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Sample records for pillars thermal spectroscopic

  1. Pillar Structured Thermal Neutron Detector

    SciTech Connect

    Nikolic, R; Conway, A; Reinhardt, C; Graff, R; Wang, T; Deo, N; Cheung, C

    2008-06-10

    This work describes an innovative solid state device structure that leverages advanced semiconductor fabrication technology to produce an efficient device for thermal neutron detection which we have coined the 'Pillar Detector'. State-of-the-art thermal neutron detectors have shortcomings in simultaneously achieving high efficiency, low operating voltage while maintaining adequate fieldability performance. By using a three dimensional silicon PIN diode pillar array filled with isotopic {sup 10}boron ({sup 10}B), a high efficiency device is theoretically possible. Here we review the design considerations for going from a 2-D to 3-D device and discuss the materials trade-offs. The relationship between the geometrical features and efficiency within our 3-D device is investigated by Monte Carlo radiation transport method coupled with finite element drift-diffusion carrier transport simulations. To benchmark our simulations and validate the predicted efficiency scaling, experimental results of a prototype device are illustrated. The fabricated pillar structures reported in this work are composed of 2 {micro}m diameter silicon pillars with a 2 {micro}m spacing and pillar height of 12 {micro}m. The pillar detector with a 12 {micro}m height achieved a thermal neutron detection efficiency of 7.3% at a reverse bias of -2 V.

  2. Fabrication of Pillar-Structured Thermal Neutron Detectors

    SciTech Connect

    Nikolic, R J; Conway, A M; Reinhardt, C E; Graff, R T; Wang, T F; Deo, N; Cheung, C L

    2007-11-19

    Pillar detector is an innovative solid state device structure that leverages advanced semiconductor fabrication technology to produce a device for thermal neutron detection. State-of-the-art thermal neutron detectors have shortcomings in achieving simultaneously high efficiency, low operating voltage while maintaining adequate fieldability performance. By using a 3-dimensional silicon PIN diode pillar array filled with isotopic boron 10, ({sup 10}B) a high efficiency device is theoretically possible. The fabricated pillar structures reported in this work are composed of 2 {micro}m diameter silicon pillars with a 4 {micro}m pitch and pillar heights of 6 and 12 {micro}m. The pillar detector with a 12 {micro}m height achieved a thermal neutron detection efficiency of 7.3% at 2V.

  3. Thermal simulation of flexible LED package enhanced with copper pillars

    NASA Astrophysics Data System (ADS)

    Yang, Liu; Leung, Stanley Y. Y.; Wong, Cell K. Y.; Yuan, Cadmus A.; Guoqi, Zhang; Fenglian, Sun

    2015-06-01

    Chip on flexible substrate (COF) is a new packaging technology for light emitting diodes (LED). This paper investigated the effect of Cu-pillar in the polyimide (PI) layer on the thermal properties of COF LED packages by finite element analysis. The thermal distribution and thermal resistance were studied in both COF LED packages with and without Cu-pillar. The PI layer showed the highest thermal resistance in the typical package and led to a high chip temperature. With the addition of Cu-pillars, however, the thermal resistance of the PI layer significantly decreased due to the improvement of vertical thermal dissipation under LED chips. Based on the results of simulation and calculation, the relationship between the amount of Cu-pillar and thermal resistance of the COF package has been built. For the packages studied in this research, an 8 × 8 Cu-pillars array was adequate to improve the thermal performance of COF packages. Project supported by the Research and Scientific Foundation of Heilongjiang Education Department (No. 12541112).

  4. Gamma discrimination in pillar structured thermal neutron detectors

    NASA Astrophysics Data System (ADS)

    Shao, Q.; Radev, R. P.; Conway, A. M.; Voss, L. F.; Wang, T. F.; Nikolić, R. J.; Deo, N.; Cheung, C. L.

    2012-06-01

    Solid-state thermal neutron detectors are desired to replace 3He tube based technology for the detection of special nuclear materials. 3He tubes have some issues with stability, sensitivity to microphonics and very recently, a shortage of 3He. There are numerous solid-state approaches being investigated that utilize various architectures and material combinations. By using the combination of high-aspect-ratio silicon PIN pillars, which are 2 μm wide with a 2 μm separation, arranged in a square matrix, and surrounded by 10B, the neutron converter material, a high efficiency thermal neutron detector is possible. Besides intrinsic neutron detection efficiency, neutron to gamma discrimination is an important figure of merit for unambiguous signal identification. In this work, theoretical calculations and experimental measurements are conducted to determine the effect of structure design of pillar structured thermal neutron detectors including: intrinsic layer thickness, pillar height, substrate doping and incident gamma energy on neutron to gamma discrimination.

  5. Gamma discrimination in pillar structured thermal neutron detectors

    SciTech Connect

    Shao, Q; Radev, R P; Conway, A M; Voss, L F; Wang, T F; Nikolic, R J; Deo, N; Cheung, C L

    2012-03-26

    Solid-state thermal neutron detectors are desired to replace {sup 3}He tube based technology for the detection of special nuclear materials. {sup 3}He tubes have some issues with stability, sensitivity to microphonics and very recently, a shortage of {sup 3}He. There are numerous solid-state approaches being investigated that utilize various architectures and material combinations. By using the combination of high-aspect-ratio silicon PIN pillars, which are 2 {micro}m wide with a 2 {micro}m separation, arranged in a square matrix, and surrounded by {sup 10}B, the neutron converter material, a high efficiency thermal neutron detector is possible. Besides intrinsic neutron detection efficiency, neutron to gamma discrimination is an important figure of merit for unambiguous signal identification. In this work, theoretical calculations and experimental measurements are conducted to determine the effect of structure design of pillar structured thermal neutron detectors including: intrinsic layer thickness, pillar height, substrate doping and incident gamma energy on neutron to gamma discrimination.

  6. Langevin simulation of thermally activated magnetization reversal in nanoscale pillars

    SciTech Connect

    Brown, Gregory; Novotny, M. A.; Rikvold, Per Arne

    2001-10-01

    Numerical solutions of the Landau-Lifshitz-Gilbert micromagnetic model incorporating thermal fluctuations and dipole-dipole interactions (calculated by the fast multipole method) are presented for systems composed of nanoscale iron pillars of dimension 9nm x 9nm x 150nm. Hysteresis loops generated under sinusoidally varying fields are obtained, while the coercive field is estimated to be 1979{+-}14 Oe using linear field sweeps at T=0 K. Thermal effects are essential to the relaxation of magnetization trapped in a metastable orientation, such as happens after a rapid reversal of an external magnetic field less than the coercive value. The distribution of switching times is compared to a simple analytic theory that describes reversal with nucleation at the ends of the nanomagnets. Results are also presented for arrays of nanomagnets oriented perpendicular to a flat substrate. Even at a separation of 300 nm, where the field from neighboring pillars is only {approx}1 Oe, the interactions have a significant effect on the switching of the magnets.

  7. Numerical Simulations of Pillar Structured Solid State Thermal Neutron Detector Efficiency and Gamma Discrimination

    SciTech Connect

    Conway, A; Wang, T; Deo, N; Cheung, C; Nikolic, R

    2008-06-24

    This work reports numerical simulations of a novel three-dimensionally integrated, {sup 10}boron ({sup 10}B) and silicon p+, intrinsic, n+ (PIN) diode micropillar array for thermal neutron detection. The inter-digitated device structure has a high probability of interaction between the Si PIN pillars and the charged particles (alpha and {sup 7}Li) created from the neutron - {sup 10}B reaction. In this work, the effect of both the 3-D geometry (including pillar diameter, separation and height) and energy loss mechanisms are investigated via simulations to predict the neutron detection efficiency and gamma discrimination of this structure. The simulation results are demonstrated to compare well with the measurement results. This indicates that upon scaling the pillar height, a high efficiency thermal neutron detector is possible.

  8. 6:1 aspect ratio silicon pillar based thermal neutron detector filled with {sup 10}B

    SciTech Connect

    Nikolic, R. J.; Conway, A. M.; Reinhardt, C. E.; Graff, R. T.; Wang, T. F.; Deo, N.; Cheung, C. L.

    2008-09-29

    Current helium-3 tube based thermal neutron detectors have shortcomings in achieving simultaneously high efficiency and low voltage while maintaining adequate fieldability performance. By using a three-dimensional silicon p-i-n diode pillar array filled with boron-10 these constraints can be overcome. The fabricated pillar structured detector reported here is composed of 2 {mu}m diameter silicon pillars with a 4 {mu}m pitch and height of 12 {mu}m. A thermal neutron detection efficiency of 7.3+/-0.6% and a neutron-to-gamma discrimination of 10{sup 5} at 2 V reverse bias were measured for this detector. When scaled to larger aspect ratio, a high efficiency device is possible.

  9. Spectroscopic data for thermal infrared remote sensing

    NASA Technical Reports Server (NTRS)

    Varanasi, P.; Nemtchinov, V.; Li, Z.

    1995-01-01

    There has been extensive world-wide use of chloro-fluoro-carbons (CFC's), especially CFC-11 (CFCl3) and CFC-12 (CF2Cl2), hydro-chloro-fluoro-carbons (HCFC's), HCFC-22 (CHFCl2) in particular, and sulphur hexaflouride (SF6) in numerous many industrial applications. These chemicals possess either a strong ozone-depletion potential or a global-warming potential, or both, and pose a threat to the inhabitability of our planet. Recognition of this fact has led to significant curtailment, if not total banishment, of their use globally. However, as recent satellite observations have shown, decline in their atmospheric concentrations may not be immediate. The marked depletion of ozone which has been observed in recent years at high latitudes has made infrared remote sensing of the atmosphere an activity of high priority. The success of any infrared remote sensing experiment conducted in the atmosphere depends upon the availability of accurate, high-resolution, spectroscopic data that are applicable to that experiment. This paper presents a preliminary phase of a multi-faceted work using a Fourier-transform spectrometer (FTS) which is in progress in our laboratory. The concept of how laboratory-borne measurements can be geared toward obtaining a database that is directly applicable to satellite-borne remote sensing missions is the main thrust of this paper which addresses itself to ongoing or planned international space missions. Spectroscopic data on the unresolvable bands of the above mentioned as well as several other man-made gases and on the individual spectral lines of such naturally present trace gases as CO2, N2O, NH3, and CH4 are presented. There is often significant overlap between the isolated lines of better known bands of the more abundant species and the weaker absorption features identifiable as bands of the currently less abundant CFC's, HCFC's, and SF6.

  10. Experimental verification of the formation mechanism for pillar arrays in nanofilms subject to large thermal gradients.

    PubMed

    McLeod, Euan; Liu, Yu; Troian, Sandra M

    2011-04-29

    The free surface of molten nanofilms is known to undergo spontaneous formation of periodic protrusions when exposed to a large transverse thermal gradient. Early time measurements of the array pitch and growth rate in polymer melts confirm a formation process based on a long wavelength thermocapillary instability and not electrostatic attraction or acoustic phonon driven growth as previously believed. We find excellent agreement with theoretical predictions provided the nanofilm out-of-plane thermal conductivity is several times larger than bulk, an enhancement suggestive of polymer chain alignment. PMID:21635044

  11. Experimental Verification of the Formation Mechanism for Pillar Arrays in Nanofilms Subject to Large Thermal Gradients

    NASA Astrophysics Data System (ADS)

    McLeod, Euan; Liu, Yu; Troian, Sandra M.

    2011-04-01

    The free surface of molten nanofilms is known to undergo spontaneous formation of periodic protrusions when exposed to a large transverse thermal gradient. Early time measurements of the array pitch and growth rate in polymer melts confirm a formation process based on a long wavelength thermocapillary instability and not electrostatic attraction or acoustic phonon driven growth as previously believed. We find excellent agreement with theoretical predictions provided the nanofilm out-of-plane thermal conductivity is several times larger than bulk, an enhancement suggestive of polymer chain alignment.

  12. Mixed-linker solid solutions of functionalized pillared-layer MOFs - adjusting structural flexibility, gas sorption, and thermal responsiveness.

    PubMed

    Schwedler, Inke; Henke, Sebastian; Wharmby, Michael T; Bajpe, Sneha R; Cheetham, Anthony K; Fischer, Roland A

    2016-03-14

    Flexible metal-organic frameworks (MOFs) can undergo fascinating structural transitions triggered by external stimuli, such as adsorption/desorption of specific guest molecules or temperature changes. In this detailed study we investigate the potentials and limitations of tuning framework flexibility systematically by exploiting the powerful concept of mixed-linker solid solutions. We chose the prototypical family of functionalized pillared-layer MOFs of the general type Zn2(fu(1)-bdc)2x(fu(2)-bdc)(2-2x)dabco (with x = 1.00, 0.75, 0.50, 0.25 and 0.00; fu-bdc = 2,5-dialkoxy-1,4-benzenedicarboxylate with varying alkoxy chain length, dabco = 1,4-diazabicyclo[2.2.2]octane) and examined their guest responsive, as well as intrinsic temperature dependent structural flexibility by X-ray diffraction, gas physisorption and calorimetric measurements. The ratio of the different fu-bdc linkers can be adjusted freely, offering opportunity for a targeted design of these functional materials by modulating their key features, such as magnitude of framework contraction upon guest removal, breathing behaviour upon CO2 adsorption/desorption, thermoresponsive phase behaviour, and their general thermal expansivity, by the careful choice of fu-bdc linkers and their combination. PMID:26526973

  13. Thermally switchable adhesions of polystyrene-block-poly(n-isopropylacrylamide) copolymer pillar array mimicking climb attitude of geckos

    NASA Astrophysics Data System (ADS)

    Chen, Jem-Kun; Wang, Jing-Hong; Chang, Jia-Yaw; Fan, Shih-Kang

    2012-09-01

    Inspired by the gecko foot pad, we fabricated polystyrene-block-poly(N-isopropylacrylamide) (PS-b-PNIPAAm) copolymer pillar array to mimic climbing attitude of a gecko, alternately attach to and detach from a surface. The pillar array structure of the PS segment significantly enhances both of the hydrophilic and hydrophobic property of PNIPAAm segment tips at 25 and 50 °C, respectively, which could generate alternating adhesive forces of approximately 120 and 11 nN. The dramatic change in adhesive and friction force difference at 25 and 50 °C may guide the design of bio-inspired artificial analogues, which could approach gecko's climbing behavior.

  14. Thermal treatment-induced ductile-to-brittle transition of submicron-sized Si pillars fabricated by focused ion beam

    SciTech Connect

    Wang, Yue-cun; Xie, De-gang; Ning, Xiao-hui; Shan, Zhi-wei

    2015-02-23

    Si pillars fabricated by focused ion beam (FIB) had been reported to have a critical size of 310–400 nm, below which their deformation behavior would experience a brittle-to-ductile transition at room temperature. Here, we demonstrated that the size-dependent transition was actually stemmed from the amorphous Si (a-Si) shell introduced during the FIB fabrication process. Once the a-Si shell was crystallized, Si pillars would behave brittle again with their modulus comparable to their bulk counterpart. The analytical model we developed has been proved to be valid in deriving the moduli of crystalline Si core and a-Si shell.

  15. Infrared-spectroscopic nanoimaging with a thermal source.

    PubMed

    Huth, F; Schnell, M; Wittborn, J; Ocelic, N; Hillenbrand, R

    2011-05-01

    Fourier-transform infrared (FTIR) spectroscopy is a widely used analytical tool for chemical identification of inorganic, organic and biomedical materials, as well as for exploring conduction phenomena. Because of the diffraction limit, however, conventional FTIR cannot be applied for nanoscale imaging. Here we demonstrate a novel FTIR system that allows for infrared-spectroscopic nanoimaging of dielectric properties (nano-FTIR). Based on superfocusing of thermal radiation with an infrared antenna, detection of the scattered light, and strong signal enhancement employing an asymmetric FTIR spectrometer, we improve the spatial resolution of conventional infrared spectroscopy by more than two orders of magnitude. By mapping a semiconductor device, we demonstrate spectroscopic identification of silicon oxides and quantification of the free-carrier concentration in doped Si regions with a spatial resolution better than 100  nm. We envisage nano-FTIR becoming a powerful tool for chemical identification of nanomaterials, as well as for quantitative and contact-free measurement of the local free-carrier concentration and mobility in doped nanostructures. PMID:21499314

  16. Thermal, optical and spectroscopic characterizations of borate laser crystals

    SciTech Connect

    Chavoutier, M.; Jubera, V.; Veber, P.; Velazquez, M.; Viraphong, O.; Hejtmanek, J.; Decourt, R.; Debray, J.; Menaert, B.; Segonds, P.; Adamietz, F.; Rodriguez, V.; Manek-Hoenninger, I.; Fargues, A.; Descamps, D.; Garcia, A.

    2011-02-15

    The Yb-content Li{sub 6}Ln(BO{sub 3}){sub 3} (Ln: Gd, Y) solid solution has been investigated. Crystal growth has been successful for several compositions. A 22% molar content of ytterbium ions was determined by chemical analysis (ICP). Physical properties relevant to laser operation like mechanical hardness, thermal expansion and thermal conductivity were measured on single crystals. Optical measurements, including refractive index and low temperature spectroscopy, were also performed. Finally, the effect of the Y/Gd ratio is discussed. -- Graphical abstract: Several solid solutions of a rare earth borate were studied. The figure illustrates one of these single crystals obtained by Czochralski and shows thermal behaviour and absorption spectra at low temperature. Display Omitted Research highlights: {yields} We have grown by Czochralski method five Li{sub 6}Ln(BO{sub 3}){sub 3} (Ln=Y, Gd,Yb) single crystals. {yields} Chemical, physical and spectroscopic characteristics are reported. {yields} Data relevant to laser operation are listed.

  17. Investigation into Spectroscopic Techniques for Thermal Barrier Coating Spall Detection

    NASA Technical Reports Server (NTRS)

    deGroot, Wim; Opila, Beth

    2001-01-01

    Spectroscopic methods are proposed for detection of thermal barrier coating (TBC) spallation from engine hot zone components. These methods include absorption and emission of airborne marker species originally embedded in the TBC bond coat. In this study, candidate marker materials for this application were evaluated. Thermochemical analysis of candidate marker materials combined with additional constraints such as toxicity and uniqueness to engine environment, provided a short list of four potential species: platinum, copper oxide, zinc oxide. and indium. The melting point of indium was considered to be too low for serious consideration. The other three candidate marker materials, platinum, copper oxide, and zinc oxide were placed in a high temperature furnace and emission and absorption properties were measured over a temperature range from 800-1400 C and a spectral range from 250 to 18000 nm. Platinum did not provide the desired response, likely due to the low vapor Pressure of the metallic species and the low absorption of the oxide species. It was also found, however. that platinum caused a broadening of the carbon dioxide absorption at 4300 nm. The nature of this effect is not known. Absorption and emission caused by sodium and potassium impurities in the platinum were found in the platinum tests. Zinc oxide did not provide the desired response, again, most likely due to the low vapor pressure of the metallic species and the low absorption of the oxide species. Copper oxide generated two strongly temperature dependent absorption peaks at 324.8 and 327.4 nm. The melting point of copper oxide was determined to be too low for serious consideration as marker material.

  18. Nanoscale pillar arrays for separations

    DOE PAGESBeta

    Kirchner, Teresa; Strickhouser, Rachel; Hatab, Nahla; Charlton, Jennifer; Kravchenko, Ivan I.; Lavrik, Nickolay V.; Sepaniak, Michael J.

    2015-04-01

    The work presented herein evaluates silicon nano-pillar arrays for use in planar chromatography. Electron beam lithography and metal thermal dewetting protocols were used to create nano-thin layer chromatography platforms. With these fabrication methods we are able to reduce the size of the characteristic features in a separation medium below that used in ultra-thin layer chromatography; i.e. pillar heights are 1-2μm and pillar diameters are typically in the 200- 400nm range. In addition to the intrinsic nanoscale aspects of the systems, it is shown they can be further functionalized with nanoporous layers and traditional stationary phases for chromatography; hence exhibit broad-rangingmore » lab-on-a-chip and point-of-care potential. Because of an inherent high permeability and very small effective mass transfer distance between pillars, chromatographic efficiency can be very high but is enhanced herein by stacking during development and focusing while drying, yielding plate heights in the nm range separated band volumes. Practical separations of fluorescent dyes, fluorescently derivatized amines, and anti-tumor drugs are illustrated.« less

  19. Nanoscale pillar arrays for separations

    SciTech Connect

    Kirchner, Teresa; Strickhouser, Rachel; Hatab, Nahla; Charlton, Jennifer; Kravchenko, Ivan I.; Lavrik, Nickolay V.; Sepaniak, Michael J.

    2015-04-01

    The work presented herein evaluates silicon nano-pillar arrays for use in planar chromatography. Electron beam lithography and metal thermal dewetting protocols were used to create nano-thin layer chromatography platforms. With these fabrication methods we are able to reduce the size of the characteristic features in a separation medium below that used in ultra-thin layer chromatography; i.e. pillar heights are 1-2μm and pillar diameters are typically in the 200- 400nm range. In addition to the intrinsic nanoscale aspects of the systems, it is shown they can be further functionalized with nanoporous layers and traditional stationary phases for chromatography; hence exhibit broad-ranging lab-on-a-chip and point-of-care potential. Because of an inherent high permeability and very small effective mass transfer distance between pillars, chromatographic efficiency can be very high but is enhanced herein by stacking during development and focusing while drying, yielding plate heights in the nm range separated band volumes. Practical separations of fluorescent dyes, fluorescently derivatized amines, and anti-tumor drugs are illustrated.

