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At least 325 records · Page 18

Smoke detection in low-G fires

Fires in spacecraft are considered a credible risk. To respond to this risk, NASA flew fire detectors on Skylab and the Space Shuttle (STS) and included them in the design for International Space Station Alpha (ISSA). In previous missions (Mercury, Gemini and Apollo), the crew quarters were so cramped that it was not considered credible that the astronauts could fail to observe a fire. The Skylab nodule included approximately 20 UV fire detectors. The space shuttle has 9 ionization detectors in the mid deck and flight deck and Spacelab has six additional ionization detectors. The planned detectors for ISSA are laser-diode, forward-scattering, smoke or particulate detectors. Current plans for the ISSA call for two detectors in the open area of the module and detectors in racks that have both cooling air flow and electrical power. Due to the complete absence of data concerning the nature of particulate and radiant emission from low-g fires, all three of these detector systems were designed based upon 1-g test data. As planned mission durations and complexity increase and the volume of spacecraft increases, the need for and importance of effective, crew independent, fire detection grows significantly. This requires more knowledge concerning low-gravity fires and how they might be detected. To date, no combustion-generated particulate samples have been collected for well-developed microgravity flames. All of the extant data come from drop tower tests and therefore only correspond to the early stages of a fire. The fuel sources were restricted to laminar gas-jet diffusion flames and rapidly overheated wire insulation. These gas-jet drop tower tests indicate, through thermophoretic sampling, that soot primaries and aggregates (groups of primary particles) in micro-g may be significantly larger than those in normal-g (ng). This raises new scientific questions about soot processes as well as practical issues for particulate detection/alarm threshold levels used in on-orbit smoke detectors. Furthermore, it is widely speculated but unverified that the aggregates will grow to very large scales in a microgravity fire of longer duration than available on the ground. Preliminary tests in the 2.2 second drop tower suggest that particulate generated by overheated wire insulation will also be larger in microgravity than in normal gravity. TEM grids downstream of the fire region in the WIF experiment as well as visual observation of long string-like aggregates, further confirm this suggestion. The combined impact of these limited results and theoretical predictions is that direct knowledge of low-g combustion particulate as opposed to extrapolation from 1-g data is needed for a more confident design of smoke detectors for spacecraft.

Urban, David L.↗

Extended chondrule formation intervals in distinct physicochemical environments: Evidence from Al-Mg isotope systematics of CR chondrite chondrules with unaltered plagioclase

Al-Mg isotope systematics of twelve FeO-poor (type I) chondrules from CR chondrites Queen Alexandra Range 99177 and Meteorite Hills 00426 were investigated by secondary ion mass spectrometry (SIMS). Five chondrules with Mg#’s of 99.0 to 99.2 and Δ 17 O of -4.2‰ to -5.3‰ have resolvable excess 26 Mg. Their inferred ( 26 Al/ 27 Al) 0 values range from (3.5 ± 1.3) × 10 -6 to (6.0 ± 3.9) × 10 -6 . This corresponds to formation times of 2.2 (–0.5/+1.1) Myr to 2.8 (-0.3/+0.5) Myr after CAIs, using a canonical ( 26 Al/ 27 Al) 0 of 5.23 × 10 -5 , and assuming homogeneously distributed 26Al that yielded a uniform initial 26 Al/ 27 Al in the Solar System. Seven chondrules lack resolvable excess 26 Mg. They have lower Mg#’s (94.2 to 98.7) and generally higher Δ 17 O (-0.9‰ to -4.9‰) than chondrules with resolvable excess 26 Mg. Their inferred ( 26 Al/ 27 Al) 0 upper limits range from 1.3 × 10 -6 to 3.2 × 10 -6 , corresponding to formation >2.9 to >3.7 Myr after CAIs. Al-Mg isochrons depend critically on chondrule plagioclase, and several characteristics indicate the chondrule plagioclase is unaltered: (1) SIMS 27 Al/ 24 Mg depth profile patterns match those from anorthite standards, and SEM/EDS of chondrule SIMS pits show no foreign inclusions; (2) transmission electron microscopy (TEM) reveals no nanometer-scale micro-inclusions and no alteration due to thermal metamorphism; (3) oxygen isotopes of chondrule plagioclase match those of coexisting olivine and pyroxene, indicating a low extent of thermal metamorphism; and (4) electron microprobe data show chondrule plagioclase is anorthite-rich, with excess structural silica and high MgO, consistent with such plagioclase from other petrologic type 3.00-3.05 chondrites. We conclude that the resolvable ( 26 Al/ 27 Al) 0 variabilities among chondrules studied are robust, corresponding to a formation interval of at least 1.1 Myr.

