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1,132 records · Page 63

Mineralogical and chemical characterization of iron-, manganese-, and copper-containing synthetic hydroxyapatites

The National Aeronautics and Space Administration's (NASA) Advanced Life Support (ALS) Program is evaluating the use of Fe-, Mn-, and Cu-containing synthetic hydroxyapatite (SHA) as a slow release fertilizer for crops that might be grown on the International Space Station or at Lunar and Martian outposts. Separate Fe-, Mn-, and Cu-containing SHA materials along with a transition-metal free SHA (pure-SHA) were synthesized using a precipitation method. Chemical and mineralogical analyses determined if and how Fe, Mn, and Cu were incorporated into the SHA structure. X-ray diffraction (XRD), Rietveld refinement, and transmission electron microscopy (TEM) confirmed that SHA materials with the apatite structure were produced. Chemical analyses indicated that the metal containing SHA materials were deficient in Ca relative to pure-SHA. The shift in the infrared PO4-mu 3 vibrations, smaller unit cell parameters, smaller particle size, and greater structural strain for Fe-, Mn-, and Cu-containing SHA compared with pure-SHA suggested that Fe, Mn, and Cu were incorporated into SHA structure. Rietveld analyses revealed that Fe, Mn, and Cu substituted into the Ca2 site of SHA. An Fe-rich phase was detected by TEM analyses and backscattered electron microscopy in the Fe-containing SHA material with the greatest Fe content. The substitution of metals into SHA suggests that metal-SHA materials are potential slow-release sources of micronutrients for plant uptake in addition to Ca and P.

NASA Center JSC↗

A high-throughput energy-dispersive tender X-ray spectrometer for shot-to-shot sulfur measurements

An X-ray emission spectrometer that can detect the sulfur K α emission lines with large throughput and a high energy resolution is presented. The instrument is based on a large d -spacing perfect Bragg analyzer that diffracts the sulfur K α emission at close to backscattering angles. This facilitates the application of efficient concepts routinely employed in hard X-ray spectrometers towards the tender X-ray regime. The instrument described in this work is based on an energy-dispersive von Hamos geometry that is well suited for photon-in photon-out spectroscopy at X-ray free-electron laser and synchrotron sources. Comparison of its performance with previously used instrumentation is presented through measurements using sulfur-containing species performed at the LCLS. It is shown that the overall signal intensity is increased by a factor of ∼15. Implementation of this approach in the design of a tender X-ray spectroscopy endstation for LCLS-II is also discussed.

36 MATERIALS SCIENCE↗

Effect of Thickness on the Structure, Composition and Properties of Titanium Nitride Nano-Coatings

Titanium nitride (TiNx) coatings were grown by magnetron sputtering onto Si(1 0 0) substrates by varying time of deposition to produce coatings with variable thickness (dTiN) in the range of 20-120 nm. TiNx coatings were characterized by studying their structure, composition, and mechanical properties. Nuclear reaction analysis (NRA) combined with Rutherford backscattering spectrometry (RBS) analyses indicate that the grown coatings were stoichiometric TiN. Grazing incidence X-ray diffraction (GIXRD) measurements indicate that the texturing of TiN coatings changes as a function of dTiN. The (1 1 1) and (0 0 2) peaks appear initially; (1 1 1) becomes intense while (0 0 2) disappears with increasing dTiN. Dense, columnar grain structure was evident for all the coatings in electron microscopy analyses. The residual stress for TiN coatings with dTiN~120 nm was 1.07 GPa in compression while thinner samples exhibit higher values of stress.

Coatings↗

Investigation of Zr-doped BSCF perovskite membrane for oxygen separation in the intermediate temperature range