  20. Thermal, optical and spectroscopic characterizations of borate laser crystals

    NASA Astrophysics Data System (ADS)

    Chavoutier, M.; Jubera, V.; Veber, P.; Velazquez, M.; Viraphong, O.; Hejtmanek, J.; Decourt, R.; Debray, J.; Menaert, B.; Segonds, P.; Adamietz, F.; Rodriguez, V.; Manek-Hönninger, I.; Fargues, A.; Descamps, D.; Garcia, A.

    2011-02-01

    The Yb-content Li 6Ln(BO 3) 3 ( Ln: Gd, Y) solid solution has been investigated. Crystal growth has been successful for several compositions. A 22% molar content of ytterbium ions was determined by chemical analysis (ICP). Physical properties relevant to laser operation like mechanical hardness, thermal expansion and thermal conductivity were measured on single crystals. Optical measurements, including refractive index and low temperature spectroscopy, were also performed. Finally, the effect of the Y/Gd ratio is discussed.

  1. Spectroscopic study of photo and thermal destruction of riboflavin

    NASA Astrophysics Data System (ADS)

    Astanov, Salikh; Sharipov, Mirzo Z.; Fayzullaev, Askar R.; Kurtaliev, Eldar N.; Nizomov, Negmat

    2014-08-01

    Influence of temperature and light irradiation on the spectroscopic properties of aqueous solutions of riboflavin was studied using linear dichroism method, absorption and fluorescence spectroscopy. It was established that in a wide temperature range 290-423 K there is a decline of absorbance and fluorescence ability, which is explained by thermodestruction of riboflavin. It is shown that the proportion of molecules, which have undergone degradation, are in the range of 4-28%, and depends on the concentration and quantity of temperature effects. Introduction of hydrochloric and sulfuric acids, as well as different metal ions leads to an increase in the photostability of riboflavin solutions by 2-2.5 times. The observed phenomena are explained by the formation protonation form of riboflavin and a complex between the metal ions and oxygen atoms of the carbonyl group of riboflavin, respectively.

  2. Spectroscopic, thermal and structural studies on manganous malate crystals

    SciTech Connect

    Thomas, J. Lincy, A. Mahalakshmi, V.; Saban, K. V.

    2013-01-15

    Prismatic crystals of manganous malate have been prepared by controlled ionic diffusion in hydrosilica gel. The structure was elucidated using single crystal X-ray diffraction. The crystals are orthorhombic with space group Pbca. Vibrations of the functional groups were identified by the FTIR spectrum. Thermogravimetric and differential thermal analyses (TG-DTA) were carried out to explore the thermal decomposition pattern of the material. Structural information derived from FTIR and TG-DTA studies is in conformity with the single crystal XRD data.

  3. Analysis of longwall pillar stability

    SciTech Connect

    Mark, C.

    1987-01-01

    This dissertation proposes a new method for longwall pillar design, developed primarily from underground measurements. This dissertation addresses three areas of direct relevance to longwall pillar design: (1) The magnitude, time-of-arrival, and distribution of the abutment loads applied to longwall pillars; (2) The strength and behavior of coal pillars; (3) The relationship between pillar sizing and entry stability, and other factors affecting the roof/pillar/floor interaction during longwall mining. The research focused on two field studies performed in adjacent longwall panels at a West Virginia coal mine. In each study, measurements of pillar stress, pillar deformation, and entry stability were obtained during and after the approach of the longwall face. Other research included detailed reanalyses of field data from other studies, an in-depth comparative study of available longwall pillar design methods, numerical modeling to determine post-development longwall pillar loads, and an evaluation of two index tests used to determine coal strength. The proposed longwall pillar design method incorporates a new approach to estimating abutment loads hat was developed from the research. The method also employs existing empirical pillar strength formulas that were shown to be applicable to longwall pillars. The proposed design method represents an improvement over the existing methods, because it can be used with designs employing combinations of differently sized pillars, and because it can calculate stability factors for the several different service functions of pillars around a longwall.

  4. Thermal decomposition and vibrational spectroscopic aspects of pyridinium hexafluorophosphate (C5H5NHPF6)

    NASA Astrophysics Data System (ADS)

    Lekgoathi, M. D. S.; Kock, L. D.

    2016-12-01

    Thermal decomposition and vibrational spectroscopic properties of pyridinium hexafluorophosphate (C5H5NHPF6) have been studied. The structure of the compound is better interpreted as having a cubic space group, based on Raman and infrared vibrational spectroscopy experiments and group theoretical correlation data between site symmetry species and the spectroscopic space group. The 13C NMR data shows three significant signals corresponding to the three chemical environments expected on the pyridinium ring i.e. γ, β and α carbons, suggesting that the position of the anion must be symmetrical with respect to the pyridinium ring's C2v symmetry. The process of thermal decomposition of the compound using TGA methods was found to follow a contracting volume model. The activation energy associated with the thermal decomposition reaction of the compound is 108.5 kJ mol-1, while the pre exponential factor is 1.51 × 109 sec-1.

  5. Short-Term and Long-Term Variability of Antenna Position Due to Thermal Bending of Pillar Monument at Permanent GNSS Station

    NASA Astrophysics Data System (ADS)

    Gerhatova, Lubomira; Hefty, Jan; Spanik, Peter

    2016-06-01

    The variability of daily site coordinates at permanent GNSS station is a sum of many disturbing factors influencing the actual satellite observations, data processing, and bias modelling. In the paper are analysed possibilities of monitoring the instability of GNSS antenna pillar monument by the independent observations using the precise inclination sensor. Long-term series from three different types of pillars show specific features in amplitude and temporal evolution of monument bending. Correlations with daily temperature and/or solar radiation changes were proved.

  6. Naphthene upgrading with pillared synthetic clay catalysts

    SciTech Connect

    Sharma, R.K.; Olson, E.S.

    1995-12-31

    Catalytic hydrotreatment of methylcyclohexane was investigated to model upgrading of coal-derived naphthenes. Nickel-substituted synthetic mica montmorillonite (NiSMM), alumina-pillared NiSMM, and zirconia-pillared NiSMM were prepared and tested for hydrocracking and hydroisomerization of mediylcyclohexane. Infrared and thermal desorption studies of the pyridine-adsorbed catalysts indicated the presence of Lewis as well as Bronsted acid sites. Total acidity and surface area increased with pillaring of NiSMM with polyoxy aluminum and polyoxy zirconium cations. Most of the products were branched alkanes (isoparaffins). These compositions are highly desirable for environmentally acceptable transportation fuels. Furthermore, dehydrogenation was not a major pathway, as indicated by the minimal formation of aromatic hydrocarbons, coke, or other oligomeric materials. This paper describes the effect of various operating conditions, which included reaction temperature, contact time, hydrogen pressure, and catalyst on the product distribution.

  7. Zinc acetylacetonate hydrate adducted with nitrogen donor ligands: Synthesis, spectroscopic characterization, and thermal analysis

    NASA Astrophysics Data System (ADS)

    Brahma, Sanjaya; Shivashankar, S. A.

    2015-12-01

    We report synthesis, spectroscopic characterization, and thermal analysis of zinc acetylacetonate complex adducted by nitrogen donor ligands, such as pyridine, bipyridine, and phenanthroline. The pyridine adducted complex crystallizes to monoclinic crystal structure, whereas other two adducted complexes have orthorhombic structure. Addition of nitrogen donor ligands enhances the thermal property of these complexes as that with parent metal-organic complex. Zinc acetylacetonate adducted with pyridine shows much higher volatility (106 °C), decomposition temperature (202 °C) as that with zinc acetylacetonate (136 °C, 220 °C), and other adducted complexes. All the adducted complexes are thermally stable, highly volatile and are considered to be suitable precursors for metal organic chemical vapor deposition. The formation of these complexes is confirmed by powder X-ray diffraction, Fourier transform infrared spectroscopy, mass spectroscopy, and elemental analysis. The complexes are widely used as starting precursor materials for the synthesis of ZnO nanostructures by microwave irradiation assisted coating process.

  8. Thermal Physical, and Infrared Spectroscopic Studies on Glasses Prepared by Microwave Route

    SciTech Connect

    Jagadeesha, N.; Gowda, V. C. Veeranna; Chakradhar, R. P. S.; Reddy, C. Narayana

    2011-07-15

    This paper describes thermal, physical and spectroscopic properties of glasses prepared by a novel micro wave method. These studies exhibited a strong compositional dependent trend and existence of characteristic boro-vanadate groups in these glasses. The scheme of modification of borate and vanadate groups is controlled by Sanderson's electronegativity principle. Analysis of density and glass transition temperatures suggests the presence of characteristic four coordinated borate and diboro - vanadate groups in these glasses. The presence of [BO{sub 4/2}]{sup -} and [B{sub 2}V{sub 2}O{sub 9}]{sup 2-}) groups are confirmed by Infrared Spectroscopy of investigated glasses.

  9. Simultaneous microscopic measurements of thermal and spectroscopic fields of a phase change material

    NASA Astrophysics Data System (ADS)

    Romano, M.; Ryu, M.; Morikawa, J.; Batsale, J. C.; Pradere, C.

    2016-05-01

    In this paper, simultaneous microscopic measurements of thermal and spectroscopic fields of a paraffin wax n-alkane phase change material are reported. Measurements collected using an original set-up are presented and discussed with emphasis on the ability to perform simultaneous characterization of the system when the proposed imaging process is used. Finally, this work reveals that the infrared wavelength contains two sets of important information. Furthermore, this versatile and flexible technique is well adapted to characterize many systems in which the mass and heat transfers effects are coupled.

  10. Naphthene upgrading with pillared synthetic clay catalysts

    SciTech Connect

    Sharma, R.K.; Olson, E.S.

    1995-12-31

    Catalytic hydrotreatment of methylcyclohexane was investigated to model upgrading of coal-derived naphthenes. Nickel-substituted synthetic mica montmorillonite (NiSMM), alumina-pillared NiSMM and Zirconia-pillared NiSMM were prepared and tested for hydrocracking and hydroisomerization of methylcyclohexane. Infrared and thermal desorption studies of the pyridine-adsorbed catalysts indicated the presence of Lewis and Bronsted acid sites. Total acidity and surface area increased with pillaring of NiSMM with polyoxy aluminum and polyoxy zirconium cations. Methylcyclohexane was reacted with these catalysts under a variety of conditions. Pillared clays gave higher gas yields and higher hydrocracking but lower hydroisomerization activity than nonpillared clay. The majority of the products were branched alkanes (isoparaffinic). These catalysts effectively use hydrogen as indicated by the minimal formation of aromatic hydrocarbons, coke, or other oligomeric materials. The effect of various operating conditions, i.e., reaction temperature, contact time, H{sub 2} pressure, and catalyst, on the product distribution will be described.

  11. FT-IR spectroscopic, thermal analysis of human urinary stones and their characterization

    NASA Astrophysics Data System (ADS)

    Selvaraju, R.; Raja, A.; Thiruppathi, G.

    2015-02-01

    In the present study, FT-IR, XRD, TGA-DTA spectral methods have been used to investigate the chemical compositions of urinary calculi. Multi-components of urinary calculi such as calcium oxalate, hydroxyl apatite, struvite and uric acid have been studied. The chemical compounds are identified by FT-IR spectroscopic technique. The mineral identification was confirmed by powder X-ray diffraction patterns as compared with JCPDS reported values. Thermal analysis techniques are considered the best techniques for the characterization and detection of endothermic and exothermic behaviors of the urinary stones. The percentages of each hydrate (COM and COD) are present together, in the presences of MAPH or UA. Finally, the present study suggests that the Urolithiasis is significant health problem in children, and is very common in some parts of the world, especially in India. So that present study is so useful and helpful to the scientific community for identification of latest human health problems and their remedies using spectroscopic techniques.

  12. Spectroscopic and thermal properties of minerals from density-functional perturbation theory

    NASA Astrophysics Data System (ADS)

    Refson, K.

    2003-12-01

    Ab-initio calculations based on density-functional theory have provento give a highly accurate description of structural and elastic properties of minerals under pressure. To evaluate spectroscopic, dielectric and thermal properties it is necessary to compute the second derivatives of the energy with respect to a displacement or electric field perturbation. While the Hellman-Feynmann theorem makes the computation of forces (first derivatives of the energy) straightforward, second derivatives depend on the linear response of the orbitals and density to the perturbation. I will sketch the variational formulation of density-function perturbation theory, and it's implementation in the CASTEP plane-wave code. The capabilities will be illustrated with calculation of the full phonon dispersion spectra and dielectric properties of a-quartz, ZrO2 and NaHF2.

  13. Stress reduction for pillar filled structures

    DOEpatents

    Nikolic, Rebecca J.; Conway, Adam; Shao, Qinghui; Voss, Lars; Cheung, Chin Li; Dar, Mushtaq A.

    2015-09-01

    According to one embodiment, an apparatus for detecting neutrons includes an array of pillars, wherein each of the pillars comprises a rounded cross sectional shape where the cross section is taken perpendicular to a longitudinal axis of the respective pillar, a cavity region between each of the pillars, and a neutron sensitive material located in each cavity region.

  14. Densification effects of the carbon nanotube pillar array on field-emission properties

    NASA Astrophysics Data System (ADS)

    Wang, Kuang-Yu; Chou, Chia-Hsin; Liao, Chan-Yu; Li, Yu-Ren; Cheng, Huang-Chung

    2016-06-01

    In this study, a simple densification method for carbon nanotube (CNT) pillars is proposed to achieve high-performance field emission characteristics and stable emission. Through capillary force during solution evaporation, the CNT density in each pillar can be increased by about six times without causing damage to the crystallinity of CNTs. The densified CNT pillars exhibit lower series resistance, sharper pillars, better contacts, higher thermal conductivity, and better mechanical stiffness than as-grown ones. Therefore, the threshold field of the field emitter with such CNT pillars of 50 µm height can be reduced to 1.98 V/µm, as compared with 2.2 V/µm for the undensified ones. Moreover, the fluctuation of field-emission current decreases from 15.5 to 9.4% after the stress tests at a field of 2 V/µm for 1800 s. These findings imply that the densified CNT pillars are promising for the field-emission applications.

  15. The effect of refluxing on the alkoxide-based sodium potassium niobate sol-gel system: Thermal and spectroscopic studies

    SciTech Connect

    Chowdhury, Anirban; Bould, Jonathan; Londesborough, Michael G.S.; Milne, Steven J.

    2011-02-15

    A study on the effects of prolonged heating under reflux conditions of up to 70 h on alkoxides of sodium, potassium and niobium dissolved in 2-methoxyethanol for the synthesis of sols of composition Na{sub 0.5}K{sub 0.5}NbO{sub 3} (NKN) has been carried out using combined thermogravimetric-Fourier transform infrared spectroscopic analyses. Extended refluxing increases the homogeneity of the Na{sub 0.5}K{sub 0.5}NbO{sub 3} (NKN) system. Spectroscopic analyses on the non-refluxed and 70 h refluxed NKN gels reveal the existence of inorganic hydrated carbonates and bicarbonates, which we propose arise from the hydration and carbonation of the samples on standing in air. The X-ray diffraction patterns of these two types of gels show orthorhombic NKN phase evolutions at higher temperatures. -- Graphical abstract: Total organic evolution plots over time for NKN dried gels obtained under different refluxing times show different thermochemical behaviours and these were investigated by thermal and spectroscopic analysis tools to find a correlation between the extent of -M-O-M- chain link formation and the amount of solvent vapour (methoxyethanol) evolution. Display Omitted Research highlights: > Prolonged refluxing of sol-gel NKN precursor solutions improves final properties of an NKN system. > An NKN process thermo-chemistry with thermal and spectroscopic analysis tools was explored. > An FTIR of NKN gels reveals tendency of NKN systems for rehydration and recarbonation on standing.

  16. Thermal and Spectroscopic Characterization of a Proton Pumping Rhodopsin from an Extreme Thermophile*

    PubMed Central

    Tsukamoto, Takashi; Inoue, Keiichi; Kandori, Hideki; Sudo, Yuki

    2013-01-01

    So far retinylidene proteins (∼rhodopsin) have not been discovered in thermophilic organisms. In this study we investigated and characterized a microbial rhodopsin derived from the extreme thermophilic bacterium Thermus thermophilus, which lives in a hot spring at around 75 °C. The gene for the retinylidene protein, named thermophilic rhodopsin (TR), was chemically synthesized with codon optimization. The codon optimized TR protein was functionally expressed in the cell membranes of Escherichia coli cells and showed active proton transport upon photoillumination. Spectroscopic measurements revealed that the purified TR bound only all-trans-retinal as a chromophore and showed an absorption maximum at 530 nm. In addition, TR exhibited both photocycle kinetics and pH-dependent absorption changes, which are characteristic of rhodopsins. Of note, time-dependent thermal denaturation experiments revealed that TR maintained its absorption even at 75 °C, and the denaturation rate constant of TR was much lower than those of other proton pumping rhodopsins such as archaerhodopsin-3 (200 ×), Haloquadratum walsbyi bacteriorhodopsin (by 10-times), and Gloeobacter rhodopsin (100 ×). Thus, these results suggest that microbial rhodopsins are also distributed among thermophilic organisms and have high stability. TR should allow the investigation of the molecular mechanisms of ion transport and protein folding. PMID:23740255

  17. Pillar cuvettes: capillary-filled, microliter quartz cuvettes with microscale path lengths for optical spectroscopy.

    PubMed

    Holzner, Gregor; Kriel, Frederik Hermanus; Priest, Craig

    2015-05-01

    The goal of most analytical techniques is to reduce the lower limit of detection; however, it is sometimes necessary to do the opposite. High sample concentrations or samples with high molar absorptivity (e.g., dyes and metal complexes) often require multiple dilution steps or laborious sample preparation prior to spectroscopic analysis. Here, we demonstrate dilution-free, one-step UV-vis spectroscopic analysis of high concentrations of platinum(IV) hexachloride in a micropillar array, that is, "pillar cuvette". The cuvette is spontaneously filled by wicking of the liquid sample into the micropillar array. The pillar height (thus, the film thickness) defines the optical path length, which was reduced to between 10 and 20 μm in this study (3 orders of magnitude smaller than in a typical cuvette). Only one small droplet (∼2 μL) of sample is required, and the dispensed volume need not be precise or even known to the analyst for accurate spectroscopy measurements. For opaque pillars, we show that absorbance is linearly related to platinum concentration (the Beer-Lambert Law). For fully transparent or semitransparent pillars, the measured absorbance was successfully corrected for the fractional surface coverage of the pillars and the transmittance of the pillars and reference. Thus, both opaque and transparent pillars can be applied to absorbance spectroscopy of high absorptivity, microliter samples. It is also shown here that the pillar array has a useful secondary function as an integrated (in-cuvette) filter for particulates. For pillar cuvette measurements of platinum solutions spiked with 6 μm diameter polystyrene spheres, filtered and unfiltered samples gave identical spectra. PMID:25844800

  18. THERMAL AND SPECTROSCOPIC ANALYSES OF CAUSTIC SIDE SOLVENT EXTRACTION SOLVENT CONTACTED WITH 1 MOLARAND 3 MOLAR NITRIC ACID

    SciTech Connect

    Fondeur, F; David Hobbs, D; Samuel Fink, S

    2007-07-23

    Thermal and spectroscopic analyses were performed on multiple layers formed from contacting Caustic Side Solvent Extraction (CSSX) solvent with 1 M or 3 M nitric acid. A slow chemical reaction occurs (i.e., over several weeks) between the solvent and 1 M or 3 M nitric acid as evidenced by color changes and the detection of nitro groups in the infrared spectrum of the aged samples. Thermal analysis revealed that decomposition of the resulting mixture does not meet the definition of explosive or deflagrating material.

  19. THERMAL AND SPECTROSCOPIC ANALYSES OF CAUSTIC LIDE SOLVENT EXTRACTION SOLVENT CONTACTED WITH 16 MOLAR AND 8 MOLAR NITRIC ACID

    SciTech Connect

    Fondeur, F; David Hobbs, D; Samuel Fink, S

    2007-07-12

    Thermal and spectroscopic analyses were performed on multiple layers formed from contacting Caustic Side Solvent Extraction (CSSX) solvent with 1 M or 3 M nitric acid. A slow chemical reaction occurs (i.e., over several weeks) between the solvent and 1 M or 3 M nitric acid as evidenced by color changes and the detection of nitro groups in the infrared spectrum of the aged samples. Thermal analysis revealed that decomposition of the resulting mixture does not meet the definition of explosive or deflagrating material.

  20. Thermal treatment effects imposed on solid DNA cationic lipid complex with hexadecyltrimethylammonium chloride, observed by variable angle spectroscopic ellipsometry

    SciTech Connect

    Nizioł, Jacek

    2014-12-21

    DNA cationic lipid complexes are materials of properties required for applications in organic electronics and optoelectronics. Often, their thermal stability demonstrated by thermogravimetry is cited in the literature as important issue. However, little is known about processes occurring in heated solid DNA cationic lipid complexes. In frame of this work, thin films of Deoxyribonucleic acid-hexadecyltrimethylammonium chloride (DNA-CTMA) were deposited on silicon wafers. Samples were thermally annealed, and simultaneously, their optical functions were measured by spectroscopic ellipsometry. At lower temperatures, thermal expansion coefficient of solid DNA-CTMA was negative, but at higher temperatures positive. Thermally induced modification of absorption spectrum in UV-vis was observed. It occurred at a range of temperatures higher than this of DNA denaturation in solution. The observed phenomenon was irreversible, at least in time scale of the experiment (one day)

  1. Six Pillars of Organic Chemistry

    ERIC Educational Resources Information Center

    Mullins, Joseph J.