79 ASTRONOMY AND ASTROPHYSICS↗

On the microstructure characterization of the AA2098-T351 alloy welded by FSW

Highlights: • The microstructural characterization of the AA2098-T351 Al-Cu-Li alloy welded by FSW was carried out. • There was strong correlation between the results of the various techniques. • DSC was an effective technique for characterization of GP zones complementing the microstructural characterization by TEM. - Abstract: The complex structure of the AA2098-T351 alloy welded by friction stir welding (FSW) was investigated by transmission electron microscopy (TEM), differential scanning calorimetry (DSC) and microhardness measurements. Thermal modelling process of the FSW process was carried out by soldering thermocouples at distances of 6, 9 and 12 mm from the weld centerline, and thermocouple measurements were used as input data into the model. Finite element software COMSOL v5.2 was used for data analysis. The prevailing phases in the base metal (BM) are T1 (Al{sub 2}CuLi) θ′ (Al{sub 2}Cu), δ′/β′(Al{sub 3}(Li,Zr)) and Ω (Al{sub 2}Cu). In the heat affected zone (HAZ), either in the retreating or advancing sides, θ′ phase was not identified. In the thermomechanical affected zone (TMAZ), T1, δ′/β′, GP zones phase were detected in the retreating side, whereas T1 and Guinier-Preston (GP) zones were not observed in the advancing side. This result supports the asymmetric behavior observed in the microhardness profile of the weld. In the stir zone (SZ), GP zones, T1, δ′/β′ (Al{sub 3}(Li,Zr)) and Ω were identified.

36 MATERIALS SCIENCE↗

Water oxidation catalysis via immobilization of the dimanganese complex [Mn 2 (μ-O) 2 Cl(μ-O 2 CCH 3 )(bpy) 2 (H 2 O)](NO 3 ) 2 onto silica

Adsorption of a dinuclear μ -oxo bridged Mn complex onto mesoporous silica was observed when SBA15 was treated with an acetonitrile solution of [Mn 2 ( μ -O) 2 Cl( μ -O 2 CCH 3 )(H 2 O)(bpy) 2 ](NO 3 ) 2 ( 1 ). This complex was immobilized via the displacement of NO 3 - into solution, and characterization by spectroscopic (DRIFTS and DRUV-vis) and magnetic data indicates that the intact dication is electrostatically bound to the silica surface. Loadings of up to 4.1% by weight of [Mn 2 ( μ -O) 2 Cl( μ -O 2 CCH 3 )(H 2 O)(bpy) 2 ] 2+ were achieved. TEM images of the grafted material revealed retention of the mesoporous structure of SBA15, and no clusters of manganese greater than ca. 10 nm were observed. The SBA15-supported dimanganese complex functions as a catalyst for the oxidation of H 2 O with (NH 4 ) 2 Ce(NO 3 ) 6 as stoichiometric oxidant. In contrast, homogenous aqueous solutions of 1 do not evolve oxygen upon treatment with (NH 4 ) 2 Ce(NO 3 ) 6 . Labeling studies with H 2 18 O confirm that the oxygen formed in this catalysis is derived from water. Monitoring the O 2 evolution allowed determination of an initial rate for the catalysis (TOF i = 1.1 × 10 -3 s -1 ). Finally, these studies also reveal a first order dependence on manganese surface concentration, and a zero order rate dependence for (NH 4 )Ce(NO 3 ) 6 . Spectroscopic investigations were employed to investigate the difference in activities between dissolved and supported dimanganese complexes.

