of environments. When X-ray measurements are performed consistently in apertures set by the galaxy stellar content, we deduce that all early types (independent of galaxy mass, environment, and rotational support) follow a universal scaling law such that L{sub X,gas}∝T{sub gas}{sup ∼4.5}. We further demonstrate that the scatter in L{sub X,gas} around both K-band luminosity (L {sub K}) and the galaxy stellar velocity dispersion (σ{sub e}) is primarily driven by T{sub gas}, with no clear trends with halo mass, radio power, or angular momentum of the stars. It is not trivial to tie the gas origin directly to either stellar mass or galaxy potential. Indeed, our data require a steeper relation between L{sub X,gas},L{sub K}, and σ{sub e} than predicted by standard mass-loss models. Finally, we find that T{sub gas} is set by the galaxy potential inside the optical effective radius. We conclude that within the innermost 10–30 kpc region, early types maintain pressure-supported hot gas, with a minimum T{sub gas} set by the virial temperature, but the majority show evidence for additional heating.

79 ASTRONOMY AND ASTROPHYSICS↗

Using depolarization to quantify ice nucleating particle concentrations: a new method

We have developed a new method to determine ice nucleating particle (INP) concentrations observed by the Texas A&M University continuous flow diffusion chamber (CFDC) under a wide range of operating conditions. In this study, we evaluate differences in particle optical properties detected by the Cloud and Aerosol Spectrometer with POLarization (CASPOL) to differentiate between ice crystals, droplets, and aerosols. The depolarization signal from the CASPOL instrument is used to determine the occurrence of water droplet breakthrough (WDBT) conditions in the CFDC. The standard procedure for determining INP concentration is to count all particles that have grown beyond a nominal size cutoff as ice crystals. During WDBT this procedure overestimates INP concentration, because large droplets are miscounted as ice crystals. Here we design a new analysis method based on depolarization ratio that can extend the range of operating conditions of the CFDC. The method agrees reasonably well with the traditional method under non-WDBT conditions with a mean percent error of ±32.1 %. Additionally, a comparison with the Colorado State University CFDC shows that the new analysis method can be used reliably during WDBT conditions.

54 ENVIRONMENTAL SCIENCES↗

Probing the atomically diffuse interfaces in Pd@Pt core-shell nanoparticles in three dimensions

Deciphering the three-dimensional atomic structure of solid-solid interfaces in core-shell nanomaterials is the key to understand their catalytical, optical and electronic properties. Here, we probe the three-dimensional atomic structures of palladium-platinum core-shell nanoparticles at the single-atom level using atomic resolution electron tomography. We quantify the rich structural variety of core-shell nanoparticles with heteroepitaxy in 3D at atomic resolution. Instead of forming an atomically-sharp boundary, the core-shell interface is found to be atomically diffuse with an average thickness of 4.2 Å, irrespective of the particle’s morphology or crystallographic texture. The high concentration of Pd in the diffusive interface is highly related to the free Pd atoms dissolved from the Pd seeds, which is confirmed by atomic images of Pd and Pt single atoms and sub-nanometer clusters using cryogenic electron microscopy. These results advance our understanding of core-shell structures at the fundamental level, providing potential strategies into precise nanomaterial manipulation and chemical property regulation.

74 ATOMIC AND MOLECULAR PHYSICS↗

Collaboration on SBIR/TTO Phase II Project for Optical QC Device and Collaboration on SBIR/TTO Phase II-b Project for Advanced Quality Inspection Device Development: Cooperative Research and Development CRADA Number CRD-16-00652 (Final Report)

The overall goal of this program is to develop and commercialize a turnkey quality control solution for the entire PEM fuel cell manufacturing process including membrane, gas diffusion layers, catalyst, and assembled systems. This quality control solution is unique to each customer’s specific needs but includes a suite of in-line quality control systems for roll-to-roll manufacturing that can target thin, transparent membrane as well as opaque membrane, catalyst, and GDLs. The Phase II developed the CPNUVV system for thin, transparent membrane that operates using polarized filters to enhance defect resolution and determine thickness. However, PEM material manufacturers want a complete, turnkey solution for all components of the PEM fuel cell. In the Phase IIB, Mainstream will partner with NREL, and transition reflectance technology NREL developed (US Patent 9,234,843) to operate in real-time on a web-line to develop a total solution to PEM quality control. The device will identify and mark defects as well as monitor materials thickness in real-time to improve line efficiency and to reduce waste. The research performed at NREL under this CRADA increases the basis of knowledge about optical inspection methods, how they perform with regards to fuel cell component materials, and how they can be implemented in in-line, real-time configurations to provide quality inspection for roll-to-roll (R2R) manufacturing. Methods explored were found to be sensitive to catalyst loading in electrodes on both membrane and gas diffusion media substrates and to membrane thickness, across a broad range of thickness. The latter capability is novel and now patented and provides a previously unstudied and undemonstrated capability for R2R manufacturing of membranes.

