Microwave-assisted synthesis of layered basic zinc acetate nanosheets and their thermal decomposition into nanocrystalline ZnO

We have developed a low-cost technique using a conventional microwave oven to grow layered basic zinc acetate (LBZA) nanosheets (NSs) from a zinc acetate, zinc nitrate and HMTA solution in only 2 min. The as-grown crystals and their pyrolytic decomposition into ZnO nanocrystalline NSs are characterized by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), atomic force microscopy (AFM), X-ray diffraction (XRD) and photoluminescence (PL). SEM and AFM measurements show that the LBZA NSs have typical lateral dimensions of 1 to 5 μm and thickness of 20 to 100 nm. Annealing in air from 200°C to 1,000°C results in the formation of ZnO nanocrystalline NSs, with a nanocrystallite size ranging from 16 nm at 200°C to 104 nm at 1,000°C, as determined by SEM. SEM shows evidence of sintering at 600°C. PL shows that the shape of the visible band is greatly affected by the annealing temperature and that the exciton band to defect band intensity ratio is maximum at 400°C and decreases by a factor of 15 after annealing at 600°C. The shape and thickness of the ZnO nanocrystalline NSs are the same as LBZA NSs. This structure provides a high surface-to-volume ratio of interconnected nanoparticles that is favorable for applications requiring high specific area and low resistivity such as gas sensing and dye-sensitized solar cells (DSCs). We show that resistive gas sensors fabricated with the ZnO NSs showed a response of 1.12 and 1.65 to 12.5 ppm and 200 ppm of CO at 350°C in dry air, respectively, and that DSCs also fabricated from the material had an overall efficiency of 1.3%.

PACS

81.07.-b; 62.23.Kn; 61.82.Fk     

Formation Mechanisms of Ti3SnC2 Nanolaminate Carbide Using Fe as Additive

Reactive sintering of 3Ti:Sn:2C and 3Ti:Sn:2C:0.6Fe powder mixtures is studied in the temperature range 510°C–1200°C under argon. It is demonstrated that the recently discovered Ti₃SnC₂ phase is formed, provided that Fe is added to a 3Ti:Sn:2C reactant mixture within the synthesis conditions used. Using dilatometric and X‐Ray diffraction analyses, the formation mechanism of Ti₃SnC₂ is discussed. Results show that at low temperature (about 510°C), tin is consumed to form Fe_xSn_y intermetallics. At high temperature (about 1060°C), tin is newly available to form Ti₃SnC₂ due to the melting of Fe_xSn_y. Then, the intermediate phases, TiC and Ti₂SnC, and/or Ti₅Sn₃, TiC, C, and Ti are dissolved in the (Fe + Sn) liquid phase and Ti₃SnC₂ very likely precipitate from the melt. The second part of the study deals with the optimization of the Fe content in the initial 3Ti:Sn:2C reactant powder mixture to synthesize samples with larger Ti₃SnC₂ content by hot isostatic pressing.     

X‐ray Diffraction Study of the Effect of High‐Temperature Heat Treatment on the Microstructural Stability of Third‐Generation SiC Fibers

Third‐generation SiC fibers [High Nicalon S (HNS) and Tyranno SA3 (Ty–SA3)] were studied by X‐ray diffraction and transmission electron microscopy (TEM) after heat treatments in neutral atmosphere up to 1900°C. The microstructural changes in both materials were determined using a modified Hall–Williamson method introducing an anisotropy parameter taking into account the high density of planar defects. HNS fibers exhibit significant modifications in the coherent diffraction domains (CDD) size, which drastically increases from 24 to 70 nm in the range 1600°C–1900°C. TEM observations support these results. The residual microstrain values decrease from 0.0015 to 0.0005 between 1750°C and 1850°C. Similarly, the anisotropy parameter significantly decreases in the same temperature range. Concerning the Ty–SA3 fibers, no evolution in terms of CDD size and residual microstrain was observed. However, the anisotropy parameter decreases at 1800°C. TEM observations did not show noticeable grain growth. The grain size was found to be larger than the CDD and the planar defects density to decrease at high temperature. In both types of fibers, the CDD sizes are similar for the highest temperature heat treatments.     