Rumberger, Evan M. W.↗

Microstructure Stability During Creep of Friction Stir Welded AA2024-T3 Alloy

The poor weldability of the AA2024 aluminum alloy limits its use in industrial applications. Because friction stir welding (FSW) is a non-fusion welding process, it seems to be a promising solution for welding this alloy. In the current study, FSW was applied to butt weld AA2024-T3 aluminum alloy plates. Creep tests were conducted at 250 and at 315 °C on both the parent material and the friction stir welded specimens. The microstructures of the welded and non-welded AA2024-T3 specimens before and after the creep tests were studied and compared. A comprehensive transmission electron microscopy study together with a high-resolution scanning electron microscopy study and energy-dispersive x-ray spectroscopy analysis was conducted to investigate the microstructure stability. The parent material seems to contain two kinds of Cu-rich precipitates—coarse precipitates of a few microns each and uniformly dispersed fine nanosized precipitates. Unlike the parent material, the crept specimens were found to contain the two kinds of precipitates mentioned above together with platelet-like precipitates. In addition, extensive decoration of the grain boundaries with precipitates was clearly observed in the crept specimens. Controlled aging experiments for up to 280 h at the relevant temperatures were conducted on both the parent material and the welded specimens in order to isolate the contribution of exposure to high temperatures to the microstructure changes. TEM study showed the development of dislocation networks into a cellular dislocation structure in the case of the parent metal. Changes in the dislocation structure as a function of the creep strain and the FSW process were recorded. A detailed creep data analysis was conducted, taking into account the instability of the microstructure.

36 MATERIALS SCIENCE↗

Influence of NaCl on shape deformation of polymersomes

Polymersomes frequently appear in the literature as promising candidates for a wide range of applications from targeted drug delivery to nanoreactors. From a cell mimetic point of view, it is important to understand the size and shape changes of the vesicles in the physiological environment since that can influence the drug delivery mechanism. In this work we studied the structural features of polymersomes consisting of poly(ethylene glycol)–poly(dimethylsiloxane)–poly(ethylene glycol) at the nanoscopic length scale in the presence of NaCl, which is a very common molecule in the biotic aqueous environment. Here, we used dynamic light scattering (DLS), cryo-TEM, small angle neutron scattering (SANS) and small angle X-ray scattering (SAXS). We observed transformation of polymersomes from spherical to elongated vesicles at low salt concentration and into multivesicular structures at high salt concentration. Model fitting analysis of SANS data indicated a reduction of vesicle radius up to 47% and from the SAXS data we observed an increase in membrane thickness up to 8% and an increase of the PDMS hydrophobic segment up to 11% indicating stretching of the membrane due to osmotic imbalance. Also, from the increase in the interlamellar repeat distance up to 98% under high salt concentrations, we concluded that the shape and structural changes observed in the polymersomes are a combined result of osmotic pressure change and ion–membrane interactions.

36 MATERIALS SCIENCE↗

Effect of solvothermal synthesis parameters on the crystallite size and atomic structure of cobalt iron oxide nanoparticles

We here investigate how the synthesis method affects the crystallite size and atomic structure of cobalt iron oxide nanoparticles. By using a simple solvothermal method, we first synthesized cobalt ferrite nanoparticles of ca. 2 and 7 nm, characterized by Transmission Electron Microscopy (TEM), Small Angle X-ray scattering (SAXS), X-ray and neutron total scattering. The smallest particle size corresponds to only a few spinel unit cells. Nevertheless, Pair Distribution Function (PDF) analysis of X-ray and neutron total scattering data shows that the atomic structure, even in the smallest nanoparticles, is well described by the spinel structure, although with significant disorder and a contraction of the unit cell parameter. These effects can be explained by the surface oxidation of the small nanoparticles, which is confirmed by X-ray near edge absorption spectroscopy (XANES). Neutron total scattering data and PDF analysis reveal a higher degree of inversion in the spinel structure of the smallest nanoparticles. Neutron total scattering data also allow magnetic PDF (mPDF) analysis, which shows that the ferrimagnetic domains correspond to ca. 80% of the crystallite size in the larger particles. A similar but less well-defined magnetic ordering was observed for the smallest nanoparticles. Finally, we used a co-precipitation synthesis method at room temperature to synthesize ferrite nanoparticles similar in size to the smallest crystallites synthesized by the solvothermal method. Structural analysis with PDF demonstrates that the ferrite nanoparticles synthesized via this method exhibit a significantly more defective structure compared to those synthesized via a solvothermal method.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