The series of (Ba₀.₅Sr₀.₅)(Co₀.₈Fe₀.₂){sub 1–z}Zr{sub z}O{sub 3–δ} (z=0, 0.01, 0.03, 0.05, 0.07, and 0.09) was synthesized by a sol–gel method. The materials with a zirconium content up to 3 mol% were found to be single phase. Further increase results in formation of a mixed (Ba,Sr)ZrO₃ by-phase, which was found along the grain boundaries and in the grains. With increasing zirconium content the oxygen permeation flux decreases considerably. The effect of the zirconium substitution on the long-term phase stability was investigated by long-term oxygen permeation experiments and X-ray diffraction. A slight stabilization of the oxygen flux of (Ba₀.₅Sr{sub 0.5})(Co₀.₈Fe₀.₂)₀.₉₇Zr₀.₀₃O{sub 3–δ} was found after 180 h at 1023 K. However, all compositions show a decrease in permeation flux with time, but the pure BSCF membrane exhibited the strongest drop after 180 h of operation. The decomposition products of the cubic perovskite phase were found to be a hexagonal Ba{sub 0.5±x}Sr{sub 0.5±x}CoO₃ and a rhombohedral Ba{sub 1–x}Sr{sub x}Co{sub 2–y}Fe{sub y}O{sub 5–δ}. - Graphical abstract: Backscattered-electron channeling contrast image of BSCF membrane cross-section after long-term oxygen permeation at 1023 K showing different phases in different colors. Highlights: • Ba₀.₅Sr₀.₅Co₀.₈Fe₀.₂O{sub 3–δ} systematically doped with increasing amount of zirconium. • Cubic single-phase materials up to 3 wt% zirconium. • Mixed (Ba,Sr)ZrO₃ by-phase formed mainly in the grain boundaries. • Jänecke prism was proposed by XRD and EDXS data. • (Ba₀.₅Sr₀.₅)(Co₀.₈Fe₀.₂)₀.₉₇Zr₀.₀₃O{sub 3–δ} showed a slight stabilization of oxygen flux as compared to pure Ba₀.₅Sr₀.₅Co₀.₈Fe₀.₂O{sub 3–δ}.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Narrow bandgap semiconducting silicides: Intrinsic infrared detectors on a silicon chip

Work done during the final report period is presented. The main technical objective was to achieve epitaxial growth on silicon of two semiconducting silicides, ReSi2 and CrSi2. ReSi2 thin films were grown on (001) silicon wafers by vacuum evaporation of rhenium onto hot substrates in ultrahigh vacuum. The preferred epitaxial relationship was found to be ReSi2(100)/Si(001) with ReSi2(010) parallel to Si(110). The lattice matching consists of a common unit mesh of 120 A(sup 2) area, and a mismatch of 1.8 percent. Transmission electron microscopy revealed the existence of rotation twins corresponding to two distinct but equivalent azimuthal orientations of the common unit mesh. MeV He(+) backscattering spectrometry revealed a minimum channeling yield of 2 percent for an approximately 1,500 A thick film grown at 650 C. Although the lateral dimension of the twins is on the order of 100 A, there is a very high degree of alignment between the ReSi2(100) and the Si(001) planes. Highly oriented films of CrSi2 were grown on (111) silicon substrates, with the matching crystallographic faces being CrSi2(001)/Si(111). The reflection high-energy electron diffraction (RHEED) patterns of the films consist of sharp streaks, symmetrically arranged. The predominant azimuthal orientation of the films was determined to be CrSi2(210) parallel to Si(110). This highly desirable heteroepitaxial relationship has been obtained previously by others; it may be described with a common unit mesh of 51 A(sup 2) and mismatch of 0.3 percent. RHEED also revealed the presence of limited film regions of a competing azimuthal orientation, CrSi2(110) parallel to Si(110). A channeling effect for MeV He(+) ions was not found for this material. Potential commercial applications of this research may be found in silicon-integrated infrared detector arrays. Optical characterizations showed that semiconducting ReSi2 is a strong absorber of infrared radiation, with the adsorption constant increasing above 2 x 10(exp 4) cm(sup -1) for photon energies above 0.2 eV. CrSi2 is of potential utility for detection at photon energies above approximately 0.3 eV.