30 DIRECT ENERGY CONVERSION↗

Measurement of Sauter Mean Diameter (SMD) in Diesel Sprays Using a Scattering-Absorption Measurement Ratio (SAMR) Technique

A new diagnostic for the quantification of Sauter Mean Diameter (SMD) in high-pressure fuel sprays has been recently developed using combined optical and x-ray measurements at the Georgia Institute of Technology and Argonne National Laboratory, respectively. This diagnostic utilizes liquid scattering extinction measurements from diffuse back-illumination imaging, conducted at Georgia Tech, and liquid absorption measurements from x-ray radiography, conducted at Argonne’s Advanced Photon Source. The new diagnostic, entitled the Scattering Absorption Measurement Ratio (SAMR), quantifies two-dimensional distributions of path integrated SMD, enabling construction of the spatial history of drop size development within practical fuel sprays. This technique offers unique benefits over conventional drop-sizing methods in that it can be more robust in optically dense regions of the spray, while also providing high spatial and temporal resolution of the corresponding droplet field. The methodology for quantification of SMD distributions using the SAMR technique has been previously introduced and demonstrated in diesel sprays using the Engine Combustion Network Spray D injector, however a more detailed treatment of measurement uncertainties has been needed. In the current work, we present a summary of the various sources of measurement uncertainty in the SAMR diagnostic, like those due to the experimental setup, data processing methods, and theoretical assumptions, and assess how these sources of uncertainty affect the quantified SMD. The spatially-resolved SMD measurements that result from the SAMR diagnostic will be especially valuable to the engine modeling community for the quantitative validation of spray submodels in engine CFD codes. Careful evaluation and quantification of measurement uncertainties is important to support accurate model validation and to ensure the development of more predictive spray models.

33 ADVANCED PROPULSION SYSTEMS↗

Zn{sub 1−x}Co{sub x}WO{sub 4} (0 ≤ x ≤ 1) full range solid solution: Structure, optical properties, and magnetism

Graphical abstract: The continuous modulation on crystal structure and band gap is achieved in the Zn{sub 1−x}Co{sub x}WO{sub 4} (0 ≤ x ≤ 1) full range solid solution. - Highlights: • Zn{sub 1−x}Co{sub x}WO{sub 4} (0 ≤ x ≤ 1) solid solution was synthesized by a hydrothermal method. • They all present a single-phase in the wolframite structure with space group P2/c. • The continuous tenability in band gap was achieved in Zn{sub 1−x}Co{sub x}WO{sub 4} (0 ≤ x ≤ 1). • CoWO{sub 4} and Zn{sub 0.5}Co{sub 0.5}WO{sub 4} are antiferromagnetic and paramagnetic, respectively. - Abstract: A novel full-range solid-solution Zn{sub 1−x}Co{sub x}WO{sub 4} (0 ≤ x ≤ 1) was successfully developed via a facile one-pot hydrothermal route. The phase structure and microstructure were characterized by X-ray diffraction (XRD), Fourier-transform infrared (FTIR) spectra and scanning electron microscopy (SEM). The Zn{sub 1−x}Co{sub x}WO{sub 4} solid solution possesses similar wolframite crystal structure with the same space group P2/c. Diffuse reflection spectroscopy (DRS) measurements on Zn{sub 1−x}Co{sub x}WO{sub 4} (0 ≤ x ≤ 1) demonstrated that the optical band gap can be continuously tuned from 3.56 eV to 2.61 eV for direct transition and 1.87 eV for indirect transition, respectively, with increasing x from 0 to 1. Magnetic susceptibility measurements reveal that CoWO{sub 4} has an antiferromagnetic transition at T{sub N} = 42 K, whereas Zn{sub 0.5}Co{sub 0.5}WO{sub 4} exhibits paramagnetic behavior. Moreover, CoWO{sub 4} and Zn{sub 0.5}Co{sub 0.5}WO{sub 4} obey the Curie–Weiss law from 200 k down to 50 K, and their effective magnetic moments were determined.