A combined TEM and SAXS study of the growth and self-assembly of ultrathin Pt nanowires

Ultrathin Pt nanowires possess high activity for various electrocatalytic applications. However, little work has focused on understanding their growth mechanisms. Herein, we utilize a combination of time-dependent, ex situ transmission electron microscopy (TEM) and small angle x-ray scattering (SAXS) techniques to observe the growth process in addition to associated surfactant-based interactions. TEM images indicate that initially nanoparticles are formed within 30 s; these small 'seed' particles quickly elongate to form ultrathin nanowires after 2 min. These motifs remain relatively unchanged in size and shape up to 480 min of reaction. Complementary SAXS data suggests that the initial nanoparticles, which are coated by a surfactant bilayer, arrange into a bcc superlattice. With increasing reaction time, the bcc lattice disappears as the nanoparticles grow into nanowires, which then self-assemble into a columnar hexagonal structure in which the individual nanowires are covered by a CTAB monolayer. The hexagonal structure eventually degrades, thereby leading to the formation of lamellar stacking phases comprised of surfactant bilayers. To the best of our knowledge, this is the first time that SAXS has been used to monitor the growth and self-assembly of Pt nanowires. In conclusion, these insights can be used to better understand and rationally control the formation of anisotropic motifs of other metallic nanostructures.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Data for Magnetic Anisotropy due to Localized Structural Defects in Strained Yttrium Iron Garnet Thin Films

This dataset contains electron microscopy, magnetic, and X-ray diffraction characterization data for YIG/YSGG thin films associated with the manuscript "Magnetic anisotropy due to localized structural defects in strained yttrium iron garnet thin films". Characterizations include: scanning electron nano diffraction (SEND, or 4D-STEM), dark field transmission electron microscopy (DF-TEM), energy dispersive X-ray spectroscopy (EDS), ferrimagnetic resonance (FMR), superconducting quantum interference device (SQUID), scanning transmission electron microscopy (STEM), X-ray diffraction (XRD).