Mahan, John E.↗

A combined QXRD/TG method to quantify the phase composition of hydrated Portland cements

A new method is reported for quantifying the mineral phases in hydrated cement pastes that is based on a combination of quantitative X-ray diffractometry (QXRD) and thermogravimetry (TG). It differs from previous methods in that it gives a precise measure of the amorphous phase content without relying on an assumed stoichiometric relationship between the principal hydration products, calcium hydroxide (CH) and calcium silicate hydrate (C–S–H). The method was successfully applied to gray and white ordinary Portland cements (GOPC and WOPC, respectively) that were cured for up to 56 days. Phase distributions determined by QXRD/TG closely matched those from gray-level analysis of backscattered scanning electron microscope (BSEM) images, whereas elemental compositions obtained for the amorphous phase by QXRD/TG agreed well with those measured by quantitative energy dispersive X-ray spectroscopy (EDS)

36 MATERIALS SCIENCE↗

Green cubic GaInN/GaN light-emitting diode on microstructured silicon (100)

GaInN/GaN light-emitting diodes free of piezoelectric polarization were prepared on standard electronic-grade Si(100) substrates. Micro-stripes of GaN and GaInN/GaN quantum wells in the cubic crystal structure were grown on intersecting (111) planes of microscale V-grooved Si in metal-organic vapor phase epitaxy, covering over 50% of the wafer surface area. Crystal phases were identified in electron back-scattering diffraction. A cross-sectional analysis reveals a cubic structure virtually free of line defects. Electroluminescence over 20 to 100 μA is found fixed at 487 nm (peak), 516 nm (dominant). Such structures therefore should allow higher efficiency, wavelength-stable light emitters throughout the visible spectrum.

36 MATERIALS SCIENCE↗

Gas source molecular beam epitaxy of scandium nitride on silicon carbide and gallium nitride surfaces

Scandium nitride (ScN) is a group IIIB transition metal nitride semiconductor with numerous potential applications in electronic and optoelectronic devices due to close lattice matching with gallium nitride (GaN). However, prior investigations of ScN have focused primarily on heteroepitaxial growth on substrates with a high lattice mismatch of 7%–20%. In this study, the authors have investigated ammonia (NH{sub 3}) gas source molecular beam epitaxy (NH{sub 3}-GSMBE) of ScN on more closely lattice matched silicon carbide (SiC) and GaN surfaces (<3% mismatch). Based on a thermodynamic analysis of the ScN phase stability window, NH{sub 3}-GSMBE conditions of 10{sup −5}–10{sup −4} Torr NH{sub 3} and 800–1050 °C where selected for initial investigation. In-situ x-ray photoelectron spectroscopy (XPS) and ex-situ Rutherford backscattering measurements showed all ScN films grown using these conditions were stoichiometric. For ScN growth on 3C-SiC (111)-(√3 × √3)R30° carbon rich surfaces, the observed attenuation of the XPS Si 2p and C 1s substrate core levels with increasing ScN thickness indicated growth initiated in a layer-by-layer fashion. This was consistent with scanning electron microscopy (SEM) images of 100–200 nm thick films that revealed featureless surfaces. In contrast, ScN films grown on 3C-SiC (111)-(3 × 3) and 3C-SiC (100)-(3 × 2) silicon rich surfaces were found to exhibit extremely rough surfaces in SEM. ScN films grown on both 3C-SiC (111)-(√3 × √3)R30° and 2H-GaN (0001)-(1 × 1) epilayer surfaces exhibited hexagonal (1 × 1) low energy electron diffraction patterns indicative of (111) oriented ScN. X-ray diffraction ω-2θ rocking curve scans for these same films showed a large full width half maximum of 0.29° (1047 arc sec) consistent with transmission electron microscopy images that revealed the films to be poly-crystalline with columnar grains oriented at ≈15° to the [0001] direction of the 6H-SiC (0001) substrate. In-situ reflection electron energy loss spectroscopy measurements determined the band-gap for the NH{sub 3}-GSMBE ScN films to be 1.5 ± 0.3 eV, and thermal probe measurements indicated all ScN films to be n-type. The four point probe sheet resistance of the ScN films was observed to increase with decreasing growth temperature and decreased with unintentional oxygen incorporation. Hg probe capacitance–voltage measurements indicated N{sub D}-N{sub A} decreased with decreasing growth temperature from 10{sup 19} to 10{sup 20}/cm{sup 3} for the lowest resistivity films to ≅5 × 10{sup 16}/cm{sup 3} for the highest resistivity films. In-situ ultraviolet photoelectron spectroscopy measurements additionally showed the valence band maximum moving from 1.4 to 0.8 eV below the Fermi level with decreasing growth temperature consistent with the increased resistivity and reduction in carrier concentration. These results suggest that additional reductions in ScN carrier concentrations can be achieved via continued optimization of ScN growth conditions and selection of substrate orientation and surface termination.