    2008-01-01

    This article describes an approach to teaching organic chemistry, which is to have students build their knowledge of organic chemistry upon a strong foundation of the fundamental concepts of the subject. Specifically, the article focuses upon a core set of concepts that I call "the six pillars of organic chemistry": electronegativity, polar…

  2. Six Pillars of Dynamic Schools

    ERIC Educational Resources Information Center

    Edwards, Steven W.; Chapman, Paul E.

    2009-01-01

    "Six Pillars of Dynamic Schools" uncovers an often overlooked truth--effective change is the product of hard work and dedication. There is no silver bullet; no matter how many programs, software packages, or new initiatives a district uses, the magic won't just "happen." Dynamic schools result from consistent and redundant focus on the fundamental…

  3. Fluorine-mediated acidity of alumina-pillared fluorohectorite

    SciTech Connect

    Butruille, J.R.; Pinnavaia, T.J. ); Michot, L.J.; Barres, O. )

    1993-02-01

    Structural fluorine atoms in the 2:1 layered silicate framework of fluorohectorite have a profound effect on the acidity of alumina-pillared derivatives prepared by intercalation of Al[sub 13] polycations and subsequent calcination at elevated temperatures. The alumina-pillared clay formed by calcination at 350[degrees]C exhibits greatly enhanced catalytic activity for propylene alkylation of biphenyl, relative to nonfluorinated smectite hosts. However, calcination of the Al[sub 13] intercalate at 500[degrees]C results in a relatively inactive clay with greatly diminished NH[sub 3] and pyridine chemisorption properties. The effect of the calcination process on the clay layer structure was carefully studied by [sup 27]Al, [sup 29]Si, and [sup 19]F MAS-NMR and FTIR spectroscopic methods and by mass spectrometric analysis of volatile by-products. It was shown that between 30 and 500[degrees]C, specific lattice fluorine atoms adjacent to charged sites in the octahedral sheet of the layers are replaced by hydroxyl groups. At calcination temperatures below 350[degrees]C the Broensted acidity of protonated hydroxyl groups in the layers is enhanced by the electron-withdrawing effect of near-neighbor fluorine atoms at neutral sites in the octahedral sheet. A mechanism for fluorine hydrolysis is proposed in which gallery water molecules, formed by the dehydroxylation of the alumina pillars, migrate to hexagonal oxygen cavities above the reactive fluorine positions. Between 350 and 500[degrees]C, a second process occurs that causes dehydroxylation of the layers, and this results in a sharp decrease in the acidity and catalytic activity of the pillared clay. The relationships between structure and reactivity suggest that the acid-catalytic activity of an alumina-pillared clay can be mediated by controlling the relative amounts of hydroxyl groups at charged octahedral sites and fluorine atoms at neutral octahedral sites in the host clay. 22 refs., 13 figs., 3 tabs.

  4. Characterization of AlFe-pillared Unye bentonite: A study of the surface acidity and catalytic property

    NASA Astrophysics Data System (ADS)

    Caglar, Bulent; Cubuk, Osman; Demir, Ersin; Coldur, Fatih; Catir, Mustafa; Topcu, Cihan; Tabak, Ahmet

    2015-06-01

    Aluminium-iron-pillared bentonite has been prepared by incorporation of the iron mixed aluminium-polyoxocation into bentonite layers and characterized by the powder X-ray diffraction, Fourier transform infrared, thermal analysis and surface area measurement techniques. The characteristic d001 basal spacing of raw bentonite increased with the pillaring process and reached to 18.05 Å. The siloxane layers of bentonite were perturbed and the positions of Si-O stretching vibrations were altered by pillaring process. However, these pillars in the interlayer gallery spacing enhanced the thermal stability of bentonite. The new micropores were formed by the pillaring process and the specific surface area of raw bentonite increased by ca. 2-fold for aluminium-iron-pillared bentonite. FTIR spectra and thermal analysis curves of pyridine adsorbed samples clearly show that the surface Lewis acidity of aluminium-iron-pillared bentonite is greater than that of raw bentonite. Raw and aluminium-iron-pillared bentonites have been utilized as solid catalysts for benzoylation of benzene with benzoyl chloride. The aluminium-iron-pillared bentonite catalyst showed promising catalytic activity whereas raw bentonite showed no catalytic activity in benzoylation of benzene with benzoyl chloride.

  5. Deformation mechanisms in nanoscale single crystalline electroplated copper pillars

    NASA Astrophysics Data System (ADS)

    Jennings, Andrew T.

    Scientific research in nanotechnology has enabled advances in a diverse range of applications, such as: electronics, chemical sensing, and cancer treatment. In order to transition these nanotechnology-driven innovations out of the laboratory and into real-world applications, the resilience and mechanical reliability of nanoscale structures must be well understood in order to preserve functionality under real-world operating environments. Understanding the mechanical properties of nanoscale materials is especially important because several authors have shown that single crystalline metal pillars produced through focused-ion-beam milling have unique properties when the pillar diameter, D, approaches nanotechnology-relevant dimensions. The strength, sigma, of these pillars is size-dependent and is well described through a power-law relation showing that smaller is stronger: sigma∝D-n , where n is the exponent and is found to be 0.5≤n≤1.0 in face-centered-cubic metals. In this work, the fundamental deformation mechanisms governing the size-dependent mechanical properties are investigated through uniaxial compression and tension tests of electroplated single crystalline copper pillars with diameters between 75 nm and 1000 nm. At larger pillar diameters, D >125 nm, these copper pillars are shown to obey a similar size-dependent regime, demonstrating that the "smaller is stronger" phenomenon is a function of the pillar microstructure, as opposed to the fabrication route. Furthermore, the dominant dislocation mechanism in this size-dependent regime is shown to be the result of single-arm, or spiral, sources. At smaller pillar diameters, D≤125 nm, a strain-rate-dependent mechanism transition is observed through both the size-strength relation and also quantitative, experimental measures of the activation volume. This new deformation regime is characterized by a size-independent strength and is governed by surface dislocation nucleation, a thermally activated

  6. All Pillars Point to Eta

    NASA Technical Reports Server (NTRS)

    2005-01-01

    [figure removed for brevity, see original site] [figure removed for brevity, see original site] Eta Carinae Starforming RegionSimulated Infrared View of Comet Tempel 1 (artist's concept)

    These false-color image taken by NASA's Spitzer Space Telescope shows the 'South Pillar' region of the star-forming region called the Carina Nebula. Like cracking open a watermelon and finding its seeds, the infrared telescope 'busted open' this murky cloud to reveal star embryos (yellow or white) tucked inside finger-like pillars of thick dust (pink). Hot gases are green and foreground stars are blue. Not all of the newfound star embryos can be easily spotted.

    Though the nebula's most famous and massive star, Eta Carinae, is too bright to be observed by infrared telescopes, the downward-streaming rays hint at its presence above the picture frame. Ultraviolet radiation and stellar winds from Eta Carinae and its siblings have shredded the cloud to pieces, leaving a mess of tendrils and pillars. This shredding process triggered the birth of the new stars uncovered by Spitzer.

    The inset visible-light picture (figure 2) of the Carina Nebula shows quite a different view. Dust pillars are fewer and appear dark because the dust is soaking up visible light. Spitzer's infrared detectors cut through this dust, allowing it to see the heat from warm, embedded star embryos, as well as deeper, more buried pillars. The visible-light picture is from the National Optical Astronomy Observatory.

    Eta Carina is a behemoth of a star, with more than 100 times the mass of our Sun. It is so massive that it can barely hold itself together. Over the years, it has brightened and faded as material has shot away from its surface. Some astronomers think Eta Carinae might die in a supernova blast within our lifetime.

    Eta Carina's home, the Carina Nebula, is located in the southern portion of our Milky Way galaxy, 10,000 light-years from Earth. This colossal cloud of gas and dust

  7. Influence of PbF2 concentration on thermal, structural and spectroscopic properties of Eu3+-doped lead phosphate glasses

    NASA Astrophysics Data System (ADS)

    Żur, Lidia; Sołtys, Marta; Goryczka, Tomasz; Pisarska, Joanna; Pisarski, Wojciech A.

    2014-10-01

    Effects of PbF2 content on the local structure, thermal and spectroscopic properties of Eu3+ ions in lead phosphate glass systems have been studied. The glass samples, where PbO was partially or totally replaced by PbF2, were examined using X-ray diffraction (XRD), differential scanning calorimetry (DSC) and luminescence spectroscopy. Based on DSC curves, characteristic temperatures and the thermal stability parameters useful for glass fiber drawing were determined. In order to confirm glass structure, XRD measurements were used. Luminescence spectra and their decays were analyzed in details. Especially, the changes of red-to-orange luminescence intensity ratios R/O (Eu3+) and measured lifetimes for 5D0 excited state of Eu3+ are presented and discussed as a function of PbF2 concentration.

  8. Studies of layered and pillared manganese oxide materials

    NASA Astrophysics Data System (ADS)

    Ma, Ying

    Synthetic Birnessite, an octahedral layered manganese oxide material called OL-1 was synthesized with Na+, K+, Na +/Mg2+, K+/Mg2+, Na +/K+ ions as interlayer cations by redox reactions between permanganate and alcohols in a strong basic media. Chromia pillared OL-1s were prepared under reflux conditions using trinuclear chromium hydroxyl acetate as a pillaring agent followed by calcination in a N2 atmosphere at 200°C. Vanadium oxide pillared OL-1s were obtained by intercalating neutral vanadyl acetylacetonate (VOacac) or vanadium acetylacetonate (Vacac) into the interlayer of OL-1 and subsequently calcining in air at 300°C. The synthesis procedures were monitored using X-ray diffraction studies. The resultant materials were characterized by XRD, X-ray absorption, X-ray photoelectron spectra, FTIR, UV-VIS, inductively coupled plasma, transmission electron spectroscopy, scanning electron microscopy with energy dispersive X-ray analysis, potentiometric titration, thermal analyses, TPD measurements, BET surface area and pore size distribution measurements. OL-1 materials prepared using this alcohol route showed enhanced thermal stabilities and increased Mg accommodation compared to OL-1s prepared with other methods. Based on the analysis methods developed here, Na-OL-1 exhibited recoverable and reversible structural and surface O2 oxygen species while K-OL-1 showed higher stability. Na-OL-1 had predominantly Bronsted acid sites resulting from OH groups bonded to Mn on Na-OL-1 surfaces, while the Na/Mg-OL-1 had mainly Lewis acid sites. Large porosity was obtained in chromia pillared OL-1 materials with a narrow pore size distribution centered around 18 A. Although these materials remained "amorphous" as determined by XRD after calcination, TEM morphology studies suggest that the materials were still layered. EXAFS studies indicated the formation of Cr-O-Mn bonds in the resultant materials via comer-shared linkages of CrO6 and MnO6 octahedra. Good crystallinity in

  9. From microscope to telescope: Using laboratory spectroscopic measurements to constrain the thermal evolution of silicate bodies in the solar system

    NASA Astrophysics Data System (ADS)

    Klima, Rachel L.; Young, Brianna C.; Rivkin, Andy S.

    2015-11-01

    Spectral measurements of planets and asteroids have long been used to inventory the composition of their surfaces. If laboratory techniques can be extrapolated to the larger spatial scales of remote observations, infrared spectroscopic measurements offer the potential to delve even deeper into the thermal evolution of these bodies. However, the scattering of light and mixing from the microscopic through macroscopic scales greatly complicates the analysis of components present even when surfaces are viewed at comparably high spatial resolution (<10-100 m/pixel). For this project, we have prepared and measured a set of meteorites and terrestrial analog rocks to perform coordinated spectroscopic studies, from microscopic spectral measurements across individual grains through measurement of bulk mineral and rock samples in ultra-high vacuum (UHV), to investigate two questions: (1) can microscopic mineral textures related to cation ordering and exsolution be reliably distinguished from physical mixtures as occur in regoliths and (2) can internally bound water in minerals be distinguished from water that has adsorbed from the environment. In each case, we explore how well the laboratory techniques address these questions and, through spectral modeling, what the limitations and challenges are for extrapolating these measurements to remote observations.

  10. Spectroscopic, thermal and mechanical studies on 4-methylanilinium p-toluenesulfonate - a new organic NLO single crystal.

    PubMed

    Shanmugam, G; Brahadeeswaran, S

    2012-09-01

    Bulk crystals of newly identified organic nonlinear optical material 4-methylanilinium p-toluenesulfonate (PMPT) were grown by slow evaporation solution growth method using ethanol as a solvent. It crystallizes in monoclinic system with a noncentrosymmetric space group P2(1). The formation of the title compound was confirmed through microanalysis, X-ray diffraction and density measurements. The proton positions and functional groups have been identified and confirmed through nuclear magnetic resonance and Fourier transform infrared spectrums respectively. Optical properties are determined by UV-Visible and photoluminescence spectroscopic studies to explore its efficacy towards device fabrications. Thermal studies exhibited that the newly obtained PMPT crystals are stable up to 199 °C. Its mechanical strength was studied by Vickers micro hardness studies. PMID:22634406

  11. 30 CFR 75.207 - Pillar recovery.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... Resources MINE SAFETY AND HEALTH ADMINISTRATION, DEPARTMENT OF LABOR COAL MINE SAFETY AND HEALTH MANDATORY SAFETY STANDARDS-UNDERGROUND COAL MINES Roof Support § 75.207 Pillar recovery. Pillar recovery shall be... unstable floor or roof, falls of roof, oil and gas well barriers or surface subsidence require that...

  12. 30 CFR 75.207 - Pillar recovery.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... Resources MINE SAFETY AND HEALTH ADMINISTRATION, DEPARTMENT OF LABOR COAL MINE SAFETY AND HEALTH MANDATORY SAFETY STANDARDS-UNDERGROUND COAL MINES Roof Support § 75.207 Pillar recovery. Pillar recovery shall be... unstable floor or roof, falls of roof, oil and gas well barriers or surface subsidence require that...

  13. 30 CFR 75.207 - Pillar recovery.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... Resources MINE SAFETY AND HEALTH ADMINISTRATION, DEPARTMENT OF LABOR COAL MINE SAFETY AND HEALTH MANDATORY SAFETY STANDARDS-UNDERGROUND COAL MINES Roof Support § 75.207 Pillar recovery. Pillar recovery shall be... unstable floor or roof, falls of roof, oil and gas well barriers or surface subsidence require that...

  14. 30 CFR 75.207 - Pillar recovery.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... Resources MINE SAFETY AND HEALTH ADMINISTRATION, DEPARTMENT OF LABOR COAL MINE SAFETY AND HEALTH MANDATORY SAFETY STANDARDS-UNDERGROUND COAL MINES Roof Support § 75.207 Pillar recovery. Pillar recovery shall be... unstable floor or roof, falls of roof, oil and gas well barriers or surface subsidence require that...

  15. 30 CFR 75.207 - Pillar recovery.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... Resources MINE SAFETY AND HEALTH ADMINISTRATION, DEPARTMENT OF LABOR COAL MINE SAFETY AND HEALTH MANDATORY SAFETY STANDARDS-UNDERGROUND COAL MINES Roof Support § 75.207 Pillar recovery. Pillar recovery shall be... unstable floor or roof, falls of roof, oil and gas well barriers or surface subsidence require that...

  16. Novel isatinoxime molybdenum and chromium complexes: Synthesis, spectroscopic, and thermal characterization

    NASA Astrophysics Data System (ADS)

    Nassar, Mostafa Y.; Attia, Attia S.; Adawy, Shaymaa; El-Shahat, M. F.

    2012-10-01

    Reactions of molybdenum and chromium hexacarbonyls with isatin-3-oxime (H2L) in THF were carried out under sun light or according to the traditional thermal reflux synthetic routes. Di-μ-oxo bimolybdenum complex, [Mo(H2L)(THF)(O)2]2 was successfully synthesized under the reflux conditions. However, the dichromium oxo complex, [Cr(H2L)(O)2]2 was prepared using the sun light route. The prepared complexes were characterized using elemental analysis, IR, mass spectrometry, UV-Vis spectra, thermal analysis, and magnetic measurements.

  17. Synthesis, spectroscopic and thermal studies of some IIB group complexes with a new N 2-Schiff base ligand

    NASA Astrophysics Data System (ADS)

    Montazerozohori, Morteza; Khani, Sara; Tavakol, Hosein; Hojjati, Ahmad; Kazemi, Mostafa

    2011-10-01

    Synthesis, spectroscopic and thermal studies of some complexes of a new N 2-Schiff base ligand of N1, N2-bis((E)-2-methyl-3-phenylallylidene)ethane-1,2-diamine (L) with a general formula of MLX 2 (M = Zn(II), Cd(II) and Hg(II); X = Cl -, Br -, I -, SCN - and N 3-) are described. The ligand and its complexes were characterized by elemental analysis, molar conductance, UV-vis spectra, FT-IR spectra, MS, 1H NMR and 13C NMR spectra. The conductivity measurement as well as spectral data indicated that the complexes are non-electrolyte. 1H and 13C NMR spectra have been studied in DMSO-d 6 and/or CDCl 3. The thermal behavior of the complexes shows weight loss by decomposition of the anions and ligand segments in the subsequent steps. Activation thermodynamic parameters of decomposition such as E*, Δ H*, Δ S* and Δ G* were calculated from TG curves.

  18. Thermal and spectroscopic properties of the nano-system (ZnO(1-x)SiO2(x))

    NASA Astrophysics Data System (ADS)

    El-Kabbany, F.; Taha, S.; Hafez, M.; Yahia, I. S.

    2016-05-01

    Structural and thermal properties of the investigated nano-matrix ZnO(1-x)SiO2(x) samples were characterized by various techniques such as X-ray analysis, scanning electron microscopy (SEM), thermogravimetric analysis (TGA) and differential thermal analysis (DTA). IR spectroscopic analysis in the frequency range 400-4000 cm-1 is used here to investigate the new nano-system at room temperature. The variation of enthalpy (ΔH) with the concentration of SiO2 nanoparticles for the five systems of the ZnO(1-x)SiO2(x) matrix is determined. Seven different fundamental modes have been investigated. All of the vibrations of the investigated nano-system (ZnO(1-x)SiO2(x)) were found to be 449 cm-1, 469 cm-1, 798 cm-1, 959 cm-1, 1096 cm-1, 1630 cm-1 and 3447 cm-1 correspond to normal vibrations of stretching mode of ZnO, Si - O - Si or O - Si - O bending mode, Si - O - Si symmetric stretching, vibrational mode of Si-O - Zn, Si - O - Si asymmetric stretching, bending vibration mode of adsorbed water and stretching vibration of OH group respectively in which the variations strongly support the variation of ZnO and SiO2 nanoparticles concentration in the studied matrix. Measurements and interpretation of IR spectra as a function of ZnO and SiO2 nanoparticles concentration is reported.

  19. Synthesis, structural, spectroscopic and thermal characteristics of disubstituted biphenyl derivative: Biphenyl-4,4‧-diacetic acid

    NASA Astrophysics Data System (ADS)

    Sienkiewicz-Gromiuk, Justyna; Głuchowska, Halina; Tarasiuk, Bogdan; Mazur, Liliana; Rzączyńska, Zofia

    2014-07-01

    A novel 4,4‧-disubstituted biphenyl derivative featuring two acetic acid side arms symmetrically attached to a biphenyl system, that is biphenyl-4,4‧-diacetic acid (H2bpda), has been successfully synthesized by means of the three-stage organic strategy. The synthesis product was characterized by elemental analysis, various spectroscopic techniques including FT-IR, Raman, 1H and 13C NMR as well as thermogravimetric and TG-FT-IR coupled measurements. The phase purity of material was verified on the basis of the X-ray powder diffraction. The studied compound crystallizes in the monoclinic P21/c space group with half of the molecule in the asymmetric unit. Structural studies indicate intermolecular Osbnd H⋯O hydrogen bonding between the carboxylic groups of the adjacent molecules of H2bpda. The occurrence of intermolecularly associated carboxylic groups can also be clearly seen in the vibrational spectra of the acid. On thermal analysis both in air and nitrogen an anhydrous compound demonstrates considerable thermal stability.

  20. Spectroscopic, thermal and electrochemical studies on some nickel(II) thiosemicarbazone complexes

    NASA Astrophysics Data System (ADS)

    El-Shazly, R. M.; Al-Hazmi, G. A. A.; Ghazy, S. E.; El-Shahawi, M. S.; El-Asmy, A. A.

    2005-01-01

    Several complexes of thiosemicarbazone derivatives with Ni(II) have been prepared. Structural investigation of the ligands and their complexes has been made based on elemental analysis, magnetic moment, spectral (UV-Vis, i.r., 1H NMR, ms), and thermal studies. The i.r. spectra suggest the bidentate mononegative and tridentate (neutral, mono-, and binegative) behavior of the ligands. Different stereochemistries were suggested for the isolated complexes. The thermogravimetry (TG) and derivative thermogravimetry (DTG) have been used to study the thermal decomposition and kinetic parameters of some ligands and complexes using the Coats-Redfern and Horowitz-Metzger equations. The redox properties and stability of the complexes toward oxidation waves explored by cyclic voltammetry are related to the electron withdrawing or releasing ability of the substituent of thiosemicarbazone moiety. The samples displayed Ni II/Ni I couples irreversible waves associated with Ni III/Ni II process.