Electron microscopy↗

Transmission Electron Microscopy of Itokawa Regolith Grains

Introduction: In a remarkable engineering achievement, the JAXA space agency successfully recovered the Hayabusa space-craft in June 2010, following a non-optimal encounter and sur-face sampling mission to asteroid 25143 Itokawa. These are the first direct samples ever obtained and returned from the surface of an asteroid. The Hayabusa samples thus present a special op-portunity to directly investigate the evolution of asteroidal sur-faces, from the development of the regolith to the study of the effects of space weathering. Here we report on our preliminary TEM measurements on two Itokawa samples. Methods: We were allocated particles RA-QD02-0125 and RA-QD02-0211. Both particles were embedded in low viscosity epoxy and thin sections were prepared using ultramicrotomy. High resolution images and electron diffraction data were ob-tained using a JEOL 2500SE 200 kV field-emission scanning-transmission electron microscope. Quantitative maps and anal-yses were obtained using a Thermo thin-window energy-dispersive x-ray (EDX) spectrometer. Results: Both particles are olivine-rich (Fo70) with μm-sized inclusions of FeS and have microstructurally complex rims. Par-ticle RA-QD02-0125 is rounded and has numerous sub-μm grains attached to its surface including FeS, albite, olivine, and rare melt droplets. Solar flare tracks have not been observed, but the particle is surrounded by a continuous ~50 nm thick, stuctur-ally disordered rim that is compositionally similar to the core of the grain. One of the surface adhering grains is pyrrhotite show-ing a S-depleted rim (~8-10 nm thick) with nanophase Fe metal grains (<5 nm) decorating the outermost surface. The pyrrhotite displays a complex superstructure in its core that is absent in the S-depleted rim. Particle RA-QD02-0211 contains solar flare particle tracks (~2x109 cm-2) and shows a structurally disordered rim ~100 nm thick. The track density corresponds to a surface exposure of ~103-104 years based on the track production rate of [1]. The dis-ordered rim is nanocrystalline with minor amorphous material between crystalline domains. Quantitative element maps show the outermost ~10 nm of the disordered rim is Si-rich. Discussion and Conclusions: Both particles record the ef-fects of space weathering processes on Itokawa. Noguchi et al. [2] proposed that the disordered rims they observed on Itokawa particles largely result from solar wind radiation damage and we arrive at a similar conclusion for the two particles we analyzed. The microstructure of the S-depleted layer on the pyrrhotite grain in RA-QD02-0125 is similar to that observed in troilite irradiated with ~1018 4 kV He+ [3, 4]. Prolonged irradiation has also been shown to disorder pyrrhotite such that the superstructure reflec-tions are lost [5].

Keller, Lindsay P.↗

Mechanosynthesis and structural characterization of nanocrystalline Ce{sub 1–x}Y{sub x}O{sub 2–δ} (x=0.1–0.35) solid solutions

A series of nanostructured fluorite-type Ce{sub 1–x}Y{sub x}O{sub 2–δ} (0≤x≤0.35) solid solutions, prepared via high-energy milling of the CeO{sub 2}/Y{sub 2}O{sub 3} mixtures, are investigated by XRD, HR-TEM, EDS and Raman spectroscopy. For the first time, complementary information on both the long-range and short-range structural features of mechanosynthesized Ce{sub 1–x}Y{sub x}O{sub 2–δ}, obtained by Rietveld analysis of XRD data and Raman spectroscopy, is provided. The lattice parameters of the as-prepared solid solutions decrease with increasing yttrium content. Rietveld refinements of the XRD data reveal increase in microstrains in the host ceria lattice as a consequence of yttrium incorporation. Raman spectra are directly affected by the presence of oxygen vacancies; their existence is evidenced by the presence of vibration modes at ~560 and ~600 cm{sup –1}. The detailed spectroscopic investigations enable us to separate extrinsic and intrinsic origin of oxygen vacancies. It is demonstrated that mechanosynthesis can be successfully employed in the one-step preparation of nanocrystalline Ce{sub 1–x}Y{sub x}O{sub 2–δ} solid solutions. - Graphical abstract: Mechanosynthesis of nanocrystalline Ce{sub 1–x}Y{sub x}O{sub 2–δ} (x=0.1–0.35) solid solutions. - Highlights: • One-step mechanosynthesis of nanoscale Ce{sub 1–x}Y{sub x}O{sub 2–δ} (0≤x≤0.35) solid solutions. • Complementary information on the long-range and short-range structural features of mechanosynthesized Ce{sub 1–x}Y{sub x}O{sub 2–δ} is provided. • Structural variations as a response to the yttrium doping. • Separation of extrinsic and intrinsic origin of the induced oxygen vacancies.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Dielectric and ferroelectric properties of Pb{sub 0.88}La{sub 0.12}(Ti{sub 1−x}Mn{sub x}){sub 0.97}O{sub 3} nanoceramics