36 MATERIALS SCIENCE↗

Ability of Particulate Matter Index to describe sooting tendency of various gasoline formulations in a stratified-charge spark-ignition engine

This study investigates the ability of Particulate Matter Index (PMI) to describe the sooting behavior of various gasoline formulations in a stratified-charge (SC) spark-ignition engine. Specifically, the engine was operated at 2000 rpm with an intake pressure of 130 kPa where soot formation is known to primarily occur in the bulk gases. Exhaust soot emissions were measured for nine test fuels at various exhaust gas recirculation levels. A comparison between measured soot levels and PMI shows that PMI is a relatively poor predictor of the sooting tendency of the tested fuels under lean SC combustion. Among the fuels, three fuels, namely the diisobutylene blend, High Olefin, and E30 fuels exhibit measured soot behavior opposite of that predicted by PMI. Optical diagnostics were utilized to further investigate the in-cylinder phenomena for these three fuels. Analysis of natural luminosity and diffused back-illumination extinction imaging suggests that fuel-induced differences in the amount of soot formed are responsible for a majority of the discrepancy in measured versus predicted sooting tendency. Fuel-induced differences in soot oxidation and spray development seem to play minor roles. Because the combustion and air-fuel mixing processes for lean SC combustion are different from conventional stoichiometric operation it is hypothesized that the PMI correlation needs to be modified to account for differences in stoichiometric air-fuel ratio and level of oxygenation between fuels. Furthermore, the role of fuel volatility in PMI possibly needs to be de-emphasized for SC operation with fuel injection into compression-heated gases.

42 ENGINEERING↗

EXTINCTION DROPLET SIZING MEASUREMENTS IN DIESEL RELEVANT SPRAYS

A new diagnostic for the quantification of Sauter Mean Diameter (SMD) in high-pressure fuel sprays has been recently developed using combined optical and x-ray measurements at the Georgia Institute of Technology and Argonne National Laboratory, respectively. This diagnostic utilizes liquid scattering extinction measurements from diffuse back-illumination (DBI) imaging, conducted at Georgia Tech, and liquid absorption measurements from x-ray radiography, conducted at Argonne’s Advanced Photon Source. The new diagnostic, entitled the Scattering Absorption Measurement Ratio (SAMR), quantifies two-dimensional distributions of path-integrated SMD, enabling construction of the spatial history of drop size development within practical fuel sprays. This technique offers unique benefits over conventional drop-sizing methods in that it can be more robust in optically dense regions of the spray, while also providing high spatial resolution of the corresponding droplet field. The spatially-resolved SMD measurements that result from the SAMR diagnostic will be especially valuable to the engine modeling community for the quantitative validation of spray submodels in engine CFD codes. The methodology for quantification of SMD distributions using the SAMR technique has been previously introduced. This thesis aims to extend the initial development of the SAMR technique by presenting in detail: the experimental methodologies used in the SAMR technique, including the development of an ideal DBI setup for this technique; the data processing methodologies developed by the author; two-dimensional Sauter Mean Diameter measurements within diesel sprays for various experimental conditions; a summary of the various sources of measurement uncertainty; an assessment for how the sources of uncertainty affect the quantified SMD; and paths to improve the technique moving forward. The SMD results show that for low ambient density conditions droplets decrease in size as radial and axial position increases. For high ambient density conditions, however, the droplets show a stable size near the spray centerline and steadily increase in size as distance from the centerline increases. Additionally, this work provides 2-D droplet sizing maps which are particularly useful for model validation.