  1. Stability of Pin1 as revealed by thermal and spectroscopic studies

    NASA Astrophysics Data System (ADS)

    Wang, Jing-Zhang; Lin, Tao; Zhu, Guo-Fei; Du, Lin-Fang

    2010-06-01

    Pin1 is a two-domain enzyme which has peptidyl-prolyl cis/trans isomerase activity. Pin1 recognizes phospho-Ser/Thr-Pro motifs in cell-signaling proteins, and is both a cancer and an Alzheimer's disease target. The thermal stability of Pin1 was studied intensively by SDS-PAGE, enzymatic activity assay, intrinsic fluorescence spectroscopy and circular dichroism spectroscopy. The activity of Pin1 gradually decreased above 40 °C, and the Tm was 57.6 ± 1.0 °C. Fluorescence experiments indicated that heat treatment induced changes in the substructures in Pin1, resulting in that the polarity in the microenvironments of the tryptophan residues increased. It is assumed that the thermal denaturation of Pin1 involved a three-state transition. The intermediate state of Pin1 at about 60 °C was confirmed by fluorescence emission spectra, the synchronous fluorescence spectra and CD measurements. Decreases in α-helix and β-sheet appeared above 40 °C, which was balanced by an enhancement in unordered coil. The Tm values calculated from α-helix transition and β-sheet transition were 54.6 ± 0.6 °C and 70.7 ± 3.3 °C, respectively. Our results illustrated that Pin1 had a relatively high thermal stability and the WW domain had a higher stability than the PPIase domain.

  2. Laser ceramics Tm:Lu2O3. Thermal, thermo-optical, and spectroscopic properties

    NASA Astrophysics Data System (ADS)

    Ivakin, E. V.; Kisialiou, I. G.; Antipov, O. L.

    2013-01-01

    In this paper we report the measurements of in-plane thermal diffusivity, lifetime of metastable level 3F4, thermal coefficients of linear expansion and refractive index change of laser ceramics Tm(2 at.%):Lu2O3 by the transient grating technique. The wavelengths 213, 266, 355 and 796 nm from pulsed lasers were chosen for sample excitation in accordance with the desire to measure particular parameters. The experimentally determined thermal diffusivity 0.05 cm2/s was attributed to subsurface layer, which has thickness of order of grating period. The applied approach ensured more reliable measurement of lifetime of metastable 3F4 level as compared to the conventional luminescence detection. The dynamic value of linear expansion coefficient was measured under sample excitation at 213 nm and was found to be close to that as measured elsewhere in static regime. Coefficient of refraction index change was found to be as high as 2 × 10-5 K-1. The value of absorption coefficient of ceramics at 213 nm was estimated by excitation of acoustic grating in a thin layer of air adjacent to the sample surface. After the estimation, it exceeded 104 cm-1.

  3. New copper(II) complexes with dopamine hydrochloride and vanillymandelic acid: Spectroscopic and thermal characterization

    NASA Astrophysics Data System (ADS)

    Mohamed, Gehad G.; Nour El-Dien, F. A.; El-Nahas, R. G.

    2011-10-01

    The dopamine derivatives participate in the regulation of wide variety of physiological functions in the human body and in medication life. Increase and/or decrease in the concentration of dopamine in human body reflect an indication for diseases such as Schizophrenia and/or Parkinson diseases. The Cu(II) chelates with coupled products of dopamine hydrochloride (DO.HCl) and vanillymandelic acid (VMA) with 4-aminoantipyrine (4-AAP) are prepared and characterized. Different physico-chemical techniques namely IR, magnetic and UV-vis spectra are used to investigate the structure of these chelates. Cu(II) forms 1:1 (Cu:DO) and 1:2 (Cu:VMA) chelates. DO behave as a uninegative tridentate ligand in binding to the Cu(II) ion while VMA behaves as a uninegative bidentate ligand. IR spectra show that the DO is coordinated to the Cu(II) ion in a tridentate manner with ONO donor sites of the phenolic- OH, -NH and carbonyl- O, while VMA is coordinated with OO donor sites of the phenolic- OH and -NH. Magnetic moment measurements reveal the presence of Cu(II) chelates in octahedral and square planar geometries with DO and VMA, respectively. The thermal decomposition of Cu(II) complexes is studied using thermogravimetric (TG) and differential thermal analysis (DTA) techniques. The activation thermodynamic parameters, such as, energy of activation, enthalpy, entropy and free energy change of the complexes are evaluated and the relative thermal stability of the complexes are discussed.

  4. FTIR spectroscopic, thermal and XRD characterization of hydroxyapatite from new natural sources.

    PubMed

    Shaltout, Abdallah A; Allam, Moussa A; Moharram, Mohamed A

    2011-12-01

    The inorganic constituents of 5 different plants (leaves and stalks) were investigated by using Fourier transformer infrared spectroscopy (FTIR), X-ray diffraction (XRD) and thermal analysis including thermal gravimetric analysis (TGA), derivative thermogravimetry (DTG) and differential scanning calorimetry (DSC). These plants are Catha edulis (Khat), basil, mint, green tea and trifolium. The absorption bands of carbonate ions CO(3)(2-) was exhibited at 1446 cm(-1), and the phosphate ions PO(4)(3-) was assigned at 1105 and 1035 cm(-1). At high temperatures (600, 700 and 600°C) further absorption bands of the phosphate ions PO(4)(3-) was assigned at the frequencies 572, 617, 962, 1043 and 1110 cm(-1) and the vibrational absorption band of the carbonate ions CO(3)(2-) was assigned at 871, 1416 and 1461 cm(-1). X-ray diffraction and thermal analysis confirm the obtained results of FITR. Results showed that the main inorganic constituents of C. edulis and basil leaves are hydroxyapatite whereas the hydroxyapatite content in the other plant samples is less than that in case of C. edulis and basil plant leaves. PMID:21903453

  5. FTIR spectroscopic, thermal and XRD characterization of hydroxyapatite from new natural sources

    NASA Astrophysics Data System (ADS)

    Shaltout, Abdallah A.; Allam, Moussa A.; Moharram, Mohamed A.

    2011-12-01

    The inorganic constituents of 5 different plants (leaves and stalks) were investigated by using Fourier transformer infrared spectroscopy (FTIR), X-ray diffraction (XRD) and thermal analysis including thermal gravimetric analysis (TGA), derivative thermogravimetry (DTG) and differential scanning calorimetry (DSC). These plants are Catha edulis (Khat), basil, mint, green tea and trifolium. The absorption bands of carbonate ions CO 32- was exhibited at 1446 cm -1, and the phosphate ions PO 43- was assigned at 1105 and 1035 cm -1. At high temperatures (600, 700 and 600 °C) further absorption bands of the phosphate ions PO 43- was assigned at the frequencies 572, 617, 962, 1043 and 1110 cm -1 and the vibrational absorption band of the carbonate ions CO 32- was assigned at 871, 1416 and 1461 cm -1. X-ray diffraction and thermal analysis confirm the obtained results of FITR. Results showed that the main inorganic constituents of C. edulis and basil leaves are hydroxyapatite whereas the hydroxyapatite content in the other plant samples is less than that in case of C. edulis and basil plant leaves.

  6. Hydrogen-bonded pillars of alternating chiral complex cations and anions: 1. Synthesis, characterization, X-ray structure and thermal stability of catena-{[Co(H(2)oxado)(3)][Cr(C(2)O(4))(3)].5H(2)O} and of its precursor (H(3)oxado)[Co(H(2)oxado)(3)](SO(4))(2).2H(2)O.

    PubMed

    Bélombé, M M; Nenwa, J; Mbiangué, Y A; Majoumo-Mbé, F; Lönnecke, P; Hey-Hawkins, E

    2009-06-21

    Compound (H(3)oxado)[Co(H(2)oxado)(3)](SO(4))(2).2H(2)O () (H(3)oxado(+) = oxamide dioximemonoximium) reacted metathetically with Ba(6)(H(2)O)(17)[Cr(C(2)O(4))(3)](4).7H(2)O in water to give the one-dimensional complex salt {[Co(H(2)oxado)(3)][Cr(C(2)O(4))(3)].5H(2)O}(infinity) () (H(2)oxado = oxamide dioxime). Compounds and were characterized by elemental analysis, FTIR, UV-Vis and by single crystal X-ray structure determination. The structure of consists of infinite pillars of alternating chiral complex cations and anions linked together along [100] by electrostatic and longitudinal O-HO interactions, with an average intrachain CoCr separation of 4.94 A. Equatorial N-HO bridges cross-link neighboring pillars (which are of opposite chirality) and consolidate a three-dimensional lattice framework which delineates elliptic nanochannels parallel to the a axis, encapsulating highly disordered water molecules. The thermal stability of both compounds was assessed by TGA, and the effective magnetic moment of , checked at room temperature, revealed considerable spin-orbit coupling. PMID:19488450

  7. 33 CFR 80.1140 - Pillar Point Harbor, CA.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 33 Navigation and Navigable Waters 1 2010-07-01 2010-07-01 false Pillar Point Harbor, CA. 80.1140... NAVIGATION RULES COLREGS DEMARCATION LINES Pacific Coast § 80.1140 Pillar Point Harbor, CA. A line drawn from Pillar Point Harbor Light 6 to Pillar Point Harbor Entrance Light....

  8. 33 CFR 80.1140 - Pillar Point Harbor, CA.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 33 Navigation and Navigable Waters 1 2011-07-01 2011-07-01 false Pillar Point Harbor, CA. 80.1140... NAVIGATION RULES COLREGS DEMARCATION LINES Pacific Coast § 80.1140 Pillar Point Harbor, CA. A line drawn from Pillar Point Harbor Light 6 to Pillar Point Harbor Entrance Light....

  9. Aqueous citrato-oxovanadate(IV) precursor solutions for VO2: synthesis, spectroscopic investigation and thermal analysis.

    PubMed

    Peys, Nick; Adriaensens, Peter; Van Doorslaer, Sabine; Gielis, Sven; Peeters, Ellen; De Dobbelaere, Christopher; De Gendt, Stefan; Hardy, An; Van Bael, Marlies K

    2014-09-01

    An aqueous precursor solution, containing citrato-VO(2+) complexes, is synthesized for the formation of monoclinic VO2. With regard to the decomposition of the VO(2+) complexes towards vanadium oxide formation, it is important to gain insights into the chemical structure and transformations of the precursor during synthesis and thermal treatment. Hence, the conversion of the cyclic [V4O12](4-) ion to the VO(2+) ion in aqueous solution, using oxalic acid as an acidifier and a reducing agent, is studied by (51)Vanadium nuclear magnetic resonance spectroscopy. The citrate complexation of this VO(2+) ion and the differentiation between a solution containing citrato-oxalato-VO(2+) and citrato-VO(2+) complexes are studied by electron paramagnetic resonance and Fourier transform infra-red spectroscopy. In both solutions, the VO(2+) containing complex is mononuclear and has a distorted octahedral geometry with a fourfold R-CO2(-) ligation at the equatorial positions and likely a fifth R-CO2(-) ligation at the axial position. Small differences in the thermal decomposition pathway between the gel containing citrato-oxalato-VO(2+) complexes and the oxalate-free gel containing citrato-VO(2+) complexes are observed between 150 and 200 °C in air and are assigned to the presence of (NH4)2C2O4 in the citrato-oxalato-VO(2+) solution. Both precursor solutions are successfully used for the formation of crystalline vanadium oxide nanostructures on SiO2, after thermal annealing at 500 °C in a 0.1% O2 atmosphere. However, the citrato-oxalato-VO(2+) and the oxalate-free citrato-VO(2+) solution result in the formation of monoclinic V6O13 and monoclinic VO2, respectively. PMID:25005054

  10. Spectroscopic, thermal analysis and DFT computational studies of salen-type Schiff base complexes

    NASA Astrophysics Data System (ADS)

    Ebrahimi, Hossein Pasha; Hadi, Jabbar S.; Abdulnabi, Zuhair A.; Bolandnazar, Zeinab

    2014-01-01

    A new series of metal(II) complexes of Co(II), Ni(II), Cu(II), Zn(II), and Pb(II) have been synthesized from a salen-type Schiff base ligand derived from o-vanillin and 4-methyl-1,2-phenylenediamine and characterized by elemental analysis, spectral (IR, UV-Vis, 1H NMR, 13C NMR and EI-mass), molar conductance measurements and thermal analysis techniques. Coats-Redfern method has been utilized to calculate the kinetic and thermodynamic parameters of the metal complexes. The molecular geometry, Mulliken atomic charges of the studied compounds were investigated theoretically by performing density functional theory (DFT) to access reliable results to the experimental values. The theoretical 13C chemical shift results of the studied compounds have been calculated at the B3LYP, PBEPBE and PW91PW91 methods and standard 6-311+G(d,p) basis set starting from optimized geometry. The comparison of the results indicates that B3LYP/6-311+G(d,p) yields good agreement with the observed chemical shifts. The measured low molar conductance values in DMF indicate that the metal complexes are non-electrolytes. The spectral and thermal analysis reveals that all complexes have octahedral geometry except Cu(II) complex which can attain the square planner arrangement. The presence of lattice and coordinated water molecules are indicated by thermograms of the complexes. The thermogravimetric (TG/DTG) analyses confirm high stability for all complexes followed by thermal decomposition in different steps.

  11. Spectroscopic Evidence for Exceptional Thermal Contribution to Electron-Beam Induced Fragmentation

    SciTech Connect

    Caldwell, Marissa A.; Haynor, Ben; Aloni, Shaul; Ogletree, D. Frank; Wong, H.-S. Philip; Urban, Jeffrey J.; Milliron, Delia J.

    2010-11-16

    While electron beam induced fragmentation (EBIF) has been reported to result in the formation of nanocrystals of various compositions, the physical forces driving this phenomenon are still poorly understood. We report EBIF to be a much more general phenomenon than previously appreciated, operative across a wide variety of metals, semiconductors and insulators. In addition, we leverage the temperature dependent bandgap of several semiconductors to quantify -- using in situ cathodoluminescence spectroscopy -- the thermal contribution to EBIF, and find extreme temperature rises upwards of 1000K.

  12. Crystal structure, spectroscopic investigation and thermal properties of L-lysine p-toluenesulfonate

    NASA Astrophysics Data System (ADS)

    Wang, L.; Wang, D. H.; Zhang, G. H.; Xu, D.; Deng, W. X.

    2016-03-01

    A novel organic crystal was prepared from L-lysine (Lly) and p-toluenesulfonic acid (pTS), which was grown from an aqueous solution by slow cooling method. The crystal system and the lattice parameters have been confirmed by single crystal X-ray diffraction studies. The FT-IR, FT-Raman, 1H-NMR and 13C-NMR spectral of the crystal have been recorded and analyzed. The spectral analyses confirmed the presence of various functional groups and the molecular configurations in LLTS crystal. The UV-Vis-NIR transmittance spectrum has been carried out which shows the cutoff wavelength around 280 nm. The thermal properties of crystal have been evaluated from thermogravimetric (TG) and differential thermal analysis (DTA). The melting point of grown crystal is fairly high, at around 259 °C. The nonlinear optical (NLO) properties of LLTS crystal were demonstrated by powder SHG experiment and also by quantum chemical calculations. The powder SHG efficiency of LLTS crystal is relatively low and very different from theoretical calculation results.

  13. Change Spectroscopic, thermal and mechanical studies of PU/PVC blends

    NASA Astrophysics Data System (ADS)

    Hezma, A. M.; Elashmawi, I. S.; Rajeh, A.; Kamal, Mustafa

    2016-08-01

    Blends of polyurethane (PU) and polyvinyl chloride (PVC) with different concentrations were prepared by casting method. The effects of PU on PVC blends was examined by Fourier transform-infrared (FTIR), Ultra-violet visible studies (UV/VIS.), X-ray diffraction (XRD), Thermogravimetric (TGA), Differential scanning calorimetry (DSC), and mechanical properties (stress-strain curve). The interaction between PU and PVC was examined by FT-IR through the absorbance of the N-H groups and was correlated to mechanical/thermal properties. Ultra-violet visible said that optical energy gap decrease with increasing concentration of PU. Differential scanning calorimetry results was observed a single glass transition temperature (Tg) for blends this confirming existence miscibility within the blends. The causes for best thermal stability of some blends may be described by measurements of interactions between C=O groups of PU and the α-hydrogen of PVC or a dipole-dipole -C=O..Cl-C- interactions. Significant alterations in FTIR, X-ray and DSC examination shows an interactions between blends had good miscibility. X-ray shows some alterations in the intensity with additional PU. PU change the mechanical behavior of PVC through of the blends. When polyurethane content increase causes polyvinyl chloride tensile strength decreases and elongation at break increase.

  14. Mineralogy and inorganic chemistry of naturally occurring biogenic iron oxyhydroxides: Spectroscopic evidence of thermal maturation

    NASA Astrophysics Data System (ADS)

    Haddad, A.; Fakra, S.; Orcutt, B. N.; Toner, B.; Edwards, K. J.

    2011-12-01

    Microbial mats were sampled at four sites at the Lo'ihi Seamount and examined for changes in mineralogy and inorganic chemistry via synchrotron-sourced X-ray Absorption Spectroscopy (XAS). These mats are rich in iron oxyhydroxides with morphologies similar to those produced by iron oxidizing microorganisms related to Zetaproteobacteria such as Mariprofundus ferroxydans, which have been shown to be present and active in all of these mat ecosystems. The same particle morphologies are observed consistently at all four sites, which range in temperature (4 - 40°C) and hydrothermal activity (dead to very active). Fe L-edge XAS reveals no significant differences in Fe speciation between the morphologies. Mineralogy, however, as reflected in O 1s XAS measurements, appears to be a function of thermal maturation with the hottest site harboring more crystalline particles. Morphology does not factor into the changes in mineralogy. These measurements are confirmed by Fe 1s XAS spectroscopy. The C 1s XAS spectroscopy is highly variable and may be related to overall maturation (age) or undetermined factors. Elucidating the effect of thermal maturation on biogenic iron oxhydroxide particles is essential to understanding the environmental influences on their preservation in the rock record.

  15. Synthesis, spectroscopic, thermal and electrochemical studies on thiazolyl azo based disperse dyes bearing coumarin

    NASA Astrophysics Data System (ADS)

    Özkütük, Müjgan; İpek, Ezgi; Aydıner, Burcu; Mamaş, Serhat; Seferoğlu, Zeynel

    2016-03-01

    In this study, seven novel thiazolyl azo disperse dyes (6a-g) were synthesized and fully characterized by FT-IR, 1H NMR, 13C NMR, and mass spectral techniques. The electronic absorption spectra of the dyes in solvents of different polarities cover a λmax range of 404-512 nm. The absorption properties of the dyes changed drastically upon acidification. This was due to the protonation of the nitrogen in the thiazole ring, which in turn increased the donor-acceptor interplay of the π system in the dyes, and therefore increased the absorption properties of the prepared dyes. Thermal analysis showed that these dyes are thermal stable up to 269 °C. Additionally, the electrochemical behavior of the dyes (6a-g) were investigated using cyclic voltammetric and chronoamperometric techniques, in the presence of 0.10 M tetrabutylammonium tetrafluoroborate, in dimethylsulfoxide, at a glassy carbon electrode. The number of transferred electrons, and the diffusion coefficient were determined by electrochemical methods. The results showed that, for all the dyes, one oxidation peak and two reduction peaks were observed.

  16. Mononuclear metal complexes of organic carboxylic acid derivatives: Synthesis, spectroscopic characterization, thermal investigation and antimicrobial activity

    NASA Astrophysics Data System (ADS)

    Abd El-Wahab, Zeinab H.

    2007-05-01

    Two Schiff base ligands bearing organic acid moiety, vis., N-(2-thienylmethylidene)-2-amino-4-chlorobenzoic acid (HL 1) and N-(2-hydroxybenzylidene)-2-amino-4-chlorobenzoic acid (H 2L 2) have been synthesized by the interaction of 2-thiophenecarboxaldehyde and 2-hydroxybenzaldehyde with 2-amino-4-chlorobenzoic acid. Co(II), Ni(II), Cu(II) and Zn(II) complexes of these ligands have been prepared. They are characterized on the basis of analytical data, molar conductance, IR, 1H NMR, UV-vis, mass spectra, magnetic measurements, thermal analysis and X-ray powder diffraction technique. The molar conductance data reveal that these complexes are non-electrolytes. The ligands are coordinated to the metal ions in a terdentate manner with ONO/ONS donor sites of the carbonyl oxygen, azomethine nitrogen and phenolic oxygen or thiophenic sulphur. An octahedral structure is proposed for the prepared metal complexes and some ligand field parameters ( Dq, B and β) in addition to CFSE were calculated. The thermal stability of the metal complexes is evaluated. The Schiff base ligands and their metal complexes have been tested against four species of bacteria as well as four species of fungi and the results have been compared with some known antibiotics.

  17. Chemical, Thermal and Spectroscopic Methods to Assess Biodegradation of Winery-Distillery Wastes during Composting.

    PubMed

    Torres-Climent, A; Gomis, P; Martín-Mata, J; Bustamante, M A; Marhuenda-Egea, F C; Pérez-Murcia, M D; Pérez-Espinosa, A; Paredes, C; Moral, R

    2015-01-01

    The objective of this work was to study the co-composting process of wastes from the winery and distillery industry with animal manures, using the classical chemical methods traditionally used in composting studies together with advanced instrumental methods (thermal analysis, FT-IR and CPMAS 13C NMR techniques), to evaluate the development of the process and the quality of the end-products obtained. For this, three piles were elaborated by the turning composting system, using as raw materials winery-distillery wastes (grape marc and exhausted grape marc) and animal manures (cattle manure and poultry manure). The classical analytical methods showed a suitable development of the process in all the piles, but these techniques were ineffective to study the humification process during the composting of this type of materials. However, their combination with the advanced instrumental techniques clearly provided more information regarding the turnover of the organic matter pools during the composting process of these materials. Thermal analysis allowed to estimate the degradability of the remaining material and to assess qualitatively the rate of OM stabilization and recalcitrant C in the compost samples, based on the energy required to achieve the same mass losses. FT-IR spectra mainly showed variations between piles and time of sampling in the bands associated to complex organic compounds (mainly at 1420 and 1540 cm-1) and to nitrate and inorganic components (at 875 and 1384 cm-1, respectively), indicating composted material stability and maturity; while CPMAS 13C NMR provided semi-quantitatively partition of C compounds and structures during the process, being especially interesting their variation to evaluate the biotransformation of each C pool, especially in the comparison of recalcitrant C vs labile C pools, such as Alkyl /O-Alkyl ratio. PMID:26418458

  18. Chemical, Thermal and Spectroscopic Methods to Assess Biodegradation of Winery-Distillery Wastes during Composting

    PubMed Central

    Torres-Climent, A.; Gomis, P.; Martín-Mata, J.; Bustamante, M. A.; Marhuenda-Egea, F. C.; Pérez-Murcia, M. D.; Pérez-Espinosa, A.; Paredes, C.; Moral, R.