Graphical abstract: - Highlights: • The nanoceramics of La/Mn modified PbTiO{sub 3} are synthesized by mechano-thermal route. • Materials have been characterized using various experimental methods. • Drastic change in dielectric and electrical properties of PbTiO{sub 3} has been observed. • The high dielectric constant makes the material very promising candidate for DRAM. • The Mn substitution also makes the material useful for piezoelectric devices. - Abstract: The polycrystalline samples of Pb{sub 0.88}La{sub 0.12}(Ti{sub 1−x}Mn{sub x}){sub 0.97}O{sub 3} (x = 0.0, 0.04, 0.07, 0.10) (PLMT) were prepared using a mechano-thermal method. Preliminary structural analysis of the above samples, carried out using X-ray diffraction data, shows tetragonal structure. This study also shows that the basic compound PLT (Pb{sub 0.88}La{sub 0.12}TiO{sub 3}) retains its tetragonal structure even up to 10% of Mn substitution at the Ti-site. The transmission electron micrographs (TEM) of PLMT samples exhibit that materials prepared by the above method are found to be of nano-size. The temperature–frequency dependence of dielectric studies exhibits increase in relative permittivity with rise in Mn-concentration in PLMT, and hence it can make the materials useful for device applications. The temperature dependence of ac conductivity shows presence of different types of charge species. It is also observed that oxygen vacancies play a significant role in the high-temperature conduction-mechanism and dynamics of polarization of the system. Piezoelectric charge coefficient (d{sub 33}) increases with increase in the Mn content in PLMT.

36 MATERIALS SCIENCE↗

Role of Protein-Water Interface in the Stacking Interactions of Granum Thylakoid Membranes—As Revealed by the Effects of Hofmeister Salts

The thylakoid membranes of vascular plants are differentiated into stacked granum and unstacked stroma regions. The formation of grana is triggered by the macrodomain formation of photosystem II and light-harvesting complex II (PSII-LHCII) and thus their lateral segregation from the photosystem I—light-harvesting complex I (PSI-LHCI) super-complexes and the ATP-synthase; which is then stabilized by stacking interactions of the adjacent PSII-LHCII enriched regions of the thylakoid membranes. The self-assembly and dynamics of this highly organized membrane system and the nature of forces acting between the PSII-LHCII macrodomains are not well understood. By using circular dichroism (CD) spectroscopy, small-angle neutron scattering (SANS) and transmission electron microscopy (TEM), we investigated the effects of Hofmeister salts on the organization of pigment-protein complexes and on the ultrastructure of thylakoid membranes. We found that the kosmotropic agent (NH 4 ) 2 SO 4 and the Hofmeister-neutral NaCl, up to 2 M concentrations, hardly affected the macro-organization of the protein complexes and the membrane ultrastructure. In contrast, chaotropic salts, NaClO 4 , and NaSCN destroyed the mesoscopic structures, the multilamellar organization of the thylakoid membranes and the chiral macrodomains of the protein complexes but without noticeably affecting the short-range, pigment-pigment excitonic interactions. Comparison of the concentration- and time-dependences of SANS, TEM and CD parameters revealed the main steps of the disassembly of grana in the presence of chaotropes. It begins with a rapid diminishment of the long-range periodic order of the grana membranes, apparently due to an increased stacking disorder of the thylakoid membranes, as reflected by SANS experiments. SANS measurements also allowed discrimination between the cationic and anionic effects—in stacking and disorder, respectively. This step is followed by a somewhat slower disorganization of the TEM ultrastructure, due to the gradual loss of stacked membrane pairs. Occurring last is the stepwise decrease and disappearance of the long-range chiral order of the protein complexes, the rate of which was faster in LHCII-deficient membranes. These data are interpreted in terms of a theory, from our laboratory, according to which Hofmeister salts primarily affect the hydrophylic-hydrophobic interactions of proteins, and the stroma-exposed regions of the intrinsic membrane proteins, in particular—pointing to the role of protein-water interface in the stacking interactions of granum thylakoid membranes.