33 ADVANCED PROPULSION SYSTEMS↗

EXTINCTION DROPLET SIZING MEASUREMENTS IN DIESEL RELEVANT SPRAYS

A new diagnostic for the quantification of Sauter Mean Diameter (SMD) in high-pressure fuel sprays has been recently developed using combined optical and x-ray measurements at the Georgia Institute of Technology and Argonne National Laboratory, respectively. This diagnostic utilizes liquid scattering extinction measurements from diffuse back-illumination (DBI) imaging, conducted at Georgia Tech, and liquid absorption measurements from x-ray radiography, conducted at Argonne’s Advanced Photon Source. The new diagnostic, entitled the Scattering Absorption Measurement Ratio (SAMR), quantifies two-dimensional distributions of path-integrated SMD, enabling construction of the spatial history of drop size development within practical fuel sprays. This technique offers unique benefits over conventional drop-sizing methods in that it can be more robust in optically dense regions of the spray, while also providing high spatial resolution of the corresponding droplet field. The spatially-resolved SMD measurements that result from the SAMR diagnostic will be especially valuable to the engine modeling community for the quantitative validation of spray submodels in engine CFD codes. The methodology for quantification of SMD distributions using the SAMR technique has been previously introduced. This thesis aims to extend the initial developmen of SAMR technique by presenting in detail: the experimental methodologies used in the SAMR technique, including the development of an ideal DBI setup for this technique; the data processing methodologies developed by the author; two-dimensional Sauter Mean Diameter measurements within diesel sprays for various experimental conditions; a summary of the various sources of measurement uncertainty; an assessment for how the sources of uncertainty affect the quantified SMD; and paths to improve the technique moving forward. The SMD results show that for low ambient density conditions droplets decrease in size as radial and axial position increases. For high ambient density conditions, however, the droplets show a stable size near the spray centerline and steadily increase in size as distance from the centerline increases. Additionally, this work provides 2-D droplet sizing maps which are particularly useful for model validation.

33 ADVANCED PROPULSION SYSTEMS↗

Solution Processed Ternary Tin (II) Alloy as Hole–Transport Layer of Sn–Pb Perovskite Solar Cells for Enhanced Efficiency and Stability

Tin-lead (Sn-Pb) narrow bandgap (NBG) perovskites show great potential in both single-junction and all-perovskite tandem solar cells. Sn-Pb perovskite solar cells (PSCs) are still limited by low charge collection efficiency and poor stability. Here, we report a ternary Sn (II) alloy of SnOCl as the hole-transport material (HTM) with a work function of 4.95 eV for Sn-Pb PSCs. The solution processed SnOCl layer has a texture structure which not only reduces the optical loss of the devices but also changes grain growth of Sn-Pb perovskites and boosts the carrier diffusion length to 3.63 μm. The formation of small perovskite grains at the HTM/perovskite interface is suppressed. These result in an almost constant internal quantum efficiency of 96 ± 2% across the absorption spectrum of Sn-Pb perovskites. The SnOCl HTM significantly enhances the stability of Sn-Pb PSCs with 87% of its initial efficiency retained after 1-sun illumination for 1,200 h, and keep 85% efficiency under 85°C thermal stress for 1,500 h. Furthermore, the hybrid HTM further improve the stabilized efficiencies of single-function Sn-Pb PSCs and all-perovskite tandem solar cells to 23.2% and 25.9%, respectively. This discovery opens an avenue to the multi-component metal alloys as HTM in PSCs.

36 MATERIALS SCIENCE↗

Characterization of high-explosive detonations using broadband infrared external cavity quantum cascade laser absorption spectroscopy

Infrared laser absorption spectroscopy provides a powerful tool for probing physical and chemical properties of high explosive detonations. A broadly-tunable swept-wavelength external cavity quantum cascade laser (ECQCL) operating in the mid-wave infrared (MWIR) spectral region is used to measure transmission through explosive fireballs generated from 14 g charges of 4 different explosive types detonated in an enclosed chamber. Analysis of time-resolved transmission and emission at a 2 µs sampling rate shows the evolution of fireball infrared opacity in the first 10 ms after detonation. Broadband high-resolution absorption spectra acquired over the spectral range 2050-2300 cm -1 (4.35-4.88 µm) at a 100 Hz rate are used to measure properties of fireball evolution over longer time scales out to 100 s. Path-integrated concentrations of combustion products CO, CO 2 , H 2 O, and N 2 O are measured and show evolutions over multiple time scales and significant differences between explosive types. Spectral analysis is used to characterize gas temperature and to measure broadband attenuation from absorption and scattering of particulates. In conclusion, analysis of the results provides information on the MWIR optical properties, gaseous detonation/combustion products, and particulates throughout the explosive process including initial detonation, fireball expansion and cooling, and diffusive mixing in the chamber.