    2015-01-01

    The objective of this work was to study the co-composting process of wastes from the winery and distillery industry with animal manures, using the classical chemical methods traditionally used in composting studies together with advanced instrumental methods (thermal analysis, FT-IR and CPMAS 13C NMR techniques), to evaluate the development of the process and the quality of the end-products obtained. For this, three piles were elaborated by the turning composting system, using as raw materials winery-distillery wastes (grape marc and exhausted grape marc) and animal manures (cattle manure and poultry manure). The classical analytical methods showed a suitable development of the process in all the piles, but these techniques were ineffective to study the humification process during the composting of this type of materials. However, their combination with the advanced instrumental techniques clearly provided more information regarding the turnover of the organic matter pools during the composting process of these materials. Thermal analysis allowed to estimate the degradability of the remaining material and to assess qualitatively the rate of OM stabilization and recalcitrant C in the compost samples, based on the energy required to achieve the same mass losses. FT-IR spectra mainly showed variations between piles and time of sampling in the bands associated to complex organic compounds (mainly at 1420 and 1540 cm-1) and to nitrate and inorganic components (at 875 and 1384 cm-1, respectively), indicating composted material stability and maturity; while CPMAS 13C NMR provided semi-quantitatively partition of C compounds and structures during the process, being especially interesting their variation to evaluate the biotransformation of each C pool, especially in the comparison of recalcitrant C vs labile C pools, such as Alkyl /O-Alkyl ratio. PMID:26418458

  19. Irradiated lanoline as a prospective substance for biomedical applications: A spectroscopic and thermal study

    NASA Astrophysics Data System (ADS)

    Hanzlikova, Zuzana; Hybler, Peter; Fülop, Marko; Ondruska, Jan; Jomova, Klaudia; Porubska, Maria; Valko, Marian

    2015-08-01

    Refined wool wax products, such as lanoline and lanoline derivatives are key ingredients in some of the ointments, cosmetics, pharmaceuticals, waterproof coatings and other products. Beneficial medicinal effects along with melting point near normal human body temperature designated lanoline to be used in pharmacotherapy and medical treatments. Since the general requirements for sterility of medicinal substances are very strict, especially in cases of skin contact, radiation technologies represent a valuable tool to sterilize the materials for medicinal purposes. In this work, lanoline was irradiated with accelerated electron beam in air within 0-400 kG dose to simulate sterilization for medical purposes. The irradiated lanoline showed considerable fluctuation of chemical structure. The most significant fluctuation was observed for etheric species, followed by ethylene sequences with n<4. While primary and secondary alcohols, as well as epoxides species, decreased below the initial concentration within whole range of the doses, aliphatic esters and ethylene sequences (CH2)n with n≥4 indicated the most stable species. A trace amount of organic-in origin radicals was observed and that increased slightly with dose. Depending on dose, the melting temperature varied from 39.7 to 45.7 °C and the highest values were reached for 25 kGy and 156 kGy. For these same doses the highest thermal stability was also observed and, simultaneously the thermal stability was related inversely to the destruction rate. We propose, that the chemical transformation of lanoline within 0-25 kGy dose should be tested for prospective medical purposes as well as for the need to eliminate remaining outlasting organic-in-origin radicals which were detected in the lanoline even one year after the irradiation.

  20. Synthesis, spectroscopic, structural and thermal characterizations of vanadyl(IV) adenine complex prospective as antidiabetic drug agent.

    PubMed

    El-Megharbel, Samy M; Hamza, Reham Z; Refat, Moamen S

    2015-01-25

    The vanadyl(IV) adenine complex; [VO(Adn)2]⋅SO4; was synthesized and characterized. The molar conductivity of this complex was measured in DMSO solution that showed an electrolyte nature. Spectroscopic investigation of the green solid complex studied here indicate that the adenine acts as a bidentate ligand, coordinated to vanadyl(IV) ions through the nitrogen atoms N7 and nitrogen atom of amino group. Thus, from the results presented the vanadyl(IV) complex has square pyramid geometry. Further characterizations using thermal analyses and scanning electron techniques was useful. The aim of this paper was to introduce a new drug model for the diabetic complications by synthesized a novel mononuclear vanadyl(IV) adenine complex to mimic insulin action and reducing blood sugar level. The antidiabetic ability of this complex was investigated in STZ-induced diabetic mice. The results suggested that VO(IV)/adenine complex has antidiabetic activity, it improved the lipid profile, it improved liver and kidney functions, also it ameliorated insulin hormone and blood glucose levels. The vanadyl(IV) complex possesses an antioxidant activity and this was clear through studying SOD, CAT, MDA, GSH and methionine synthase. The current results support the therapeutic potentiality of vanadyl(IV)/adenine complex for the management and treatment of diabetes. PMID:25150436

  1. Synthesis, spectroscopic, structural and thermal characterizations of vanadyl(IV) adenine complex prospective as antidiabetic drug agent

    NASA Astrophysics Data System (ADS)

    El-Megharbel, Samy M.; Hamza, Reham Z.; Refat, Moamen S.

    2015-01-01

    The vanadyl(IV) adenine complex; [VO(Adn)2]ṡSO4; was synthesized and characterized. The molar conductivity of this complex was measured in DMSO solution that showed an electrolyte nature. Spectroscopic investigation of the green solid complex studied here indicate that the adenine acts as a bidentate ligand, coordinated to vanadyl(IV) ions through the nitrogen atoms N7 and nitrogen atom of amino group. Thus, from the results presented the vanadyl(IV) complex has square pyramid geometry. Further characterizations using thermal analyses and scanning electron techniques was useful. The aim of this paper was to introduce a new drug model for the diabetic complications by synthesized a novel mononuclear vanadyl(IV) adenine complex to mimic insulin action and reducing blood sugar level. The antidiabetic ability of this complex was investigated in STZ-induced diabetic mice. The results suggested that VO(IV)/adenine complex has antidiabetic activity, it improved the lipid profile, it improved liver and kidney functions, also it ameliorated insulin hormone and blood glucose levels. The vanadyl(IV) complex possesses an antioxidant activity and this was clear through studying SOD, CAT, MDA, GSH and methionine synthase. The current results support the therapeutic potentiality of vanadyl(IV)/adenine complex for the management and treatment of diabetes.

  2. Confocal and near-field spectroscopic investigation of P3HT:PCBM organic blend film upon thermal annealing

    NASA Astrophysics Data System (ADS)

    Wang, Xiao; Zhang, Dai; Braun, Kai; Egelhaaf, Hans-Joachim; Meixner, Alfred J.

    2009-08-01

    The poly(3-hexylthiophene) (P3HT) and [6,6]-phenyl C61 butyric acid methyl ester (PCBM) organic films are widely employed as electronic donor and acceptor in the field of organic film solar cell because of their high photovoltaic conversion efficiency. A home-built parabolic mirror assisted confocal and apertureless near-field optical microscope was used to investigate the degradation behavior of the film and to distinguish the donor and acceptor domains both topographically and optically. Under ambient condition, the degradation rates are decreased in the sequence of pristine P3HT, blend P3HT:PCBM film and pristine PCBM. N2 protection dramatically slows down the film degradation rate. Using confocal spectroscopic mapping, we are able to distinguish the local distributions of P3HT and PCBM. Micrometer PCBM aggregates were observed due to the thermal annealing process. Our experimental methods show the possibility to investigate morphology and the photochemistry properties of the organic solar cell films with high spatial resolution.

  3. Montmorillonite-based porous clay heterostructures (PCHs) intercalated with silica-titania pillars-synthesis and characterization

    SciTech Connect

    Chmielarz, Lucjan; Gil, Barbara; Kustrowski, Piotr; Piwowarska, Zofia; Dudek, Barbara; Michalik, Marek

    2009-05-15

    Porous clay heterostructures (PCHs) were synthesized using natural montmorillonite as a raw material. Apart from pure silica pillars also silica-titania pillars were intercalated into the interlayer space of the parent clay. The detailed studies of the calcination process of the as-prepared PCH samples as well as thermal stability of the pillared structure of these materials were performed. The pillared structure of PCHs intercalated with both silica and silica-titania clusters was found to be thermally stable up to temperatures exceeding 600 deg. C. It was found that titanium incorporated into the silica pillars was present mainly in the form of separated tetracoordinated cations. For the samples with the higher Ti loading also small contribution of titanium in the form of the polymeric oxide species was detected. Titanium incorporated into the PCH materials significantly increased their surface acidity forming mainly Bronsted acid sites. - Graphical abstract: Synthesis of the montmorillonite based porous clay heterostructures (PCHs) intercalated with silica-titania pillars has been performed. The mechanism of the thermal degradation of organic templates in the pore system of PCHs was studied. PCHs were characterized with respect to structure, texture, composition, surface acidity, thermal stability and form of introduced titanium.

  4. Spectrophotometric method for the determination, validation, spectroscopic and thermal analysis of diphenhydramine in pharmaceutical preparation

    NASA Astrophysics Data System (ADS)

    Ulu, Sevgi Tatar; Elmali, Fikriye Tuncel

    2010-09-01

    A sensitive, simple and rapid spectrophotometric method was developed for the determination of diphenhydramine in pharmaceutical preparation. The method was based on the charge-transfer complex of the drug, as n-electron donor, with 2,3-dichloro-5,6-dicyano- p-benzoquinone (DDQ), as π-acceptor. The formation of this complex was also confirmed by UV-vis, FTIR and 1H NMR spectra techniques and thermal analysis. The proposed method was validated according to the ICH guidelines with respect to linearity, limit of detection, limit of quantification, accuracy, precision, recovery and robustness. The linearity range for concentrations of diphenhydramine was found to be 12.5-150 μg/mL with acceptable correlation coefficients. The detection and quantification limits were found to be 2.09 and 6.27 μg/mL, respectively. The proposed and references methods were applied to the determination of drug in syrup. This preparation were also analyzed with an reference method and statistical comparison by t- and F-tests revealed that there was no significant difference between the results of the two methods with respect to mean values and standard deviations at the 95% confidence level.

  5. Spectroscopic, thermal analyses, structural and antibacterial studies on the interaction of some metals with ofloxacin

    NASA Astrophysics Data System (ADS)

    Zordok, W. A.; El-Shwiniy, W. H.; El-Attar, M. S.; Sadeek, S. A.

    2013-09-01

    Reaction between the fluoroquinolone antibacterial agent ofloxacin and V(IV), Zr(IV) and U(VI) in methanol and acetone was studied. The ability of ofloxacin to form metal complexes is high. The isolated solid complexes were characterized by elemental analysis, magnetic moment, conductance measurements, infrared, electronic, 1H NMR spectra and thermal investigation. In all complexes the ofloxacin ligand is coordinated through the pyridone and carboxylate oxygen forming 1:2 M:HOfl complexes. The calculated bond length and force constant, F(Udbnd O), in the uranyl complex are 1.73 Å and 640.83 N m-1, respectively. The metal-ligand binding of the V(IV) and Zr(IV) complexes was predicted by using the density functional theory (DFT) at the B3LYP-CEP-31G level of theory and total energy, dipole moment estimation of different V(IV) and Zr(IV) ofloxacin structures. All the synthesized complexes exhibited higher biocidal activity against S. aureus K1, Bacillus subtilis K22, Br. otitidis K76, Escherichia coli K32, Pseudomonas aeruginosa SW1 and Klebsiella oxytoca K42. compared to parent compounds and standard drugs.

  6. Thermal and spectroscopic studies of scandium complex of 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone

    NASA Astrophysics Data System (ADS)

    Akama, Yoshifumi; Sawada, Tadanobu; Ueda, Toyotoshi

    2005-08-01

    The scandium complexes of Sc(PMBP)3·H2O (non-crystal) and Sc(PMBP)3 (crystal) with 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP) were prepared and characterized by thermal analysis, IR, NMR and MS spectroscopies. The crystal structure of the complex, obtained by X-ray analysis, indicates that PMBP is a bidentate ligand in the complex and that the Sc atom is six-coordinate and is in a meridional octahedral environment. The order of the ring current effect on the pyrazolone ring is Sc(PMBP)3 >PMBP(enol)> PMBP(keto). The metal to ligand stoichiometry was found to be 1:3. The crystalline complex melts at 209 °C, followed by degradation at about 310 °C, with the beginning of decomposition. The enthalpy of melting was found to be 61 kJ/mol. On the other hand, the non-crystalline complex was found to change into a crystalline complex at 176 °C with an exothermic reaction before melting at 217 °C. The IR band observed at approximately, 450 cm-1 is possibly due to the stretching of the Sc-O bond.

  7. Spectrophotometric method for the determination, validation, spectroscopic and thermal analysis of diphenhydramine in pharmaceutical preparation.

    PubMed

    Ulu, Sevgi Tatar; Elmali, Fikriye Tuncel

    2010-09-15

    A sensitive, simple and rapid spectrophotometric method was developed for the determination of diphenhydramine in pharmaceutical preparation. The method was based on the charge-transfer complex of the drug, as n-electron donor, with 2,3-dichloro-5,6-dicyano-p-benzoquinone (DDQ), as pi-acceptor. The formation of this complex was also confirmed by UV-vis, FTIR and (1)H NMR spectra techniques and thermal analysis. The proposed method was validated according to the ICH guidelines with respect to linearity, limit of detection, limit of quantification, accuracy, precision, recovery and robustness. The linearity range for concentrations of diphenhydramine was found to be 12.5-150 microg/mL with acceptable correlation coefficients. The detection and quantification limits were found to be 2.09 and 6.27 microg/mL, respectively. The proposed and references methods were applied to the determination of drug in syrup. This preparation were also analyzed with an reference method and statistical comparison by t- and F-tests revealed that there was no significant difference between the results of the two methods with respect to mean values and standard deviations at the 95% confidence level. PMID:20621611

  8. Advanced Spectroscopic and Thermal Imaging Instrumentation for Shock Tube and Ballistic Range Facilities

    NASA Technical Reports Server (NTRS)

    Grinstead, Jay H.; Wilder, Michael C.; Reda, Daniel C.; Cruden, Brett A.; Bogdanoff, David W.

    2010-01-01

    The Electric Arc Shock Tube (EAST) facility and Hypervelocity Free Flight Aerodynamic Facility (HFFAF, an aeroballistic range) at NASA Ames support basic research in aerothermodynamic phenomena of atmospheric entry, specifically shock layer radiation spectroscopy, convective and radiative heat transfer, and transition to turbulence. Innovative optical instrumentation has been developed and implemented to meet the challenges posed from obtaining such data in these impulse facilities. Spatially and spectrally resolved measurements of absolute radiance of a travelling shock wave in EAST are acquired using multiplexed, time-gated imaging spectrographs. Nearly complete spectral coverage from the vacuum ultraviolet to the near infrared is possible in a single experiment. Time-gated thermal imaging of ballistic range models in flight enables quantitative, global measurements of surface temperature. These images can be interpreted to determine convective heat transfer rates and reveal transition to turbulence due to isolated and distributed surface roughness at hypersonic velocities. The focus of this paper is a detailed description of the optical instrumentation currently in use in the EAST and HFFAF.

  9. Pillar-Shaped Macrocyclic Hosts Pillar[n]arenes: New Key Players for Supramolecular Chemistry.

    PubMed

    Ogoshi, Tomoki; Yamagishi, Tada-Aki; Nakamoto, Yoshiaki

    2016-07-27

    In 2008, we reported a new class of pillar-shaped macrocyclic hosts, known as "pillar[n]arenes". Today, pillar[n]arenes are recognized as key players in supramolecular chemistry because of their facile synthesis, unique pillar shape, versatile functionality, interesting host-guest properties, and original supramolecular assembly characteristics, which have resulted in numerous electrochemical and biomedical material applications. In this Review, we have provided historical background to macrocyclic chemistry, followed by a detailed discussion of the fundamental properties of pillar[n]arenes, including their synthesis, structure, and host-guest properties. Furthermore, we have discussed the applications of pillar[n]arenes to materials science, as well as their applications in supramolecular chemistry, in terms of their fundamental properties. Finally, we have described the future perspectives of pillar[n]arene chemistry. We hope that this Review will provide a useful reference for researchers working in the field and inspire discoveries concerning pillar[n]arene chemistry. PMID:27337002

  10. Aminophenyl double decker silsesquioxanes: Spectroscopic elucidation, physical and thermal characterization, and their applications

    NASA Astrophysics Data System (ADS)

    Schoen, Beth Whitney

    The incorporation of cage-like silsesquioxanes (SQ) to form polymers has demonstrated property enhancements in areas such as: thermal and mechanical characteristics, flame retardance, dielectric properties, and oxidative resistance. However, with most hybrid polymers investigated, the attached SQs are pendant with respect to the polymer backbone. A recently developed class of these nano-structured, cage-like silsesquioxanes, formally known as double decker silsesquioxanes (DDSQ), offers the opportunity to form hybrid polymers with SQ cages as a part of the polymer backbone. However, during the capping reaction, these functionalized DDSQs generate cis and trans isomers with respect to the 3D Si-O core. Therefore, it is logical to characterize properties, which will allow for optimization of capping reaction parameters, particularly if one isomer is favored over the other. Moreover, these characteristics are also relevant when reacting or incorporating these isomers, or mixtures thereof, with other molecules to form novel materials. In this dissertation, three aminophenyl DDSQs were synthesized. More specifically, two meta- aminophenyl DDSQs, which were differentiated according to the moiety attached to the D-Si (methyl or cyclohexyl), and one para-aminophenyl DDSQ with a methyl moiety were used. Chemical, physical, and thermal characteristics were evaluated for individual isomers as well as binary mixtures of different cis/trans ratios. The 1H NMR spectra of the cis and trans isomers of these DDSQ had not previously been assigned to a degree that allowed for quantification, which was necessary for these studies. Thus, 1H-29Si HMBC correlations were applied to facilitate 1H spectral assignments and also to confirm previous 29Si assignments. Using 1H NMR not only saves time and material over 29Si NMR, but also provides a more accurate quantification, thus allowing for the ratio of cis and trans isomers present in each compound to be determined. Solubility behavior was

  11. On the structural stability and catalytic properties of smectities pillared with RE-Al, Al-Ga polyoxications

    SciTech Connect

    Caballero, L.; Dominguez, J.M.; De los Santos, J.L.

    1995-12-01

    Pillaring of Smectite type clays offers the possibility to develop highly porous catalytic materials with surface acid properties, (1) their me in hydrotreating and FCC hydrocarbon processes has been extensively discussed (2) and still some research on the stabilization of the clays structure is being carried out. Therefore, the aim of the present work was to investigate thermal stability of Montmorillonite type clays, by means of pillaring with distinct polyoxications and by ion-exchanging and treating the clays under several conditions.

  12. Growing Algae Alter Spectroscopic Characteristics and Chlorine Reactivity of Dissolved Organic Matter from Thermally-Altered Forest Litters.

    PubMed

    Tsai, Kuo-Pei; Chow, Alex T

    2016-08-01

    Previous studies demonstrated that wildfires alter spectroscopic characteristics of terrestrial dissolved organic matter (DOM) and increase specific disinfection byproduct formation potential (SDBP-FP). However, it is unclear whether characteristics of thermally altered DOM (TA-DOM) are altered by biogeochemical processes (e.g., transformed by growing algae) before entering water treatment facilities. The freshwater green algae Pseudokirchneriella subcapitata and blue-green algae Microcystis aeruginosa were separately incubated in the mixture of cultural medium and pine (Pinus palustris) litter-derived TA-DOMs (50 °C, 250 °C, and 400 °C) over 7 days to demonstrate the effects of algal growth on alterations in SDBP-FP. TA-DOM optical characteristics and SDBP-FP were quantified by absorption and fluorescence spectroscopy and chlorination-based DBP-FP experiments. After the inoculation with P. subcapitata, TA-DOM aromaticity (indicated by SUVA254) increased from 1.19 to 1.90 L/mg/m for 50 °C-extract but decreased from 4.95 to 3.75 L/mg/m for 400 °C-extract. The fraction of tyrosine-like components decreased from 25.9 to 9.3% for 50 °C-extract but increased from 0.9 to 1.3% for 400 °C-extract. Same patterns were also observed for M. aeruginosa. Growing algae generally increased chlorine reactivities and formations of trihalomethanes, haloacetonitriles, chloral hydrate, and haloketones. Our data suggest that the biodegradable dissolved organic carbon in TA-DOM decreases as fire intensity (i.e., temperature) increases. Postfire algal blooms can increase chlorine reactivity of fire-affected terrestrial DOM for DBP formation. PMID:27366813

  13. Synthesis, spectroscopic identification, thermal, potentiometric and antibacterial activity studies of 4-amino-5-mercapto-S-triazole Schiff's base complexes

    NASA Astrophysics Data System (ADS)

    Alaghaz, Abdel-Nasser M. A.; Zayed, Mohamed E.; Alharbi, Suliman A.; Ammar, Reda A. A.; Chinnathambi, Arunachalam

    2015-05-01

    Complexes of manganese(II), cobalt(II), nickel(II), copper(II) and zinc(II) of general composition [M(L)2] have been synthesized [L = 4-pyridin-2-yl-methylene amino-4H-1,2,4-triazole-3-thiol]. The elemental analyses, molar conductance, spectral (IR, UV-Vis, 1H NMR, mass), magnetic moment and thermal measurements studies of the compounds led to the conclusion that the ligand acts as a tridentate manner (SNN). The molar conductance of the metal complexes in fresh solution of DMSO lies in the range of 8.34-10.46 Ω-1 cm2 mol-1 indicating their non-electrolytic behavior. On the basis of analytical and spectroscopic techniques, octahedral geometry of the complexes was proposed. The Schiff base acts as tridentate ligand coordinated through deprotonated thiolic sulfur, azomethine nitrogen and pyridine nitrogen atoms. The ligand field parameters were calculated for Co(II), Ni(II) and Cu(II) complexes and their values were found in the range reported for a octahedral structure. The data show that the complexes have composition of ML2 type. The activation of thermodynamic parameters are calculated using Coast-Redfern, Horowitz-Metzger (HM), Piloyan-Novikova (PN) and Broido's equations. Protonation constants of Schiff base and stability constants of their binary metal complexes have been determined potentiometrically in 50% DMSO-water media at 25 °C and ionic strength 0.10 M potassium nitrate. Both the Schiff's base ligand and its complexes have been screened for antibacterial activities.