59 BASIC BIOLOGICAL SCIENCES↗

Correlations Among Microstructure, Morphology, Chemistry, and Isotopic Systematics of Hibonite in CM Chondrites

Introduction: Hibonite is a primary refractory phase occurring in many CAIs, typically with spinel and perovskite. Our microstructural studies of CAIs from carbonaceous chondrites reveal a range of stacking defect densities and correlated non-stoichiometry in hibonite. We also conducted a series of annealing experiments, demonstrating that the Mg-Al substitution stabilized the formation of defect-structured hibonite. Here, we continue a detailed TEM analysis of hibonite-bearing inclusions from CM chondrites that have been well-characterized isotopically. We examine possible correlations of microstructure, morphology, mineralogy, and chemical and isotopic systematics of CM hibonites in order to better understand the formation history of hibonite in the early solar nebula. Methods: Fifteen hibonite-bearing inclusions from the Paris CM chondrite were analyzed using a JEOL 7600F SEM and a JEOL 8530F electron microprobe. In addition to three hibonite-bearing inclusions from the Murchison CM chondrite previously reported, we selected three inclusions from Paris, Pmt1-6, 1-9, and 1-10, representing a range of 26Al/27Al ratios and minor element concentrations for a detailed TEM study. We extracted TEM sections from hibonite grains using a FEI Quanta 3D field emission gun SEM/FIB. The sections were then examined using a JEOL 2500SE field-emission scanning TEM equipped with a Thermo-Noran thin window EDX spectrometer. Results and Discussion: A total of six hibonite-bearing inclusions, including two platy hibonite crystals (PLACs) and four spinel-hibonite inclusions (SHIBs), were studied. There are notable differences in chemical and isotopic compositions between the inclusions (Table 1), indicative of their different formation environment or timing. Our TEM observations show perfectly-ordered, stoichiometric hibonite crystals without stacking defects in two PLACs, 2-7-1 and 2-8-2, and in three SHIBs, Pmt1-6, 1-9, and 1-10. In contrast, SHIB 1-9-5 hibonite grains contain a low density of stacking defects linked to an increase in MgO contents, indicating complex, disordered intergrowths of stoichiometric and MgO-enriched hibonites. From the data collected to date, we find no clear correlation between the microstructures of hibonite and its morphological and mineralogical types that reflect distinct chemical and isotopic systematics [6-8,10]. Interestingly, the presence of no or few stacking defects in hibonite from the PLACs and SHIBs are in contrast to our experimental studies that produced very high densities of stacking defects in hibonite [3-5]. Unlike our experi-ments, electron microprobe data from the PLACs and SHIBs hibonite grains show a strong correlation between (Ti4++Si4+) and Mg2+ cations, suggesting that coupled substitutions of (Ti4++Mg2+) and (Si4++Mg2+) for 2Al3+ inhibit the formation of defect-structured hibonite. However, our experimental studies suggest that kinetics (e.g., cooling rate) or other thermal effects also exert a strong control on the microstructures and chemical compositions of hibonite. In Pmt1-6, elongated perovskite grains present at the hibonite grain boundaries display (121) twinning, indicative of a fast cooling (>50degC/min) after high-temperature events. Therefore, the nebular microstructural characteristics of hibonite, at least in this inclusion, would not have destroyed by subsequent high-temperature annealing. Conclusions: Our TEM observations thus far show no clear correlation in microstructures, morphological and mineralogical characteristics, and chemical and isotopic systematics of hibonites from CM chondrites. The observed variation in stacking defect densities in the hibonites may be controlled by thermal processes in the early solar nebula. A detailed TEM analysis of additional CM hibonite samples is underway to evaluate this hypothesis.

Han, J.↗

Optically Stimulated Luminescence Data Storage (Abstract)

We will develop a tunable pulsed electron source capable of generating variable intensity highly-focused electron pulses at high repetition rates. Specifically, we need to demonstrate a high-speed variable electron gun capable of generating a variable intensity electron pulse containing between 102 and 105 electrons with an accelerating voltage of 1kV focused into a spot size <100nm in diameter at with a pulse rate >10MHz (with path to 300MHz). This combined performance cannot be achieved by commercially available electron sources. The primary technology path selected for this work will be to use a photocathode approach, where an easily modulated UV laser is used to stimulate electron emission. The approach utilizes the advances made in the development of the Dynamic TEM (DTEM), though this project will be simpler in that the pulse intensity is lower and there is no requirement for coherency. Alternate paths, including using a traditional electron beam modulated using a v-shaped slit and electrostatically deflecting the beam to adjust intensity; will also be considered for future capabilities. The electron source will then be used generate optically stimulated luminescence (OSL) in lithium fluoride (LiF) substrates to demonstrate the potential for OSL to serve as a basis technology for next generation data storage systems.