36 MATERIALS SCIENCE↗

A Transmission Electron Microscopy Study of a Refractory Metal Grain from a Calcium-Aluminum-Rich Inclusion in the Leoville CV3 Chondrite

Introduction: Calcium-aluminum-rich inclusions (CAIs) are an important component of chondritic meteorites. They can contain materials that are thermodynamically predicted and isotopically age dated to be among the first-formed solids in our solar system [1-5]. Observed in some CAIs are micron to sub-micron sized inclusions rich in Fe, Ni, and high-Z elements such as Pt, Os, Ir and W, in the form of refractory metal nuggets (RMNs), fremdlinges, and ‘nugget like objects’ (NLOs) [1,6]. Refractory siderophile elements such as Os, Ir and Ru are thermodynamically predicted to condense at temperatures well in excess of the major CAI phases such as melilite, perovskite, spinel and hibonite [2,7-9]. These refractory metal inclusions in CAIs can therefore serve as probes into the thermodynamic landscape of the early solar protoplanetary disk. Here we report on a refractory grain identified in a CAI of the Leoville CV3 chondrite. This work is part of an ongoing effort to gain insight into the thermochemistry of the early solar system through systematic analyses of the structure and chemistry of various components in CAIs [10-13]. Sample and Analytical Techniques: A fluffy type A CAI (Fig. 1A) was identified in a section of the Leoville, CV3 chondrite (Center for Meteorite Studies, Arizona State University collection, #821_C_3) using a JOEL-JXA 8530F electron microprobe at Arizona State University. Backscattered electron (BSE) imaging and energy-dispersive X-ray spectroscopy (EDS) were used to identify refractory metal grains in the CAI using a Thermo Fisher (formerly FEI) Helios NanoLab 660 G3 focused-ion-beam scanning-electron microscope (FIBSEM) located at the Kuiper Materials Imaging and Characterization Facility (KMICF) at the Lunar and Planetary Laboratory, University of Arizona. The FIB is equipped with an EDAX EDS system. We selected one of the larger (micron-sized) refractory metal grains, designated as ‘Spud’ (Fig. 1B) for further analysis. ‘Spud’ was extracted and thinned to electron transparency (<100 nm) using the FIB-SEM located in KMICF, following methods described by [14- 15]. The FIB section was analyzed using a 200 keV Hitachi HF5000 scanning transmission electron microscope (S/TEM) located at KMICF. The HF5000 is equipped with cold-field emission gun, 3rd-order spherical aberration corrector for STEM imaging, and an Oxford Instruments X-Max N 100 TLE energydispersive spectroscopy (EDS) system with dual 100 mm2 windowless silicon-drift detectors (Ω = 2.0 sr). Selected-area electron-diffraction (SAED) patterns were acquired to aid in determination of crystallinity and phase. Results: The mineralogy, texture, and morphology of the CAI are consistent with that of a fluffy type A (FTA) CAI [16]. BSE imaging at high magnifications revealed grains with high contrast, indicative of compositions rich in elements of higher atomic number relative to surrounding material. These high-Z grains have sizes that range from ∼250 nm to 4 µm. EDS analyses confirm that the bright grains are metal-rich inclusions. A minor fraction of the grains are composed of only Fe and Ni, but the majority (∼60%) of the identified inclusions also contained various refractory siderophiles including Os, Ru, Zr, Ir and Mo. EDS analysis on the FIB-SEM of Spud shows that it contains Fe, Ni, Mo and Ru. High-angle annular dark-field (HAAFD) imaging and EDS mapping in the TEM (Fig. 2) show that Spud occurs