  14. Water condensation on ultrahydrophobic flexible micro pillar surface

    NASA Astrophysics Data System (ADS)

    Narhe, Ramchandra

    2016-05-01

    We investigated the growth dynamics of water drops in controlled condensation on ultrahydrophobic geometrically patterned polydimethylsiloxane (PDMS) cylindrical micro pillars. At the beginning, the condensed drops size is comparable to the pattern dimensions. The interesting phenomenon we observe is that, as the condensation progresses, water drops between the pillars become unstable and enforced to grow in the upward direction along the pillars surface. The capillary force of these drops is of the order of μ\\text{N} and acts on neighboring pillars. That results into bending of the pillars. Pillars bending enhances the condensation and favors the most energetically stable Wenzel state.

  15. Active containment systems incorporating modified pillared clays

    SciTech Connect

    Lundie, P. |; McLeod, N.

    1997-12-31

    The application of treatment technologies in active containment systems provides a more advanced and effective method for the remediation of contaminated sites. These treatment technologies can be applied in permeable reactive walls and/or funnel and gate systems. The application of modified pillared clays in active containment systems provides a mechanism for producing permeable reactive walls with versatile properties. These pillared clays are suitably modified to incorporate reactive intercalatants capable of reacting with both a broad range of organic pollutants of varying molecular size, polarity and reactivity. Heavy metals can be removed from contaminated water by conventional ion-exchange and other reactive processes within the clay structure. Complex contamination problems can be addressed by the application of more than one modified clay on a site specific basis. This paper briefly describes the active containment system and the structure/chemistry of the modified pillared clay technology, illustrating potential applications of the in-situ treatment process for contaminated site remediation.

  16. Predicting spontaneous heating in coal mine pillars

    SciTech Connect

    Timko, R.J.; Derick, R.L.

    1995-12-31

    This work is a follow-up to previous research that attempted to predict the location of spontaneous heating episodes in underground coal mine pillars. The objective of the original work was to see if the data obtained by commonly used detection methods could accurately predict spontaneous combustion episodes in coal pillars. Data accumulation during the study was enhanced when a spontaneously generated fire occurred within one of the pillars being examined. The fire provided researchers with realistic data that could be used to determine if f ire prediction was possible. Results from the initial study found that the atmospheric status equations that were used provided little advance notice that combustion would occur where it did. This study reevaluated the accumulated data by applying it to recently developed equations and compared these results with previously obtained information to determine if a combination of these techniques could more effectively predict impending combustion.

  17. Effect of sucrose on the thermal denaturation of a protein: An FTIR spectroscopic study of a monoclonal antibody

    NASA Astrophysics Data System (ADS)

    Byler, D. M.; Lee, D. L.; Sokoloski, T. D.; Dal Monte, P. R.; Baldoni, J. M.

    1998-06-01

    The three-dimensional structure of many proteins and complex polypeptides is critically sensitive to the environment to which such a biopolymer is subjected. For example, in some cases lyophilization, which entails a complete cycle of freezing, drying in vacuo, and warming to ambient, brings about unpredictable changes to the secondary structure (conformation). Various research and development groups have suggested that the addition of sucrose or other oligosaccharides to protein solutions prior to lyophilization works to maintain the structural integrity of the native macromolecule. Less information is available, however, with regard to whether or not the presence of sugar inhibits thermal denaturation of proteins in solution. In the present study, FTIR spectroscopic examination of solutions of the monoclonal antibody in D2O suggests that 6% (w/V) added sucrose produces little change in the observed mean temperature of thermal denaturation, Tm~68 °C. Yet, when the protein solution is held at constant temperature in the range between about 60 and 75 °C, the presence of sucrose significantly alters the rate at which the protein unfolds. Based on the disappearance of the strong band near 1634 cm-1 associated with intramolecular β-structure of the native protein, the unfolding process was found to follow first-order kinetics. In the absence of sugar, the slope of a plot of ln (intensity) versus time yielded a first order rate constant of kl=2.65 hr-1 at 69 °C. By contrast, when the protein solution contained 6% sucrose (w/V), kl=1.85 hr-1 at the same temperature. Measuring the rate at different temperatures around Tm indicates that protein solutions containing sucrose unfold more slowly above ~68 °C than does the protein without the excipient. At lower temperatures, however, the opposite is true; the presence of the sugar enhances the rate of denaturation. Arrhenius plots of ln kl versus 1/T indicates that Ea=~600 kJ/mol for the protein alone, but only ~330 k

  18. Manipulating the inter pillar gap in pillar array ultra-thin layer planar chromatography platforms.

    PubMed

    Crane, Nichole A; Lavrik, Nickolay V; Sepaniak, Michael J

    2016-02-21

    An advantage of separation platforms based on deterministic micro- and nano-fabrications, relative to traditional systems based on packed beds of particles, is the exquisite control of all morphological parameters. For example, with planar platforms based on lithographically-prepared pillar arrays, the size, shape, height, geometric arrangement, and inter pillar gaps can be independently adjusted. Since the inter pillar gap is expected to be important in determining resistance to mass transfer in the mobile phase as well as the flow rate, which influences the mass transfer effect and axial diffusion, we herein study the effect of reducing inter pillar gaps on capillary action-based flow and band dispersion. Atomic layer deposition is used to narrow the gap between the pillars for photo-lithographically defined pillar arrays. The plate height of gap-adjusted arrays is modeled based on predicted and observed flow rates. A reduction in the flow rate with smaller gaps hinders the efficiency in the modeled case and is correlated with actual separations. A conclusion is drawn that simultaneously reducing both the gap and the pillar diameter is the best approach in terms of improving the chromatographic efficiency. PMID:26824088

  19. Microstructural Evolution of Cu/Solder/Cu Pillar-Type Structures with Different Diffusion Barriers

    NASA Astrophysics Data System (ADS)

    Cheng, Hsi-Kuei; Lin, Yu-Jie; Chen, Chih-Ming; Liu, Kuo-Chio; Wang, Ying-Lang; Liu, Tzeng-Feng

    2016-08-01

    Microstructural evolution of the Cu/solder/Cu pillar-type bonding structures with a reduced solder volume subjected to thermal aging at 423 K to 473 K(150 °C to 200 °C) was investigated. In a bonding structure employing a Ni single layer as the diffusion barrier, solder was consumed with formation of the Ni3Sn4 phase at the bonding interfaces due to an usual Sn/Ni interfacial reaction. However, an unusual Sn/Cu reaction occurred with formation of the Cu6Sn5 (and Cu3Sn) phase on the periphery of the Cu pillar due to out-diffusion of Sn toward the pillar periphery. Consumption of solder was accelerated by the above two reactions which led to the formation of a continuous gap in the bonding structure. Employment of a thicker Ni layer plus a Cu cap layer as the diffusion barrier in the bonding structure effectively blocked out-diffusion of Sn toward the periphery of the Cu pillar and therefore retarded the gap formation. The retardation effect was attributed to an increment of diffusion distance on the pillar periphery due to an effective diffusion barrier composed by Ni and thicker Cu-Sn (Cu6Sn5 + Cu3Sn) phase layers. Detailed phase identification and microstructural evolution in the bonding structures were also investigated using scanning electron microscopy and transmission electron microscopy.

  20. Microstructural Evolution of Cu/Solder/Cu Pillar-Type Structures with Different Diffusion Barriers

    NASA Astrophysics Data System (ADS)

    Cheng, Hsi-Kuei; Lin, Yu-Jie; Chen, Chih-Ming; Liu, Kuo-Chio; Wang, Ying-Lang; Liu, Tzeng-Feng

    2016-06-01

    Microstructural evolution of the Cu/solder/Cu pillar-type bonding structures with a reduced solder volume subjected to thermal aging at 423 K to 473 K(150 °C to 200 °C) was investigated. In a bonding structure employing a Ni single layer as the diffusion barrier, solder was consumed with formation of the Ni3Sn4 phase at the bonding interfaces due to an usual Sn/Ni interfacial reaction. However, an unusual Sn/Cu reaction occurred with formation of the Cu6Sn5 (and Cu3Sn) phase on the periphery of the Cu pillar due to out-diffusion of Sn toward the pillar periphery. Consumption of solder was accelerated by the above two reactions which led to the formation of a continuous gap in the bonding structure. Employment of a thicker Ni layer plus a Cu cap layer as the diffusion barrier in the bonding structure effectively blocked out-diffusion of Sn toward the periphery of the Cu pillar and therefore retarded the gap formation. The retardation effect was attributed to an increment of diffusion distance on the pillar periphery due to an effective diffusion barrier composed by Ni and thicker Cu-Sn (Cu6Sn5 + Cu3Sn) phase layers. Detailed phase identification and microstructural evolution in the bonding structures were also investigated using scanning electron microscopy and transmission electron microscopy.

  1. Fabrication of MnO 2-pillared layered manganese oxide through an exfoliation/reassembling and oxidation process

    NASA Astrophysics Data System (ADS)

    Yuan, Jiaqi; Liu, Zong-Huai; Qiao, Shanfeng; Ma, Xiangrong; Xu, Naicai

    MnO 2-pillared layered manganese oxide has been first fabricated by a delamination/reassembling process followed by oxidation reaction and then by heat treatment. The structural evolution of MnO 2-pillared layered manganese oxide has been characterized by XRD, SEM, DSC-GTA, IR and N 2 adsorption-desorption. MnO 2-pillared layered manganese oxide shows a relative high thermal stability and mesoporous characteristic. The layered structure with a basal spacing of 0.66 nm could be maintained up to 400 °C. The electrochemical properties of the synthesized MnO 2-pillared layered manganese oxide have been studied using cyclic voltammetry in a mild aqueous electrolyte. Sample MnO 2-BirMO (300 °C) shows good capacitive behavior and cycling stability, and the specific capacitance value is 206 F g -1.

  2. Practical design methods for barrier pillars. Information circular/1995

    SciTech Connect

    Koehler, J.R.; Tadolini, S.C.

    1995-11-01

    Effective barrier pillar design is essential for safe and productive underground coal mining. This U.S. Bureau of Mines report presents an overview of available barrier pillar design methodologies that incorporate sound engineering principles while remaining practical for everyday usage. Nomographs and examples are presented to assist in the determination of proper barrier pillar sizing. Additionally, performance evaluation techniques and criteria are included to assist in determining the effectiveness of selected barrier pillar configurations.

  3. Method of underground mining by pillar extraction

    DOEpatents

    Bowen, Ray J.; Bowen, William R.

    1980-08-12

    A method of sublevel caving and pillar and top coal extraction for mining thick coal seams includes the advance mining of rooms and crosscuts along the bottom of a seam to a height of about eight feet, and the retreat mining of the top coal from the rooms, crosscuts and portions of the pillars remaining from formation of the rooms and cross-cuts. In the retreat mining, a pocket is formed in a pillar, the top coal above the pocket is drilled, charged and shot, and then the fallen coal is loaded by a continuous miner so that the operator remains under a roof which has not been shot. The top coal from that portion of the room adjacent the pocket is then mined, and another pocket is formed in the pillar. The top coal above the second pocket is mined followed by the mining of the top coal of that portion of the room adjacent the second pocket, all by use of a continuous miner which allows the operator to remain under a roof portion which has not been shot.

  4. Elastocapillary coalescence of plates and pillars

    PubMed Central

    Wei, Z.; Schneider, T. M.; Kim, J.; Kim, H.-Y.; Aizenberg, J.; Mahadevan, L.

    2015-01-01

    When a fluid-immersed array of supported plates or pillars is dried, evaporation leads to the formation of menisci on the tips of the plates or pillars that bring them together to form complex patterns. Building on prior experimental observations, we use a combination of theory and computation to understand the nature of this instability and its evolution in both the two- and three-dimensional setting of the problem. For the case of plates, we explicitly derive the interaction torques based on the relevant physical parameters associated with pillar deformation, contact-line pinning/depinning and fluid volume changes. A Bloch-wave analysis for our periodic mechanical system captures the window of volumes where the two-plate eigenvalue characterizes the onset of the coalescence instability. We then study the evolution of these binary clusters and their eventual elastic arrest using numerical simulations that account for evaporative dynamics coupled to capillary coalescence. This explains both the formation of hierarchical clusters and the sensitive dependence of the final structures on initial perturbations, as seen in our experiments. We then generalize our analysis to treat the problem of pillar collapse in three dimensions, where the fluid domain is completely connected and the interface is a minimal surface with the uniform mean curvature. Our theory and simulations capture the salient features of experimental observations in a range of different situations and may thus be useful in controlling the ensuing patterns. PMID:25792949

  5. Construction of microcanonical entropy on thermodynamic pillars.

    PubMed

    Campisi, Michele

    2015-05-01

    A question that is currently highly debated is whether the microcanonical entropy should be expressed as the logarithm of the phase volume (volume entropy, also known as the Gibbs entropy) or as the logarithm of the density of states (surface entropy, also known as the Boltzmann entropy). Rather than postulating them and investigating the consequence of each definition, as is customary, here we adopt a bottom-up approach and construct the entropy expression within the microcanonical formalism upon two fundamental thermodynamic pillars: (i) The second law of thermodynamics as formulated for quasistatic processes: δQ/T is an exact differential, and (ii) the law of ideal gases: PV=k(B)NT. The first pillar implies that entropy must be some function of the phase volume Ω. The second pillar singles out the logarithmic function among all possible functions. Hence the construction leads uniquely to the expression S=k(B)lnΩ, that is, the volume entropy. As a consequence any entropy expression other than that of Gibbs, e.g., the Boltzmann entropy, can lead to inconsistencies with the two thermodynamic pillars. We illustrate this with the prototypical example of a macroscopic collection of noninteracting spins in a magnetic field, and show that the Boltzmann entropy severely fails to predict the magnetization, even in the thermodynamic limit. The uniqueness of the Gibbs entropy, as well as the demonstrated potential harm of the Boltzmann entropy, provide compelling reasons for discarding the latter at once. PMID:26066159

  6. 30 CFR 75.386 - Final mining of pillars.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 30 Mineral Resources 1 2011-07-01 2011-07-01 false Final mining of pillars. 75.386 Section 75.386... MANDATORY SAFETY STANDARDS-UNDERGROUND COAL MINES Ventilation § 75.386 Final mining of pillars. When only one mine opening is available due to final mining of pillars, no more than 20 miners at a time...

  7. 30 CFR 75.386 - Final mining of pillars.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 30 Mineral Resources 1 2013-07-01 2013-07-01 false Final mining of pillars. 75.386 Section 75.386... MANDATORY SAFETY STANDARDS-UNDERGROUND COAL MINES Ventilation § 75.386 Final mining of pillars. When only one mine opening is available due to final mining of pillars, no more than 20 miners at a time...

  8. 30 CFR 75.386 - Final mining of pillars.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 30 Mineral Resources 1 2010-07-01 2010-07-01 false Final mining of pillars. 75.386 Section 75.386... MANDATORY SAFETY STANDARDS-UNDERGROUND COAL MINES Ventilation § 75.386 Final mining of pillars. When only one mine opening is available due to final mining of pillars, no more than 20 miners at a time...

  9. 30 CFR 75.386 - Final mining of pillars.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 30 Mineral Resources 1 2014-07-01 2014-07-01 false Final mining of pillars. 75.386 Section 75.386... MANDATORY SAFETY STANDARDS-UNDERGROUND COAL MINES Ventilation § 75.386 Final mining of pillars. When only one mine opening is available due to final mining of pillars, no more than 20 miners at a time...

  10. 30 CFR 75.386 - Final mining of pillars.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 30 Mineral Resources 1 2012-07-01 2012-07-01 false Final mining of pillars. 75.386 Section 75.386... MANDATORY SAFETY STANDARDS-UNDERGROUND COAL MINES Ventilation § 75.386 Final mining of pillars. When only one mine opening is available due to final mining of pillars, no more than 20 miners at a time...

  11. Design methods to control violent pillar failures in room-and-pillar mines

    SciTech Connect

    Zipf, R.K. Jr.; Mark, C.

    1996-12-01

    The sudden, violent collapse of large areas of room-and-pillar mines poses a special hazard to miners and mine operators. This type of failure, termed a {open_quotes}Cascading Pillar Failure{close_quotes} (CPF), occurs when one pillar in a mine layout fails transfering its load to neighboring pillars causing them to fail, and so forth. Recent examples of this kind of failure in coal, metal and nonmetal mines in the U.S. are documented. Mining engineers can limit the danger posed by these failures through improved mine design practices. Whether failure occurs in a slow, nonviolent manner or in a rapid, violent manner is governed by the local mine stiffness stability criterion. This stability criterion is used as the basis for three design approaches to control cascading pillar failure in room-and-pillar mines, namely, the containment approach, the prevention approach, and the full extraction mining approach. These design approaches are illustrated with practical examples for coal mining.

  12. A theoretical description of elastic pillar substrates in biophysical experiments.

    PubMed

    Mohrdieck, Camilla; Wanner, Alexander; Roos, Wouter; Roth, Alexander; Sackmann, Erich; Spatz, Joachim P; Arzt, Eduard

    2005-08-12

    Arrays of elastic pillars are used in biophysical experiments as sensors for traction forces. The evaluation of the forces can be complicated if they are coupled to the pillar displacements over large distances. This is the case if many of the pillars are interconnected by elastic linkages as, for example, in fiber networks that are grown on top of pillars. To calculate the traction forces in such a network, we developed a set of nonlinear inhomogeneous equations relating the forces in the linking elements to the resulting pillar deflections. We chose a homogeneous, activated two-dimensional network of cytoskeletal actin filaments to illustrate that a pillar substrate is generally not a force sensor but a force-gradient sensor. In homogeneous networks the forces acting along the filaments can be approximated by analyzing only pillar deflections in the edge zones of the substrate and by integration over the corresponding force gradients. PMID:16082672

  13. Pillared montmorillonite catalysts for coal liquefaction

    SciTech Connect

    Sharma, R.K.; Olson, E.S.

    1994-12-31

    Pillared clays contain large micropores and have considerable potential for catalytic hydrogenation and cleavage of coal macromolecules. Pillared montmorillonite-supported catalysts were prepared by the intercalation of polynuclear hydroxychromium cations and subsequent impregnation of nickel and molybdenum. Infrared and thermogravimetric studies of pyridine-adsorbed catalysts indicated the presence of both Lewis and Bronsted acid sites. Thus, the catalysts have both acidic properties that can aid in hydrocracking and cleavage of carbon-heteroatom bonds as well as hydrogen-activating bimetallic sites. These catalysts were applied to the hydrodesulfurization and liquefaction of coal-derived intermediates. The reactions of model organosulfur compounds and coal liquids were carried out at 300{degrees}-400{degrees}C for 3 hours in the presence of 1000 psi of molecular hydrogen. Reaction products were analyzed by GC/FT-IR/MS/AED. The catalysts have been found to be very effective in removing sulfur from model compounds as well as liquefaction products.

  14. Radionuclide separations using pillared layered materials

    SciTech Connect

    Schroeder, N.C.; Wade, K.L.; Morgan, D.M.

    1998-12-31

    This is the final report of a two-year Laboratory Directed Research and Development (LDRD) project at the Los Alamos National Laboratory (LANL). Pillared Layered Materials (PLMs) are layered inorganic ion exchangers propped apart by metal oxide pillars. PLMs have been synthesized to sorb strontium from liquid nuclear wastes. A study that compared over 60 sorbers for their ability to sorb strontium from Hanford simulants showed that PLMs were the best sorbers; strontium distribution coefficients ({sup Sr}K{sub d}) > 20000 mL/g were obtained. In addition, PLMs showed a high degree of selectivity for strontium over cesium, transition metals, lanthanides and actinides. The sorption of strontium is, however, inhibited by complexants (EDTA); {sup Sr}K{sub d} values drop to <20 mL/g when they are present. The most promising PLMs were the Cr, Ti, Zr, and Si pillared tantalum tungstate. The K{sub d} values for Sr{sup 2+} and Ba{sup 2+} show a strong pH dependence; K{sub d} values increase to >10{sup 4} above pH 12. The general surface complexation mechanism explains the sorption of these cations on PLMs.