42 ENGINEERING↗

Estimating the Probability of Electrical Short Circuits from Tin Whiskers

To comply with lead-free legislation, many manufacturers have converted from tin-lead to pure tin finishes of electronic components. However, pure tin finishes have a greater propensity to grow tin whiskers than tin-lead finishes. Since tin whiskers present an electrical short circuit hazard in electronic components, simulations have been developed to quantify the risk of said short circuits occurring. Existing risk simulations make the assumption that when a free tin whisker has bridged two adjacent exposed electrical conductors, the result is an electrical short circuit. This conservative assumption is made because shorting is a random event that had an unknown probability associated with it. Note however that due to contact resistance electrical shorts may not occur at lower voltage levels. In our first article we developed an empirical probability model for tin whisker shorting. In this paper, we develop a more comprehensive empirical model using a refined experiment with a larger sample size, in which we studied the effect of varying voltage on the breakdown of the contact resistance which leads to a short circuit. From the resulting data we estimated the probability distribution of an electrical short, as a function of voltage. In addition, the unexpected polycrystalline structure seen in the focused ion beam (FIB) cross section in the first experiment was confirmed in this experiment using transmission electron microscopy (TEM). The FIB was also used to cross section two card guides to facilitate the measurement of the grain size of each card guide's tin plating to determine its finish .

Courey, Karim J.↗

Tin Whisker Electrical Short Circuit Characteristics

Existing risk simulations make the assumption that when a free tin whisker has bridged two adjacent exposed electrical conductors, the result is an electrical short circuit. This conservative assumption is made because shorting is a random event that has an unknown probability associated with it. Note however that due to contact resistance electrical shorts may not occur at lower voltage levels. In our first article we developed an empirical probability model for tin whisker shorting. In this paper, we develop a more comprehensive empirical model using a refined experiment with a larger sample size, in which we studied the effect of varying voltage on the breakdown of the contact resistance which leads to a short circuit. From the resulting data we estimated the probability distribution of an electrical short, as a function of voltage. In addition, the unexpected polycrystalline structure seen in the focused ion beam (FIB) cross section in the first experiment was confirmed in this experiment using transmission electron microscopy (TEM). The FIB was also used to cross section two card guides to facilitate the measurement of the grain size of each card guide's tin plating to determine its finish.

Courey, Karim J.↗

Developing an Empirical Model for Estimating the Probability of Electrical Short Circuits from Tin Whiskers

To comply with lead-free legislation, many manufacturers have converted from tin-lead to pure tin finishes of electronic components. However, pure tin finishes have a greater propensity to grow tin whiskers than tin-lead finishes. Since tin whiskers present an electrical short circuit hazard in electronic components, simulations have been developed to quantify the risk of said short circuits occurring. Existing risk simulations make the assumption that when a free tin whisker has bridged two adjacent exposed electrical conductors, the result is an electrical short circuit. This conservative assumption is made because shorting is a random event that had an unknown probability associated with it. Note however that due to contact resistance electrical shorts may not occur at lower voltage levels. In our first article we developed an empirical probability model for tin whisker shorting. In this paper, we develop a more comprehensive empirical model using a refined experiment with a larger sample size, in which we studied the effect of varying voltage on the breakdown of the contact resistance which leads to a short circuit. From the resulting data we estimated the probability distribution of an electrical short, as a function of voltage. In addition, the unexpected polycrystalline structure seen in the focused ion beam (FIB) cross section in the first experiment was confirmed in this experiment using transmission electron microscopy (TEM). The FIB was also used to cross section two card guides to facilitate the measurement of the grain size of each card guide's tin plating to determine its finish.

Courey, Karim J.↗