in melilite (Ca1.9Al1.99Si1.06O7). Spud contains a subhedral to anhedral morphology and is compositionally heterogenous (polyphasic, Fig. 2). Local spatial correlation occurs among Fe, Ni, and Pt, and also among Os, Ru, and Mo. SAED patterns show that the Fe-Ni-Pt, Fe-Os-Mo-Ru and Fe-Pt regions are crystalline. Discussion: CAIs can contain various types of inclusions rich in Fe, Ni and refractory siderophiles such as Os, Ru, W and Pt [1]. RMNs are micron-sized, single phase alloy grains and can contain Os, Ir, Ru and Rh [1,7,17]. NLOs are also micron-sized inclusions, but contain two phases, a refractory metal, and an oxide [6]. Fremdlinge are the largest of such inclusions (tens of microns in size) and are complex aggregates of Fe-Ni alloy, silicates, oxides, and sulfides [1,17]. While the size of Spud matches previous descriptions of RMNs and NLOs, Spud is neither a single-phase alloy like RMNs, nor does it contain one metal phase and one oxide like NLOs. Spud does not match the above described categories of refractory metal inclusions. The presence of refractory siderophiles such as Mo, Os, Ru, and Pt suggests a high-temperature origin. Thermodynamic modelling by [7] indicates condensation temperatures of 1917 K, 1693 K, 1613 K and 1415 K for Os, Mo, Ru and Pt respectively. These models also show that following the initial condensation of a refractory metal, alloying of solutes such as Fe, Ni and W, occurs in levels proportional to their partial pressures in the surrounding gas. Such alloying occurs at temperatures above the condensation temperatures of common CAI phases such as melilite (1529 K), perovskite (1441 K), spinel (197 K) and forsterite (1354 K) [2]. The polyphasic nature of Spud could be the result of such high-temperature alloying, possibly shortly after the condensation of Mo and Ru at 1693 K and 1613 K respectively. That Spud occurs as an inclusion is consistent with it having formed prior to and at temperature above that of its host melilite in this FTA CAI, which is qualitatively consistent with such prior thermodynamic modeling. Further, the polyphasic nature of Spud is similar to refractory grains from a FTA CAI in the Northwest Africa (NWA) 8323, CV3 chondrite [11-13]. These data suggest that such refractory metal grains could have been widespread in the inner and early solar protoplanetary disk and represent some of the earliest formed solids to have condensed. Acknowledgments: Research and instrumentation supported by NASA grants #NNX12AL47G, #NNX15AJ22G and #80NSSC19K0509, and NSF grants #1531243 and #0619599. Fig 2. STEM data on ‘Spud’. HAADF Image (Top) False-color EDS Maps (Bottom) References: [1] MacPherson G. J. (2014) T. of Geochem. Vol I: Met. And Cosmochem. Processes, 139-179. [2] Lodders K. (2003) ApJ, 591, 1220-1247. [3] Ebel D. S. (2006) Met. & the Early S. Sys. II., 253- 277. [4] Amelin Y. (2002) Science, 297, 1678-1683. [5] Connelly J.N. et.al. (2012) Science, 338, 651-655. [6] Schwander D. et al. (2015) GCA, 18, 70-87. [7] Palme H. and Wlotzka F. (1976) EPSL, 33, 45-60. [8] Berg T. et al. (2009) ApJ, 702, 172-176. [9] Liffman K. et al. (2021) Icarus, 221, 89-105. [10] Zega T.J. et al. (2021) PSJ, 2, 115. [11] Ramprasad T. et al. (2020) LPSC LI, Abstract #2472. [12] Ramprasad T. et al. (2021) Microscopy & Microanalysis, S1, 2792-2794. [13] Ramprasad T. et al. (2021) 84th MetSoc, Abstract #6123. [14] Zega T.J. et al. (2007) MAPS, 42, 1373-1386. [15] Ramprasad T. et al. (2022) MAPS, in revision. [16] Grossman L. (1975), GCA, 39, 433-454. [17] El Goresy A. et al. (1978) LPSC IX, Abstract#1100