  15. Pillars for the care of older persons in the Caribbean.

    PubMed

    Powell, Dorothy L; Price, Addie J; Burns, Faith A; McConnell, Eleanor S; Hendrix, Cristina C; McWhinney-Dehaney, Leila; Lombardi, Marilyn M

    2012-01-01

    Pillars for the Care of Older Persons in the Caribbean: A Comprehensive Community-Based Framework (Pillars) is a hybrid of multiple public health frameworks developed through community-based participatory research processes. Health and social service professionals, governmental organizations, elderly persons, and others from across the English-speaking Caribbean countries developed the Pillars framework to address the growing elderly population and with an aim to increase the number of healthy and active years of life. The Pillars framework consists of four interrelated pillars organized across multiple sectors of society: primary care with care management; integrated services coordination; population-based health promotion and disease prevention; and planning and accountability. Pillars is enabled by an envisioned integrated system of information technology that will increase community-based services delivery, interprofessional communication and coordination, and will aggregate data with all identifiers removed for surveillance, planning, forecasting, policy making, evaluation, and research. PMID:22211755

  16. Radionuclide separations using pillared layered materials. Final report

    SciTech Connect

    Clearfield, A.

    1995-08-31

    The objective of this project is to prepare an all inorganic strontium specific sorbent or ion exchanger for the removal of highly alkaline nuclear waste solutions. A series of clays and layered titanates were pillared and calcined to convert their essentially two dimensional structure to three dimensional porous structures with high surface areas. The pillaring agents were alumina, zirconia, chromia and silica based. The pillared clays, particularly those containing Zr pillars, achieved moderate (Kd as high at 13,700 ml/g with V:m = 28) selectivities for Sr{sup 2+}. In contrast, the silica pillared titanates showed exceptional affinities for Sr{sup 2+} with Kd values in excess of 100,000 ml/g in 5M NaNO{sup 3} + 1M NaOH. These latter results suggest a more detailed study of the pillared titanates in the presence of simulants closely resembling real waste solutions.

  17. Study of Transport Behavior and Conversion Efficiency in Pillar Structured Neutron Detectors

    SciTech Connect

    Nikolic, R

    2007-04-26

    Room temperature, high efficiency and scalable radiation detectors can be realized by manipulating materials at the micro scale. With micro-semiconductor-pillars, we will advance the thermal neutron detection efficiency of semiconductor detectors to over 70% with 50 mm in detector thickness. New material science, new transport behavior, neutron to alpha conversion dynamics and their relationship with neutron detection will be discovered with the proposed structures.

  18. Mid-infrared silicon pillar waveguides

    NASA Astrophysics Data System (ADS)

    Singh, Neetesh; Hudson, Darren D.; Eggleton, Benjamin J.

    2015-12-01

    In this work silicon pillar waveguides have been proposed to exploit the entire transparent window of silicon. These geometries posses a broad and at dispersion (from 2 to 6 μm) with four zero dispersion wavelengths. We calculate supercontinuum generation spanning over two octaves (2 to >8 μm) with long wavelengths interacting weakly with the lossy substrate. These structures have higher mode confinement in the silicon - away from the substrate, which makes them substrate independent and are promising for exploring new nonlinear phenomena and highly sensitive molecular sensing over the entire silicon's transparency range

  19. Catalytic Wastewater Treatment Using Pillared Clays

    NASA Astrophysics Data System (ADS)

    Perathoner, Siglinda; Centi, Gabriele

    After introduction on the use of solid catalysts in wastewater treatment technologies, particularly advanced oxidation processes (AOPs), this review discussed the use of pillared clay (PILC) materials in three applications: (i) wet air catalytic oxidation (WACO), (ii) wet hydrogen peroxide catalytic oxidation (WHPCO) on Cu-PILC and Fe-PILC, and (iii) behavior of Ti-PILC and Fe-PILC in the photocatalytic or photo-Fenton conversion of pollutants. Literature data are critically analyzed to evidence the main direction to further investigate, in particularly with reference to the possible practical application of these technologies to treat industrial, municipal, or agro-food production wastewater.

  20. Synthesis, spectroscopic, thermal and antimicrobial investigations of charge-transfer complexes formed from the drug procaine hydrochloride with quinol, picric acid and TCNQ

    NASA Astrophysics Data System (ADS)

    Adam, Abdel Majid A.

    2012-12-01

    Intermolecular charge-transfer or proton-transfer complexes between the drug procaine hydrochloride (PC-HCl) as a donor and quinol (QL), picric acid (PA) or 7,7',8,8'-tetracyanoquinodimethane (TCNQ) as a π-acceptor have been synthesized and spectroscopically studied in methanol at room temperature. Based on elemental analyses and photometric titrations, the stoichiometry of the complexes (donor:acceptor molar ratios) was determined to be 1:1 for all three complexes. The formation constant (KCT), molar extinction coefficient (ɛCT) and other spectroscopic data have been determined using the Benesi-Hildebrand method and its modifications. The newly synthesized CT complexes have been characterized via elemental analysis, IR, Raman, 1H NMR, and electronic absorption spectroscopy. The morphological features of these complexes were investigated using scanning electron microscopy (SEM), and the sharp, well-defined Bragg reflections at specific 2θ angles have been identified from the powder X-ray diffraction patterns. Thermogravimetric analyses (TGAs) and kinetic thermodynamic parameters were also used to investigate the thermal stability of the synthesized solid CT complexes. Finally, the CT complexes were screened for their antibacterial and antifungal activities against various bacterial and fungal strains, and only the complex obtained using picric acid exhibited moderate antibacterial activity against all of the tested strains.

  1. An RDL UBM Structural Design for Solving Ultralow- K Delamination Problem of Cu Pillar Bump Flip Chip BGA Packaging

    NASA Astrophysics Data System (ADS)

    Chen, K. M.; Wu, C. Y.; Wang, C. H.; Cheng, H. C.; Huang, N. C.

    2014-11-01

    Copper (Cu) pillar bumps tend to induce high thermal-mechanical stress during environmental tests and fabrication processes due to the high hardness of Cu, especially when applied with an ultralow- K (ULK) chip. A previous experiment showed that interfacial delamination was often observed in the ULK layers of conventional Cu pillar bump-type flip chip ball grid array (FCBGA) packages under thermal cycling, where under bump metallurgy (UBM) layers directly sit on the metal pads of silicon chips (herein termed ``direct UBM structure''). In this study, a UBM pad relocation scheme through redistribution layer (RDL) technology (herein termed ``RDL UBM structure'') is proposed to relieve the stress or ULK delamination issue. The proposed technique is tested on Cu pillar bump-type FCBGA packages subjected to thermal loading, the effectiveness of which is demonstrated through finite element stress simulation and experimental reliability tests. Simulation results reveal that the RDL UBM structure can greatly reduce the maximum stress in the ULK layers by as much as about 10% to 44%. Besides, it turns out that the Cu pillar bump-type FCBGA packages with the RDL UBM structure show good interconnect reliability performance in terms of thermal cycling, highly accelerated stress, and high-temperature storage.

  2. Supercapacitors based on pillared graphene nanostructures.

    PubMed

    Lin, Jian; Zhong, Jiebin; Bao, Duoduo; Reiber-Kyle, Jennifer; Wang, Wei; Vullev, Valentine; Ozkan, Mihrimah; Ozkan, Cengiz S

    2012-03-01

    We describe the fabrication of highly conductive and large-area three dimensional pillared graphene nanostructure (PGN) films from assembly of vertically aligned CNT pillars on flexible copper foils for applications in electric double layer capacitors (EDLC). The PGN films synthesized via a one-step chemical vapor deposition process on flexible copper foils exhibit high conductivity with sheet resistance as low as 1.6 ohms per square and possessing high mechanical flexibility. Raman spectroscopy indicates the presence of multi walled carbon nanotubes (MWCNT) and their morphology can be controlled by the growth conditions. It was discovered that nitric acid treatment can significantly increase the specific capacitance of the devices. EDLC devices based on PGN electrodes (surface area of 565 m2/g) demonstrate enhanced performance with specific capacitance value as high as 330 F/g extracted from the current density-voltage (CV) measurements and energy density value of 45.8 Wh/kg. The hybrid graphene-CNT nanostructures are attractive for applications including supercapacitors, fuel cells and batteries. PMID:22754980

  3. Synthesis, structure and photoluminescent behavior of a novel pillar-layered {Zn3}-based metal-organic framework

    NASA Astrophysics Data System (ADS)

    Song, Xue-Zhi; Mu, Wen-Sheng; Han, Bing-Yan; Yan, Yang

    2016-09-01

    A novel 3D metal-organic framework (MOF) {[Zn3(bpdc)3 (p-4-bpmb)](DMF)2}n ( 1) (H2bpdc=biphenyl-4,4‧-dicarboxylic acid; p-4-bpmb=1,4-bis(pyridine-4-ylmethoxy)benzene) has been solvothermally synthesized and structurally characterized. Compound 1 exhibits a 3D pillar-layered framework based on the trinuclear {Zn3} building blocks, consisting of Zn-dicarboxylate layers and bipyridyl-derivative pillars. Furthermore, it features three-fold interpenetrating 8-connected hex-type topology. In addition, its thermal stability and luminescent property have also been investigated.

  4. High aspect ratio composite structures with 48.5% thermal neutron detection efficiency

    SciTech Connect

    Shao, Q.; Voss, L. F.; Conway, A. M.; Nikolic, R. J.; Dar, M. A.; Cheung, C. L.

    2013-02-11

    The pillar structured thermal neutron detector is based on the combination of high aspect ratio silicon p-i-n pillars surrounded by the neutron converter material {sup 10}B. By etching high aspect ratio pillar structures into silicon, the result is a device that efficiently absorbs the thermal neutron flux by accommodating a large volume fraction of {sup 10}B within the silicon pillar array. Here, we report a thermal neutron detection efficiency of 48.5% using a 50 {mu}m pillar array with an aspect ratio of 25:1.

  5. Synthesis, spectroscopic characterisation, thermal analysis, DNA interaction and antibacterial activity of copper(I) complexes with N, N‧- disubstituted thiourea

    NASA Astrophysics Data System (ADS)

    Chetana, P. R.; Srinatha, B. S.; Somashekar, M. N.; Policegoudra, R. S.

    2016-02-01

    copper(I) complexes [Cu(4MTU)2Cl] (2), [Cu(4MTU) (B)Cl] (3), [Cu(6MTU)2Cl] (5) and [Cu(6MTU) (B)Cl] (6) where 4MTU = 1-Benzyl-3-(4-methyl-pyridin-2-yl)-thiourea (1) and 6MTU = 1-Benzyl-3-(6-methyl-pyridin-2-yl)-thiourea (4), B is a N,N-donor heterocyclic base, viz. 1,10-phenanthroline (phen 3, 6), were synthesized, characterized by various physico-chemical and spectroscopic techniques. The elemental analysis suggests that the stoichiometry to be 1:2 (metal:ligand) for 2, 5 1:1:1 (metal:ligand:B) for 3, 6. X-ray powder diffraction illustrates that the complexes have crystalline nature. IR data coupled with electronic spectra and molar conductance values suggest that the complex 2, 5 show the presence of a trigonal planar geometry and the complex 3, 6 show the presence of a tetrahedral geometry about the Cu(I) centre. The binding affinity towards calf thymus (CT) DNA was determined using UV-Vis, fluorescence spectroscopic titrations and viscosity studies. These studies showed that the tested phen complexes 3, 6 bind moderately (in the order of 105 M-1) to CT DNA. The complex 2, 5 does not show any apparent binding to the DNA and hence poor cleavage efficiency. Complex 3, 6 shows efficient oxidative cleavage of plasmid DNA in the presence of H2O2 involving hydroxyl radical species as evidenced from the control data showing inhibition of DNA cleavage in the presence of DMSO and KI. The in vitro antibacterial assay indicates that these complexes are good antimicrobial agents against various pathogens. Anti-bacterial activity is higher when thiourea coordinates to metal ion than the thiourea alone.

  6. Spectroscopic ellipsometry study of the effect of illumination and thermal annealing on the optical constants of thin Ge-As-S films

    NASA Astrophysics Data System (ADS)

    Pamukchieva, V.; Szekeres, A.; Arsova, D.

    2011-02-01

    The effects of illumination and post-illumination thermal annealing on the optical properties of chalcogenide thin (~150 nm) films were studied by spectroscopic ellipsometry. The films were thermally evaporated from Ge30.8As5.7S63.5 and Ge32As5S63 glasses. They were exposed to illumination with an HBO 500 lamp and to subsequent thermal annealing at a temperature of 350 °C. Ellipsometric measurements in the spectral range 300-820 nm were carried out after each technological step. From the ellipsometric data analysis the optical constants (n, k, ɛ), optical band gap energy Eog and film thickness have been determined, while the oscillator energies E0 and Ed have been estimated applying the single-oscillator approximation theory. In the ɛ2 spectra three peaks, denoted by E1, E2 and E3, have appeared, which are attributed to interband transitions. By illumination, the values of the complex refractive index (\\tilde n = n - {\\rm{i}}k), dielectric function (\\skew3\\tilde \\varepsilon = \\varepsilon _1 - {\\rm{i}}\\varepsilon _{\\rm{2}} ) and dispersion energy Ed decrease, whereas the band gap energy (Eog) and the oscillator energy (E0) values increase. All these are accompanied by a ~12-13% enhancement of film thickness. Thermal annealing leads to a further increase of the energetic parameters values, but causes a ~14-15% decrease of film thickness in comparison to that of illuminated films. The E1 and E2 peaks diminish on illumination and post-illumination annealing, whereas the magnitude of the E3 peak decreases on illumination and increases by annealing, approaching its initial value for the as-deposited state.

  7. Biomechanical Characterization of Cardiomyocyte Using PDMS Pillar with Microgrooves.

    PubMed

    Oyunbaatar, Nomin-Erdene; Lee, Deok-Hyu; Patil, Swati J; Kim, Eung-Sam; Lee, Dong-Weon

    2016-01-01

    This paper describes the surface-patterned polydimethylsiloxane (PDMS) pillar arrays for enhancing cell alignment and contraction force in cardiomyocytes. The PDMS micropillar (μpillar) arrays with microgrooves (μgrooves) were fabricated using a unique micro-mold made using SU-8 double layer processes. The spring constant of the μpillar arrays was experimentally confirmed using atomic force microscopy (AFM). After culturing cardiac cells on the two different types of μpillar arrays, with and without grooves on the top of μpillar, the characteristics of the cardiomyocytes were analyzed using a custom-made image analysis system. The alignment of the cardiomyocytes on the μgrooves of the μpillars was clearly observed using a DAPI staining process. The mechanical force generated by the contraction force of the cardiomyocytes was derived from the displacement of the μpillar arrays. The contraction force of the cardiomyocytes aligned on the μgrooves was 20% higher than that of the μpillar arrays without μgrooves. The experimental results prove that applied geometrical stimulus is an effective method for aligning and improving the contraction force of cardiomyocytes. PMID:27517924

  8. Periodically structured Si pillars for high-performing heterojunction photodetectors

    NASA Astrophysics Data System (ADS)

    Melvin David Kumar, M.; Yun, Ju-Hyung; Kim, Joondong

    2015-03-01

    A periodical array of silicon (Si) micro pillar structures was fabricated on Si substrates using PR etching process. Indium tin oxide (ITO) layer of 80 nm thickness was deposited over patterned Si substrates so as to make ITO/n-Si heterojunction devices. The influences of width and period of pillars on the optical and electrical properties of prepared devices were investigated. The surface morphology of the Si substrates revealed the uniform array of pillar structures. The 5/10 (width/period) Si pillar pattern reduced the optical reflectance to 6.5% from 17% which is of 5/7 pillar pattern. The current rectifying ratio was found higher for the device in which the pillars are situated in optimum periods. At both visible (600 nm) and near infrared (900 nm) range of wavelengths, the 5/7 and 5/10 pillar patterned device exhibited the better photoresponses which are suitable for making advanced photodetectors. This highly transmittance and photoresponsive pillar patterned Si substrates with an ITO layer would be a promising device for various photoelectric applications.

  9. 43 CFR 3931.100 - Boundary pillars and buffer zones.

    Code of Federal Regulations, 2013 CFR

    2013-10-01

    ... 43 Public Lands: Interior 2 2013-10-01 2013-10-01 false Boundary pillars and buffer zones. 3931... EXPLORATION AND LEASES Plans of Development and Exploration Plans § 3931.100 Boundary pillars and buffer zones... prior written consent or on the BLM's order. For in-situ operations, a 50-foot buffer zone from...

  10. 43 CFR 3931.100 - Boundary pillars and buffer zones.

    Code of Federal Regulations, 2012 CFR

    2012-10-01

    ... 43 Public Lands: Interior 2 2012-10-01 2012-10-01 false Boundary pillars and buffer zones. 3931... EXPLORATION AND LEASES Plans of Development and Exploration Plans § 3931.100 Boundary pillars and buffer zones... prior written consent or on the BLM's order. For in-situ operations, a 50-foot buffer zone from...

  11. 43 CFR 3931.100 - Boundary pillars and buffer zones.

    Code of Federal Regulations, 2011 CFR

    2011-10-01

    ... 43 Public Lands: Interior 2 2011-10-01 2011-10-01 false Boundary pillars and buffer zones. 3931... AND LEASES Plans of Development and Exploration Plans § 3931.100 Boundary pillars and buffer zones. (a... prior written consent or on the BLM's order. For in-situ operations, a 50-foot buffer zone from...

  12. 43 CFR 3931.100 - Boundary pillars and buffer zones.

    Code of Federal Regulations, 2014 CFR

    2014-10-01

    ... 43 Public Lands: Interior 2 2014-10-01 2014-10-01 false Boundary pillars and buffer zones. 3931... EXPLORATION AND LEASES Plans of Development and Exploration Plans § 3931.100 Boundary pillars and buffer zones... prior written consent or on the BLM's order. For in-situ operations, a 50-foot buffer zone from...

  13. Ten Pillars of a Good Childhood: A Finnish Perspective

    ERIC Educational Resources Information Center

    Pulkkinen, Lea

    2012-01-01

    The organizers of the Decade for Childhood have formulated Ten Pillars of a Good Childhood as basic requirements for an optimal childhood. The pillars can be used to analyze the quality of childhood in homes and nations, and to guide policies and practices related to the experience of childhood. In this article, the author shall illustrate, pillar…

  14. Fabrication of nano-structured hemispheres and pillars using laterally migrating polymer templates.

    PubMed

    Nam, Hye Jin; Yi, Gi-Ra; Jeong, Seong-Hun; Boo, Jin-Hyo; Jung, Duk-Young

    2009-10-01

    We report herein a reliable method of fabricating 2D periodic gold nanopillars with well-defined anisotropic shapes by the combinational actions of colloidal crystals and gold evaporation. The deposition of gold on a polymer template produced dual functional Janus-like nanopillars up to 633 nm in height as well as hemispherical shells with 120 nm. The thermal-induced active migration of the nanopillars from the pristine position in the lateral direction occurred at the colloidal defects while some cavity space was formed inside the gold pillars. The nano-structured gold pillars exhibited a strong surface plasmon resonance at 598 nm, as compared to that of the solid gold nanospheres at 520 nm, and a noticeable red shift to 640 nm was induced by the removal of the polymer template. PMID:19908488

  15. Numerical Modeling for Yield Pillar Design: A Case Study

    NASA Astrophysics Data System (ADS)

    Li, Wenfeng; Bai, Jianbiao; Peng, Syd; Wang, Xiangyu; Xu, Ying

    2015-01-01

    Two single-entry gateroad systems employing a yield pillar for bump control in a Chinese coal mine were introduced. The overburden depth of the longwall panels was approximately 390 m. When the width/height (W/H) ratio of the yield pillar was 2.67, coal bumps in the tailgate occurred in front of the longwall retreating face. However, in another panel, the coal bump was eliminated because the W/H ratio was reduced to 1.67. Under this condition, instrumentation results indicated that the roof-to-floor and rib-to-rib convergences reached 1,050 and 790 mm, respectively, during longwall retreat. The numerical model was used to back-analyze the two cases of yield pillar application in the hope to find the principle for yield pillar design. In order to improve the reliability of the numerical model, the strain-hardening gob and strain-softening pillar materials were meticulously calibrated, and the coal/rock interface strength was determined by laboratory direct shear tests. The results of the validated model indicate that if the W/H ratio of the yield pillar equals 1.67, the peak vertical stress in the panel rib (37.7 MPa) is much larger than that in the yield pillar (21.1 MPa); however, the peak vertical stress in the panel rib (30.87 MPa) is smaller than that in the yield pillar (36 MPa) when the W/H ratio of yield pillar is 2.67. These findings may be helpful to the design of yield pillars for bump control.