Evaluation of the Skin Peptide Defenses of the Oregon Spotted Frog Rana pretiosa Against Infection by the Chytrid Fungus Batrachochytrium dendrobatidis

Population declines due to amphibian chytridiomycosis among selected species of ranid frogs from western North America have been severe, but there is evidence that the Oregon spotted frog, Rana pretiosa Baird and Girard, 1853, displays resistance to the disease. Norepinephrine-stimulated skin secretions were collected from a non-declining population of R. pretiosa that had been exposed to the causative agent Batrachochytrium dendrobatidis. Peptidomic analysis led to identification and isolation, in pure form, of a total of 18 host-defense peptides that were characterized structurally. Brevinin-1PRa, -1PRb, -1PRc, and -1PRd, esculentin-2PRa and -PRb, ranatuerin-2PRa, -2PRb, -2PRc, and -2PRe, temporin-PRb and -PRc were identified in an earlier study of skin secretions of frogs from a different population of R. pretiosa known to be declining. Ranatuerin-2PRf, -2PRg, -2PRh, temporin-PRd, -PRe, and -PRf were not identified in skin secretions from frogs from the declining population, whereas temporin-PRa and ranatuerin-2PRd, present in skin secretions from the declining population, were not detected in the current study. All purified peptides inhibited the growth of B. dendrobatidis zoospores. Peptides of the brevinin-1 and esculentin-2 families displayed the highest potency (minimum inhibitory concentration = 6.25–12.5 μM). The study provides support for the hypothesis that the multiplicity and diversity of the antimicrobial peptide repertoire in R. pretiosa and the high growth-inhibitory potency of certain peptides against B. dendrobatidis are important in conferring a measure of resistance to fatal chytridiomycosis.     

Major Ampullate Spider Silk with Indistinguishable Spidroin Dope Conformations Leads to Different Fiber Molecular Structures

To plentifully benefit from its properties (mechanical, optical, biological) and its potential to manufacture green materials, the structure of spider silk has to be known accurately. To this aim, the major ampullate (MA) silk of Araneus diadematus (AD) and Nephila clavipes (NC) has been compared quantitatively in the liquid and fiber states using Raman spectromicroscopy. The data show that the spidroin conformations of the two dopes are indistinguishable despite their specific amino acid composition. This result suggests that GlyGlyX and GlyProGlyXX amino acid motifs (X = Leu, Glu, Tyr, Ser, etc.) are conformationally equivalent due to the chain flexibility in the aqueous environment. Species-related sequence specificity is expressed more extensively in the fiber: the β-sheet content is lower and width of the orientation distribution of the carbonyl groups is broader for AD (29% and 58°, respectively) as compared to NC (37% and 51°, respectively). β-Sheet content values are close to the proportion of polyalanine segments, suggesting that β-sheet formation is mainly dictated by the spidroin sequence. The extent of molecular alignment seems to be related to the presence of proline (Pro) that may decrease conformational flexibility and inhibit chain extension and alignment upon drawing. It appears that besides the presence of Pro, secondary structure and molecular orientation contribute to the different mechanical properties of MA threads.     

Impact of the surface roughness on the electrical capacitance

A new hybrid approach consists to use the advantages of both systems namely the high geometric aspects of the electrodes of the ultracapacitor and the high dielectric strength of polymer materials used in dielectric capacitors. The surface roughness of the electrodes of the ultracapacitor is manufactured with nano-porous materials; activated carbon and carbon nanotubes (CNTs).Many compositions of both carbonaceous materials are tested with different insulating materials (liquid and solid) to constitute the hybrid capacitor. It appears that the capacitance increases with the carbonaceous composition: An increasing from 15 to 40% is observed as compared to a plane capacitor, it can be twice with a 100 wt% of CNTs content. But, the impregnation of the insulating material in the surface roughness remains the key point of the realization of the hybrid capacitor. The roughness accessibility is a major property to optimize in order to improve the impregnation of the insulating material to increase the electrical capacitance.     

Child pedestrian anthropometry: evaluation of potential impact points during a crash

This paper highlights the potential impact points of a child pedestrian during a crash with the front end of a vehicle. Child anthropometry was defined for ages between 3 and 15 years. It was based on the measurement of seven different segment body heights (knee, femur, pelvis, shoulder, neck, chin, vertex) performed on about 2,000 French children. For each dimension, the 5^th, 50^th and 95^th percentile values were reported, and the corresponding linear regression lines were given. Then these heights were confronted with three different vehicle shapes, corresponding to a passenger car, a sport utility vehicle and a light truck, to identify impact points. In particular, we show that the thigh is directly hit by the bumper for children above 12 years of age, whereas the head principally impacts the hood. The influence of child anthropometry on the pedestrian trajectory and the comparison with test procedures in regulation are discussed.     

Investigations on high temperature polyimide potentialities for silicon carbide power device passivation

The operation of silicon carbide (SiC) power devices under severe conditions requires the development of thermally, electrically and chemically stable package. Passivation layer provides electrical insulation and environmental protection for the SiC die. As higher junction temperature and higher electric field can be reached within SiC component, consideration must be given to the thermal stability of the dielectric properties of the material in the die surrounding. Due to their supposed high operating temperature and dielectric strength, spin coated polyimide materials appear as a possible candidate for such passivation and insulation purposes. In this paper, we study the potentialities of a high temperature polyimide from HD Microsystems, for SiC power device passivation, at temperature up to 300 °C.