45 MILITARY TECHNOLOGY, WEAPONRY, AND NATIONAL DEF↗

INTERSTELLAR-MEDIUM MAPPING IN M82 THROUGH LIGHT ECHOES AROUND SUPERNOVA 2014J

We present multiple-epoch measurements of the size and surface brightness of the light echoes from supernova (SN) 2014J in the nearby starburst galaxy M82. Hubble Space Telescope ( HST ) ACS/WFC images were taken ∼277 and ∼416 days after B -band maximum in the filters F 475 W , F 606 W , and F 775 W . Observations with HST WFC3/UVIS images at epochs ∼216 and ∼365 days are included for a more complete analysis. The images reveal the temporal evolution of at least two major light-echo components. The first one exhibits a filled ring structure with position-angle-dependent intensity. This radially extended, diffuse echo indicates the presence of an inhomogeneous interstellar dust cloud ranging from ∼100 to ∼500 pc in the foreground of the SN. The second echo component appears as an unresolved luminous quarter-circle arc centered on the SN. The wavelength dependence of scattering measured in different dust components suggests that the dust producing the luminous arc favors smaller grain sizes, while that causing the diffuse light echo may have sizes similar to those of the Milky Way dust. Smaller grains can produce an optical depth consistent with that along the supernova-Earth line of sight measured by previous studies around maximum light. Therefore, it is possible that the dust slab from which the luminous arc arises is also responsible for most of the extinction toward SN 2014J. The optical depths determined from the Milky Way-like dust in the scattering matters are lower than the optical depth produced by the dust slab.

79 ASTRONOMY AND ASTROPHYSICS↗

Measurement of Sauter mean diameter in diesel sprays using a scattering–absorption measurement ratio technique

A new diagnostic for the quantification of Sauter mean diameter in high-pressure fuel sprays has been recently developed using combined optical and X-ray measurements at the Georgia Institute of Technology and Argonne National Laboratory, respectively. This diagnostic utilizes liquid scattering extinction measurements from diffuse back-illumination imaging, conducted at Georgia Tech, and liquid absorption measurements from X-ray radiography, conducted at Argonne’s Advanced Photon Source. The new diagnostic, entitled the scattering–absorption measurement ratio, quantifies two-dimensional distributions of path-integrated Sauter mean diameter, enabling the construction of the spatial history of drop size development within practical fuel sprays. This technique offers unique benefits over conventional drop-sizing methods in that it can be more robust in optically dense regions of the spray, while also providing high spatial resolution of the corresponding droplet field. The methodology for quantification of Sauter mean diameter distributions using the scattering–absorption measurement ratio technique has been previously introduced and demonstrated in diesel sprays using the Engine Combustion Network Spray D injector; however, a more detailed treatment of measurement uncertainties has been needed. In this work, we present a summary of the various sources of measurement uncertainty in the scattering–absorption measurement ratio diagnostic, like those due to the experimental setup, data processing methods, and theoretical assumptions, and assess how these sources of uncertainty affect the quantified Sauter mean diameter. The spatially resolved Sauter mean diameter measurements that result from the scattering–absorption measurement ratio diagnostic will be especially valuable to the engine modeling community for the quantitative validation of spray submodels in engine computational fluid dynamics codes. Careful evaluation and quantification of measurement uncertainties are important to support accurate model validation and to ensure the development of more predictive spray models.

42 ENGINEERING↗

High-precision phase control of an optical lattice with up to 50 dB noise suppression

An optical lattice is a periodic light crystal constructed from the standing-wave interference patterns of laser beams. It can be used to store and manipulate quantum degenerate atoms and is an ideal platform for the quantum simulation of many-body physics. A principal feature is that optical lattices are flexible and possess a variety of multidimensional geometries with modifiable band structure. An even richer landscape emerges when control functions can be applied to the lattice by modulation of the position or amplitude with Floquet driving. However, the desire of realizing high-modulation bandwidths while preserving extreme lattice stability has been difficult to achieve. In this paper, we demonstrate an effective solution that consists of overlapping two counterpropagating lattice beams and controlling the phase and intensity of each with independent acousto-optic modulators. Our phase controller mixes sampled light from both lattice beams with a common optical reference. This dual heterodyne locking method allows exquisite determination of the lattice position, while also removing parasitic phase noise accrued as the beams travel along separate paths. Here, we report up to 50 dB suppression in lattice phase noise in the 0.1–1 Hz band, along with significant suppression spanning more than 4 decades of frequency. The absolute phase diffusion of the lattice position is only 10 Å when integrated over 10 s. This method permits precise, high-bandwidth modulation (greater than 50 kHz) of the optical lattice intensity and phase. We demonstrate the efficacy of this approach by executing intricate time-varying phase profiles for atom interferometry.