T. Ramprasad↗

Compositional dependence of the band-gap of Ge{sub 1−x−y}Si{sub x}Sn{sub y} alloys

The group-IV semiconductor alloy Ge{sub 1−x−y}Si{sub x}Sn{sub y} has recently attracted great interest due to its prospective potential for use in optoelectronics, electronics, and photovoltaics. Here, we investigate molecular beam epitaxy grown Ge{sub 1−x−y}Si{sub x}Sn{sub y} alloys lattice-matched to Ge with large Si and Sn concentrations of up to 42% and 10%, respectively. The samples were characterized in detail by Rutherford backscattering/channeling spectroscopy for composition and crystal quality, x-ray diffraction for strain determination, and photoluminescence spectroscopy for the assessment of band-gap energies. Moreover, the experimentally extracted material parameters were used to determine the SiSn bowing and to make predictions about the optical transition energy.

36 MATERIALS SCIENCE↗

Residual Strain Analysis in Linear Friction Welds of Similar and Dissimilar Titanium Alloys Using Energy Dispersive X-ray Diffraction

Residual strains in linear friction welds (LFW) of similar, Ti-6Al-4V (Ti64) welded to Ti-6Al-4V, and dissimilar, Ti-6Al-4V welded to Ti-5Al-5V-5Mo-3Cr (Ti5553), titanium alloys have been characterized using energy-dispersive X-ray diffraction. For each type of LFW, one sample was chosen in the as-welded (AW) condition and another sample was selected after a post-weld heat treatment (HT). Residual strains have been separately studied in the alpha and beta phases of the material, and five components (three axial and two shear) have been reported in each case. In-plane axial components of the residual strains show a smooth and symmetric behavior about the weld center for the Ti64-Ti64 LFW samples in the AW condition, whereas these components in the Ti64-Ti5553 LFW sample show a symmetric trend with jump discontinuities. Such jump discontinuities, observed in both the AW and HT conditions of the Ti64-Ti5553 samples, suggest different strain-free lattice parameters in the weld region and the parent material, whereas the results from the Ti64-Ti64 LFW samples in both AW and HT conditions suggest nearly uniform strain-free lattice parameters throughout the weld region. Finally, the observed trends in the in-plane axial residual strain components have been rationalized by the corresponding microstructural changes and variations across the weld region via backscatter electron (BSE) images.

36 MATERIALS SCIENCE↗

Beyond magnons in Nd 2 ScNbO 7 : An Ising pyrochlore antiferromagnet with all-in–all-out order and random fields

We report the low-temperature magnetic properties of Nd 3+ pyrochlore Nd 2 ScNbO 7 . Susceptibility and magnetization show an easy-axis moment, and heat capacity reveals a phase transition to long-range order at T N =371(2) mK with a fully recovered ΔS=Rln(2), 53% of it recovered for T>T N . Elastic neutron scattering shows a long-range all-in all-out magnetic order with low-Q diffuse elastic scattering. Inelastic neutron scattering shows a low-energy flat band, indicating a magnetic Hamiltonian similar to Nd 2 Zr 2 O 7 . Nuclear hyperfine excitations measured by ultra-high-resolution neutron backscattering indicate a distribution of static electronic moments below T N , which may be due to B-site disorder influencing Nd crystal electric fields. Analysis of heat-capacity data shows an unexpected T-linear or T 3/2 term which is inconsistent with conventional magnon quasiparticles, but is consistent with fractionalized spinons or gapless local spin excitations. We use legacy data to show similar behavior in Nd 2 Zr 2 O 7 . Comparing local static moments also reveals a suppression of the nuclear Schottky anomaly in temperature, evidencing a fraction of Nd sites with nearly zero static moment, consistent with exchange-disorder-induced random singlet formation. Finally, taken together, these measurements suggest an unusual fluctuating magnetic ground state which mimics a spin liquid, but may not actually be one.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Large Aperture Scanning Lidar Based on Holographic Optical Elements