Atom interferometry↗

SeTe alloy semiconductor core optical fibers

Highlights: • Phosphate glass-clad Se{sub 0.5}Te{sub 0.5} semiconductor core optical fibers were fabricated. • Crystalline Se{sub 0.5}Te{sub 0.5} semiconductor core optical fibers were successfully obtained. • The fibers can detect light incident on it from at any point along its entire length. • The fibers can be used as stress sensing without the use of optical probing signals. - Abstract: Se{sub 0.5}Te{sub 0.5} semiconductor core optical fibers with phosphate glass cladding were fabricated by using a reactive molten core approach. The core was found to be amorphous with some oxygen diffusing in from the cladding glass. Crystalline Se{sub 0.5}Te{sub 0.5} (c-Se{sub 0.5}Te{sub 0.5}) semiconductor core fibers were obtained by a post-drawing annealing process. Significant disparities in conductivity under stress and without stress were observed in c-Se{sub 0.5}Te{sub 0.5} semiconductor core fibers. To the best of our knowledge, this is the first time that stress sensing can be realized in c-Se{sub 0.5}Te{sub 0.5} semiconductor core optical fibers. This is in contrast to all previous work on stress sensing using fibers, which require the use of optical probing signals. In addition, it is found that more than 60 times change in conductivity between dark and illuminated states in c-Se{sub 0.5}Te{sub 0.5} semiconductor core fibers. These results demonstrate that c-Se{sub 0.5}Te{sub 0.5} semiconductor core optical fibers have promising applications in stress sensor, photodetector, and optical switch.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Well-aligned polycrystalline lanthanum silicate oxyapatite grown by reactive diffusion between solid La{sub 2}SiO{sub 5} and gases [SiO+1/2O{sub 2}]

The c-axis-oriented polycrystalline lanthanum silicate oxyapatite, La{sub 9.48}(Si{sub 5.89}□{sub 0.11})O{sub 26} (□ denotes a vacancy in the Si site), was successfully prepared by the reactive diffusion between randomly grain-oriented La{sub 2}SiO{sub 5} polycrystal and [SiO+1/2O{sub 2}] gases at 1873 K in Ar atmosphere. The polycrystal was characterized using optical microscopy, scanning electron microscopy equipped with energy dispersive X-ray spectroscopy, micro-Raman spectroscopy, X-ray diffractometry, and impedance spectroscopy. The crystal structure (space group P6{sub 3}/m) showed the deficiency of Si site at ca. 1.9%. The bulk oxide-ion conductivity along the grain-alignment direction steadily increased from 9.2 × 10{sup −3} to 1.17 × 10{sup −2} S/cm with increasing temperature from 923 to 1073 K. The activation energy of conduction was 0.23(2) eV. - Graphical abstract: We have successfully prepared the highly c-axis-oriented polycrystalline La{sub 9.48}(Si{sub 5.89}□{sub 0.11})O{sub 26} by the reactive diffusion between randomly grain-oriented La{sub 2}SiO{sub 5} polycrystal and [SiO + 1/2O{sub 2}] gases at 1873 K in Ar atmosphere. The crystal structure (space group P6{sub 3}/m) showed the deficiency of Si site of ca. 1.9%. - Highlights: • The c-axis-oriented polycrystalline La{sub 9.48}(Si{sub 5.89}□{sub 0.11})O{sub 26} is successfully prepared. • Crystal structure of La{sub 9.48}(Si{sub 5.89}□{sub 0.11})O{sub 26} is determined by single-crystal XRD. • The polycrystal shows relatively high oxide ion conductivity along the common c-axis. • Reactive diffusion is successfully used for the preparation of grain-aligned ceramics.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