Lidar remote sensing instruments can make a significant contribution to satisfying many of the required measurements of atmospheric and surface parameters for future spaceborne platforms, including topographic altimeters, atmospheric profiles of, wind, humidity, temperature, trace molecules, aerosols, and clouds. It is highly desirable to have wide measurement swaths for rapid coverage rather than just the narrow ribbon of data that is obtained with a nadir only observation. For most applications global coverage is required, and for wind measurements scanning or pointing is required in order to retrieve the full 3-D wind vector from multiple line-of-sight Doppler measurements. Conventional lidar receivers make up a substantial portion of the instrument's size and weight. Wide angle scanning typically requires a large scanning mirror in front of the receiver telescope, or pointing the entire telescope and aft optics assembly, Either of these methods entails the use of large bearings, motors, gearing and their associated electronics. Spaceborne instruments also need reaction wheels to counter the torque applied to the spacecraft by these motions. NASA has developed simplified conical scanning telescopes using Holographic Optical Elements (HOEs) to reduce the size, mass, angular momentum, and cost of scanning lidar systems. NASA has developed two operating lidar systems based on 40 cm diameter HOEs. The first such system, named Prototype Holographic Atmospheric Scanner for Environmental Remote Sensing (PHASERS) was a joint development between NASA Goddard Space Flight Center (GSFC) and the University of Maryland College Park. PHASERS is based on a reflection HOE for use at the doubled Nd:YAG laser wavelength of 532 nm and has recently undergone a number of design changes in a collaborative effort between GSFC and Saint Anselm College in New Hampshire. The next step was to develop IR transmission HOEs for use with the Nd:YAG fundamental in the Holographic Airborne Rotating Lidar Instrument Experiment (HARLIE). The HOE spins like a compact disk in a large ring ball bearing. In an aircraft the HOE faces down, looking out through a window at an angle of 45 degrees off-nadir. The HOE diffracts 85% of the incident 532 nm light into a 160 micron spot at a focal length of 1 meter. HARLIE is a field deployable lidar measuring aerosol, cloud, and boundary layer backscatter for atmospheric research. It has flown several times and is also used from a ground-based trailer in an upward-looking mode. The HOE generates a 45 degree conical scan pattern by rotating at speeds up to 30 rpm. Like PHASERS, the HOE in HARLIE serves both as the laser collimating lens as well as the receiver telescope primary optic. The telescope is coupled to the receiver package via fiber optic. The transmitter is a diode pumped Nd:YAG laser operating at 1064 nm, delivering 1 mJ pulses at a 5 KHz rep-rate. The receiver has a 200 microradian field-of-view and a 0.5 nm optical bandpass. The photon counting data system utilizes a single Geiger-mode silicon avalanche photodiode detector, This new technology has also presented us with new data visualization challenges as well as new measurement techniques. The backscatter data obtained from a stationary (i.e. ground-based) scanning HOE lidar is on the surface of a cone, which when viewed over many consecutive scans can reveal atmospheric motions on this surface over time as the atmosphere advects over the site. In a moving platform such as an airplane or satellite, the data from consecutive scans cover different areas under the flight path, revealing atmospheric structure in 3-dimensions. An example of a visualization of HARLIE ground-based data is presented, showing aerosol backscatter on a 90 degree conical surface generated from one 360 degree scan of the lidar during the HOLO-1 field campaign on the afternoon of 10 March 1999. Higher backscatter levels are rendered as lighter signal against a dark background. Breaking Kelvin-Helmholtz waves are evident on the north side of the scan at an altitude of 10-11 km. Time series of successive scans made at regular intervals render unique views of atmospheric motions, from which vertical profiles of atmospheric wind vectors can be obtained using a unique data analysis approach. Wind vectors obtained from the lidar were compared with co-located radiosonde wind profiles during an intensive operating period in September-October 2000 at the Atmospheric Radiation Measurement Program's Southern Great Plains Central Facility.

Schwemmer, Geary K.↗

Development of Acoustic Backscatter for In Situ Monitoring of Nuclear Sludge Wastes During Transfer - 20117

This paper presents an overview into the use of acoustic backscatter systems (ABS) for the in situ characterization of nuclear waste sludge concentration, size and aggregation, highlighting key achievements from the University of Leeds. Previous projects funded through the Engineering and Physical Sciences Research Council (EPSRC) UK and Innovate UK are firstly reviewed and linked to current research within the new TRANSCEND consortium. Detailed are a number of developments at various stages of technology readiness level, from the use of ABS to monitor small-scale sludge settling in columns, to large-scale jet-mixing and waste transfer operations. Current work with Sellafield Ltd will see new technology and world leading analysis methods deployed to measure the consolidation of complex wastes currently undergoing containment, the first time full industrial utilization of these systems has been achieved. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

A multi-technique analysis of deuterium trapping and near-surface precipitate growth in plasma-exposed tungsten

In this work, we examine how deuterium becomes trapped in plasma-exposed tungsten and forms near-surface platelet-shaped precipitates. How these bubbles nucleate and grow, as well as the amount of deuterium trapped within, is crucial for interpreting the experimental database. Here, we use a combined experimental/theoretical approach to provide further insight into the underlying physics. With the Tritium Plasma Experiment, we exposed a series of ITER-grade tungsten samples to high flux D plasmas (up to 1.5 × 10{sup 22 }m{sup −2} s{sup −1}) at temperatures ranging between 103 and 554 °C. Retention of deuterium trapped in the bulk, assessed through thermal desorption spectrometry, reached a maximum at 230 °C and diminished rapidly thereafter for T > 300 °C. Post-mortem examination of the surfaces revealed non-uniform growth of bubbles ranging in diameter between 1 and 10 μm over the surface with a clear correlation with grain boundaries. Electron back-scattering diffraction maps over a large area of the surface confirmed this dependence; grains containing bubbles were aligned with a preferred slip vector along the <111> directions. Focused ion beam profiles suggest that these bubbles nucleated as platelets at depths of 200 nm–1 μm beneath the surface and grew as a result of expansion of sub-surface cracks. To estimate the amount of deuterium trapped in these defects relative to other sites within the material, we applied a continuum-scale treatment of hydrogen isotope precipitation. In addition, we propose a straightforward model of near-surface platelet expansion that reproduces bubble sizes consistent with our measurements. For the tungsten microstructure considered here, we find that bubbles would only weakly affect migration of D into the material, perhaps explaining why deep trapping was observed in prior studies with plasma-exposed neutron-irradiated specimens. We foresee no insurmountable issues that would prevent the theoretical framework developed here from being extended to a broader range of systems where precipitation of insoluble gases in ion beam or plasma-exposed metals is of interest.

36 MATERIALS SCIENCE↗

Preparation, phase structure and microwave dielectric properties of CoLi{sub 2/3}Ti{sub 4/3}O{sub 4} ceramic

Graphical abstract: For chemical compatibility tests with silver electrode, mixtures of ceramic powders with 20 wt% Ag powders were cofired and analyzed to detect interactions between the low-fired samples and electrodes. XRD patterns and backscattered electron image of CoLi{sub 2/3}Ti{sub 4/3}O{sub 4} ceramics added with 1.5 wt% BCB cofired with Ag at 900 Degree-Sign C for 2 h are presented in . Backscattered electron image analysis reveals no interaction to form new phases after firing. This observation is also confirmed by the evidence of no difference between the XRD patterns before and after firing. It is obvious that the reaction of low-fired CoLi{sub 2/3}Ti{sub 4/3}O{sub 4} ceramics with Ag electrodes did not occur. Highlights: Black-Right-Pointing-Pointer A new microwave dielectric ceramic with good properties was reported. Black-Right-Pointing-Pointer The addition of BaCu(B{sub 2}O{sub 5}) can lower the sintering temperature from 1050 Degree-Sign C to 900 Degree-Sign C. Black-Right-Pointing-Pointer The addition of BaCu(B{sub 2}O{sub 5}) does not induce degradation of properties. Black-Right-Pointing-Pointer BCB added CoLi{sub 2/3}Ti{sub 4/3}O{sub 4} ceramics can co-fire with Ag electrode. -- Abstract: A new low loss microwave dielectric ceramic with composition of CoLi{sub 2/3}Ti{sub 4/3}O{sub 4} was prepared by a conventional solid-state reaction method. The compound has a cubic spinel structure [Fd-3m (227)] similar to MgFe{sub 2}O{sub 4} with lattice parameters of a = 8.3939 Angstrom-Sign , V = 591.42 Angstrom-Sign {sup 3}, Z = 8 and {rho} = 4.30 g/cm{sup 3}. This ceramic has a low sintering temperature ({approx}1050 Degree-Sign C) and good microwave dielectric properties with relative permittivity of 21.4, Q Multiplication-Sign f value of 35,000 GHz and {tau}{sub f} value of -22 ppm/ Degree-Sign C. Furthermore, the addition of BaCu(B{sub 2}O{sub 5}) (BCB) can effectively lower the sintering temperature from 1050 Degree-Sign C to 900 Degree-Sign C and does not induce much degradation of the microwave dielectric properties. Compatibility with Ag electrode indicates that the BCB added CoLi{sub 2/3}Ti{sub 4/3}O{sub 4} ceramics are good candidates for LTCC applications.

36 MATERIALS SCIENCE↗