  16. Thermal, spectroscopic and laser properties of Nd3+ in gadolinium scandium gallium garnet crystal produced by optical floating zone method

    NASA Astrophysics Data System (ADS)

    Tian, Li; Wang, Shuxian; Wu, Kui; Wang, Baolin; Yu, Haohai; Zhang, Huaijin; Cai, Huaqiang; Huang, Hui

    2013-12-01

    A neodymium-doped gadolinium scandium gallium garnet (Nd:GSGG) single crystal with dimensions of Φ 5 × 20 mm2 has been grown by means of optical floating zone (OFZ). X-ray powder diffraction (XRPD) result shows that the as-grown Nd:GSGG crystal possesses a cubic structure with space group Ia3d and a cell parameter of a = 1.2561 nm. Effective elemental segregation coefficients of the Nd:GSGG as-grown crystal were calculated by using X-ray fluorescence (XRF). The thermal properties of the Nd:GSGG crystal were systematically studied by measuring the specific heat, thermal expansion and thermal diffusion coefficient, and the thermal conductivity of this crystal was calculated. The absorption and luminescence spectra of Nd:GSGG were measured at room temperature (RT). By using the Judd-Ofelt (J-O) theory, the theoretical radiative lifetime was calculated and compared with the experimental result. Continuous wave (CW) laser performance was achieved with the Nd:GSGG at the wavelength of 1062 nm when it was pumped by a laser diode (LD). A maximum output power of 0.792 W at 1062 nm was obtained with a slope efficiency of 11.89% under a pump power of 7.36 W, and an optical-optical conversion efficiency of 11.72%.

  17. Two-dimensional infrared spectroscopic study on the thermally induced structural changes of glutaraldehyde-crosslinked collagen

    NASA Astrophysics Data System (ADS)

    Tian, Zhenhua; Wu, Kun; Liu, Wentao; Shen, Lirui; Li, Guoying

    2015-04-01

    The thermal stability of collagen solution (5 mg/mL) crosslinked by glutaraldehyde (GTA) [GTA/collagen (w/w) = 0.5] was measured by differential scanning calorimetry and Fourier transform infrared spectroscopy (FTIR), and the thermally induced structural changes were analyzed using two-dimensional (2D) correlation spectra. The denaturation temperature (Td) and enthalpy change (ΔH) of crosslinked collagen were respectively about 27 °C and 88 J/g higher than those of native collagen, illuminating the thermal stability increased. With the increase of temperature, the red-shift of absorption bands and the decreased AIII/A1455 value obtained from FTIR spectra indicated that hydrogen bonds were weakened and the unwinding of triple helix occurred for both native and crosslinked collagens; whereas the less changes in red-shifting and AIII/A1455 values for crosslinked collagen also confirmed the increase in thermal stability. Additionally, the 2D correlation analysis provided information about the thermally induced structural changes. In the 2D synchronous spectra, the intensities of auto-peaks at 1655 and 1555 cm-1, respectively assigned to amide I band (Cdbnd O stretching vibration) and amide II band (combination of Nsbnd H bending and Csbnd N stretching vibrations) in helical conformation were weaker for crosslinked collagen than those for native collagen, indicating that the helical structure of crosslinked collagen was less sensitive to temperature. Moreover, the sequence of the band intensity variations showed that the band at 1555 cm-1 moved backwards owing to the addition of GTA, demonstrating that the response of helical structure of crosslinked collagen to the increased temperature lagged. It was speculated that the stabilization of collagen by GTA was due to the reinforcement of triple helical structure.

  18. Two-dimensional infrared spectroscopic study on the thermally induced structural changes of glutaraldehyde-crosslinked collagen.

    PubMed

    Tian, Zhenhua; Wu, Kun; Liu, Wentao; Shen, Lirui; Li, Guoying

    2015-04-01

    The thermal stability of collagen solution (5 mg/mL) crosslinked by glutaraldehyde (GTA) [GTA/collagen (w/w)=0.5] was measured by differential scanning calorimetry and Fourier transform infrared spectroscopy (FTIR), and the thermally induced structural changes were analyzed using two-dimensional (2D) correlation spectra. The denaturation temperature (Td) and enthalpy change (ΔH) of crosslinked collagen were respectively about 27°C and 88 J/g higher than those of native collagen, illuminating the thermal stability increased. With the increase of temperature, the red-shift of absorption bands and the decreased AIII/A1455 value obtained from FTIR spectra indicated that hydrogen bonds were weakened and the unwinding of triple helix occurred for both native and crosslinked collagens; whereas the less changes in red-shifting and AIII/A1455 values for crosslinked collagen also confirmed the increase in thermal stability. Additionally, the 2D correlation analysis provided information about the thermally induced structural changes. In the 2D synchronous spectra, the intensities of auto-peaks at 1655 and 1555 cm(-1), respectively assigned to amide I band (CO stretching vibration) and amide II band (combination of NH bending and CN stretching vibrations) in helical conformation were weaker for crosslinked collagen than those for native collagen, indicating that the helical structure of crosslinked collagen was less sensitive to temperature. Moreover, the sequence of the band intensity variations showed that the band at 1555 cm(-1) moved backwards owing to the addition of GTA, demonstrating that the response of helical structure of crosslinked collagen to the increased temperature lagged. It was speculated that the stabilization of collagen by GTA was due to the reinforcement of triple helical structure. PMID:25617846

  19. Vibrational spectroscopic characterization of mudstones in a hydrocarbon-bearing depression, South China Sea: Implications for thermal maturity evaluation

    NASA Astrophysics Data System (ADS)

    Liu, Entao; Song, Yinxian; Wang, Hua; Liu, Haibo; Ayoko, Godwin A.; Frost, Ray L.; Xi, Yunfei

    2016-01-01

    A better understanding of mineral transformations in sedimentary rocks and the controls on thermal maturity have become essential in the petroleum exploration industry in recent years. The Fushan Depression is an important hydrocarbon-bearing depression in South China Sea, which can be subdivided into three structural zones: the western, central and eastern zones. In this study, a series of mudstone samples selected from 13 drilling cores with depths ranging from 2100 to 3800 m were studied using infrared reflectance spectroscopy and X-Ray Powder Diffraction (XRD) methods. And another 10 samples have been chosen for vitrinite reflectance measurement so as to investigate the ability of using infrared spectroscopy for thermal maturity evaluations. The infrared spectra results show that quartz and silicates (e.g. illite, kaolinite, smectite) are the dominant minerals in all samples. The semi-quantitative XRD analysis reveals a clear trend in illite content as the eastern zone (mean 80.81%) > the western zone (mean 73.52%) > the central zone (mean 55.04%) as well as a contrary trend in kaolinite content. This study documents that the peak height and position of Si-O antisymmetric stretching bands at ~ 1025 cm- 1 and ~ 1000 cm- 1 have a significant correlation with the degree of kaolinite illitization, suggesting that the utility of infrared spectroscopy is a valuable tool for the study of thermal maturity in sedimentary basins. The infrared spectra and XRD results together with vitrinite reflectance data indicate that the thermal maturity in the eastern zone is anomalously high, followed by the western zone, and that in the central zone is lowest. The igneous intrusion in the eastern zone has a significant impact on thermal maturation, resulting in high degree of kaolinite illitization. By contrast, the abundance in kaolinite in the central zone represents relatively low degree of kaolinite illitization, which should be attributed to shallow burial depth.

  20. Vibrational spectroscopic characterization of mudstones in a hydrocarbon-bearing depression, South China Sea: Implications for thermal maturity evaluation.

    PubMed

    Liu, Entao; Song, Yinxian; Wang, Hua; Liu, Haibo; Ayoko, Godwin A; Frost, Ray L; Xi, Yunfei

    2016-01-15

    A better understanding of mineral transformations in sedimentary rocks and the controls on thermal maturity have become essential in the petroleum exploration industry in recent years. The Fushan Depression is an important hydrocarbon-bearing depression in South China Sea, which can be subdivided into three structural zones: the western, central and eastern zones. In this study, a series of mudstone samples selected from 13 drilling cores with depths ranging from 2100 to 3800 m were studied using infrared reflectance spectroscopy and X-Ray Powder Diffraction (XRD) methods. And another 10 samples have been chosen for vitrinite reflectance measurement so as to investigate the ability of using infrared spectroscopy for thermal maturity evaluations. The infrared spectra results show that quartz and silicates (e.g. illite, kaolinite, smectite) are the dominant minerals in all samples. The semi-quantitative XRD analysis reveals a clear trend in illite content as the eastern zone (mean 80.81%)>the western zone (mean 73.52%)>the central zone (mean 55.04%) as well as a contrary trend in kaolinite content. This study documents that the peak height and position of Si-O antisymmetric stretching bands at ~1025 cm(-1) and ~1000 cm(-1) have a significant correlation with the degree of kaolinite illitization, suggesting that the utility of infrared spectroscopy is a valuable tool for the study of thermal maturity in sedimentary basins. The infrared spectra and XRD results together with vitrinite reflectance data indicate that the thermal maturity in the eastern zone is anomalously high, followed by the western zone, and that in the central zone is lowest. The igneous intrusion in the eastern zone has a significant impact on thermal maturation, resulting in high degree of kaolinite illitization. By contrast, the abundance in kaolinite in the central zone represents relatively low degree of kaolinite illitization, which should be attributed to shallow burial depth. PMID:26318698

  1. Synthesis, spectroscopic characterization and thermal behavior of metal complexes formed with N'-(1-(4-hydroxyphenyl) ethylidene)-2-oxo-2-(phenylamino) acetohydrazide (H 3OPAH)

    NASA Astrophysics Data System (ADS)

    Ahmed, Sara F.; El-Gammal, Ola A.; El-Reash, Gaber Abu

    2011-12-01

    Complexes of Co(II), Ni(II), Cu(II), Mn(II), Cd(II), Zn(II), Hg(II) and U(IV)O 22+ with N'-(1-(4-hydroxyphenyl) ethylidene)-2-oxo-2-(phenylamino) acetohydrazide (H 3OPAH) are reported and have been characterized by various spectroscopic techniques like IR, UV-visible, 1H NMR and ESR as well as magnetic and thermal (TG and DTA) measurements. It is found that the ligand behaves as a neutral bidentate, monoanionic tridentate or tetradentate and dianionic tetradentate. An octahedral geometry for [Mn(H 3OPAH) 2Cl 2], [Co 2(H 2OPAH) 2Cl 2(H 2O) 4] and [(UO 2) 2(HOPAH)(OAc) 2(H 2O) 2] complexes, a square planar geometry for [Cu 2(H 2OPAH)Cl 3(H 2O)]H 2O complex, a tetrahedral structure for [Cd(H 3OPAH)Cl 2], [Zn(H 3OPAH)(OAc) 2] and [Hg(H 3OPAH)Cl 2]H 2O complexes. The binuclear [Ni 2(HOPAH)Cl 2(H 2O) 2]H 2O complex contains a mixed geometry of both tetrahedral and square planar structures. The protonation constants of ligand and stepwise stability constants of its complexes at 298, 308 and 318 K as well as the thermodynamic parameters are being calculated. The bond lengths, bond angles, HOMO, LUMO and dipole moments have been calculated to confirm the geometry of the ligand and the investigated complexes. Also, thermal properties and decomposition kinetics of all compounds are investigated. The interpretation, mathematical analysis and evaluation of kinetic parameters ( Ea, A, Δ H, Δ S and Δ G) of all thermal decomposition stages have been evaluated using Coats-Redfern and Horowitz-Metzger methods.

  2. Spectroscopic, thermal and cw dual-wavelength laser characteristics of Nd:LaF3 single crystal

    NASA Astrophysics Data System (ADS)

    Hong, Jiaqi; Zhang, Lianhan; Li, Jing; Wang, Zhaowei; He, Jingliang; Zhang, Peixiong; Wang, Yaqi; Hang, Yin

    2016-03-01

    A Nd-doped LaF3 crystal was grown by Czochralski method, and the rocking curves of (0 0 2) and (1 1 0) diffraction planes show good crystallinity quality of the as-grown crystal. Room-temperature fluorescence spectrum and transmittance spectrum of Nd:LaF3 crystal were investigated, both indicating probable dual-wavelength emissions at ∼1.04 μm and ∼1.06 μm. The thermal diffusivity and thermal conductivity of Nd:LaF3 crystal were detailed studied. Cw dual-wavelength laser operation of Nd:LaF3 single crystal at 1040 nm and around 1065 nm with LD pumping was demonstrated. A maximum output power of 302 mW was obtained with a slope efficiency of about 18.5% with respect to the pump power. The results of our study indicate the Nd:LaF3 crystal a promising laser crystal.

  3. Determination of the succinonitrile-benzene and succinonitrile-cyclohexanol phase diagrams by thermal and UV spectroscopic analysis

    NASA Technical Reports Server (NTRS)

    Kaukler, W. F.; Frazier, D. O.; Facemire, B.

    1984-01-01

    Equilibrium temperature-composition diagrams were determined for the two organic systems, succinonitrile-benzene and succinonitrile-cyclohexanol. Measurements were made using the common thermal analysis methods and UV spectrophotometry. Succinonitrile-benzene monotectic was chosen for its low affinity for water and because UV analysis would be simplified. Succinonitrile-cyclohexanol was chosen because both components are transparent models for metallic solidification, as opposed to the other known succinonitrile-based monotectics.

  4. Chemical Degradation of Siloxane Stress Cushions (M97 and S5370) by Thermal, Mechanical and Spectroscopic Investigations

    SciTech Connect

    Maxwell, R S; Gee, R; Balazs, B; Cohenour, R; Sung, B

    2002-04-19

    We are currently investigating the long term aging of weapon organics in an effort to develop predictive capabilities for functional service life. As part of this effort, we have been studying multimechanism aging of M97 and 53370 stress cushions. Ionizing radiation, thermal degradation, and desiccation all affect the crosslink density and motional dynamics and thus the engineering performance of these materials. Our approach has been to develop molecular level understanding of the effects of such aging mechanisms on polymer properties by a combined approach utilizing solvent swelling, thermal, DMA, molecular modeling, and solid state NMR. This presentation will offer a survey of our current work, concentrating on the application of solid state NMR for correlating structure and polymer dynamics. An overview of the relationships between crosslink density, NMR relaxation times, polymer chain dynamics, and storage modulus measurements will be presented and the advantages of NMR will be discussed. It will be shown that silicone based polymers tend to crosslink upon exposure to {gamma}-radiation, undergo chain scission upon thermal degradation, and stiffen upon desiccation.

  5. Ring-shaped polariton lasing in pillar microcavities

    SciTech Connect

    Kalevich, V. K. Afanasiev, M. M.; Lukoshkin, V. A.; Kavokin, K. V.; Tsintzos, S. I.; Savvidis, P. G.; Kavokin, A. V.

    2014-03-07

    Optically generated exciton-polaritons in cylindric semiconductor pillar microcavity with embedded GaAs/AlGaAs quantum wells demonstrate a clear polariton lasing regime. When exciting in the center of the pillar, we detect a ring-shaped emission, where the peak of intensity can be separated from the excitation spot by more than 10 μm. The spatial coherence of the ring emission is verified by interferometry measurements. These observations are interpreted by drift of the exciton polariton condensate away from the excitation spot due to its repulsion from the exciton reservoir and by its spatial confinement by the pillar boundary.

  6. Thermal analysis and vibrational spectroscopic characterization of the boro silicate mineral datolite - CaBSiO4(OH)

    NASA Astrophysics Data System (ADS)

    Frost, Ray L.; Xi, Yunfei; Scholz, Ricardo; Lima, Rosa Malena Fernandes; Horta, Laura Frota Campos; Lopez, Andres

    2013-11-01

    The objective of this work is to determine the thermal stability and vibrational spectra of datolite CaBSiO4(OH) and relate these properties to the structure of the mineral. The thermal analysis of datolite shows a mass loss of 5.83% over a 700-775 °C temperature range. This mass loss corresponds to 1 water (H2O) molecules pfu. A quantitative chemical analysis using electron probe was undertaken. The Raman spectrum of datolite is characterized by bands at 917 and 1077 cm-1 assigned to the symmetric stretching modes of BO and SiO tetrahedra. A very intense Raman band is observed at 3498 cm-1 assigned to the stretching vibration of the OH units in the structure of datolite. BOH out-of-plane vibrations are characterized by the infrared band at 782 cm-1. The vibrational spectra are based upon the structure of datolite based on sheets of four- and eight-membered rings of alternating SiO4 and BO3(OH) tetrahedra with the sheets bonded together by calcium atoms.

  7. Thermal and plasma enhanced atomic layer deposition of TiO{sub 2}: Comparison of spectroscopic and electric properties

    SciTech Connect

    Das, Chittaranjan Henkel, Karsten; Tallarida, Massimo; Schmeißer, Dieter; Gargouri, Hassan; Kärkkänen, Irina; Schneidewind, Jessica; Gruska, Bernd; Arens, Michael

    2015-01-15

    Titanium oxide (TiO{sub 2}) deposited by atomic layer deposition (ALD) is used as a protective layer in photocatalytic water splitting system as well as a dielectric in resistive memory switching. The way ALD is performed (thermally or plasma-assisted) may change the growth rate as well as the electronic properties of the deposited films. In the present work, the authors verify the influence of the ALD mode on functional parameters, by comparing the growth rate and electronic properties of TiO{sub 2} films deposited by thermal (T-) and plasma-enhanced (PE-) ALD. The authors complete the study with the electrical characterization of selected samples by means of capacitance–voltage and current–voltage measurements. In all samples, the authors found a significant presence of Ti{sup 3+} states, with the lowest content in the PE-ALD grown TiO{sub 2} films. The observation of Ti{sup 3+} states was accompanied by the presence of in-gap states above the valence band maximum. For films thinner than 10 nm, the authors found also a strong leakage current. Also in this case, the PE-ALD films showed the weakest leakage currents, showing a correlation between the presence of Ti{sup 3+} states and leakage current density.

  8. Transition metal complexes of Vanillin- 4N-(2-pyridyl) thiosemicarbazone (H 2VPT); thermal, structural and spectroscopic studies

    NASA Astrophysics Data System (ADS)

    El-Reash, Gaber Abu; El-Ayaan, Usama; Gabr, I. M.; El-Rachawy, El-Bastawesy

    2010-04-01

    The present work carried out a study on the ligational behavior of the new ligand, Vanillin- 4N-(2-pyridyl) thiosemicarbazone (H 2VPT) 1 towards some transition metal ions namely, Mn 2+, Co 2+, Ni 2+, Cu 2+, Zn 2+,Cd 2+, Hg 2+ and U 6+. These complexes namely [Mn(HVPT)Cl] 2, [Co(VPT)(H 2O)] 2H 2O 3, [Ni(HVPT)Cl(H 2O)] 4, [Cu(HVPT)Cl(H 2O)] 5, [Zn(VPT)(H 2O)]H 2O 6, [Cd(HVPT)Cl(H 2O)] 7, [Hg(VPT)(H 2O)]H 2O 8 and [UO 2(H 2VPT)(OAc) 2]H 2O 9, were characterized by elemental analysis, spectral (IR, 1H NMR and UV-vis) and magnetic moment measurements. The suggested structures were confirmed by applying geometry optimization and conformational analysis. Thermal properties and decomposition kinetics of all compounds are investigated. The interpretation, mathematical analysis and evaluation of kinetic parameters ( E, A, Δ H, Δ S and Δ G) of all thermal decomposition stages have been evaluated using Coats-Redfern equation. ESR spectra of [Cu(HVPT)Cl]H 2O at room temperature show broad signal, indicating spin-exchange interactions between copper(II) ions.

  9. Growth, Structure, Thermal Properties and Spectroscopic Characteristics of Nd3+-Doped KGdP4O12 Crystal

    PubMed Central

    Sun, Tongqing; Zhang, Yu; Shan, Pai; Zhang, Zichang; Chen, Shaolin; Kong, Yongfa; Xu, Jingjun

    2014-01-01

    A single crystal of Nd3+-doped KGdP4O12 was successfully grown with the top-seeded solution growth and slow cooling (TSSG−SC) technique. It crystallizes in space group C2/c with cell parameters a = 7.812(2) Å, b = 12.307(3) Å, c = 10.474(2) Å, β = 110.84(3)° and Z = 4. The IR and Raman spectra also indicated that the phosphoric polyhedra of Nd:KGdP4O12 has a cyclic symmetry. The chemical composition of the crystal was analyzed and the distribution coefficient of Nd3+ was calculated. The crystal morphology of KGdP4O12 was identified using X-ray diffraction. The compound has good thermal stability to 920°C. Its specific heat and thermal conductivity were determined for potential applications. The spectral properties of Nd:KGdP4O12 indicates that it exhibits broad absorption and emission bands, which are attributed to low symmetry of the crystal. The broad absorption band around 798 nm has a full-width at half-maximum (FWHM) of 14.8 nm and is suitable for AlGaAs laser diode pumping. Moreover, 5 at% Nd3+-doped KGdP4O12 crystal has a long luminescence lifetime of 300 μs and a high quantum efficiency of 96%. PMID:24968165

  10. Graphitic carbon nanospheres: A Raman spectroscopic investigation of thermal conductivity and morphological evolution by pulsed laser irradiation

    NASA Astrophysics Data System (ADS)

    Agarwal, Radhe; Sahoo, Satyaprakash; Chitturi, Venkateswara Rao; Katiyar, Ram S.

    2015-12-01

    Graphitic carbon nanospheres (GCNSs) were prepared by a unique acidic treatment of multi-walled nanotubes. Spherical morphology with a narrow size distribution was confirmed by transmission electron microscopy studies. The room temperature Raman spectra showed a clear signature of D- and G-peaks at around 1350 and 1591 cm-1, respectively. Temperature dependent Raman scattering measurements were performed to understand the phonon dynamics and first order temperature coefficients related to the D- and G-peaks. The temperature dependent Raman spectra in a range of 83-473 K were analysed, where the D-peak was observed to show a red-shift with increasing temperature. The relative intensity ratio of D- to G-peaks also showed a significant rise with increasing temperature. Such a temperature dependent behaviour can be attributed to lengthening of the C-C bond due to thermal expansion in material. The estimated value of the thermal conductivity of GCNSs ˜0.97 W m-1 K-1 was calculated using Raman spectroscopy. In addition, the effect of pulsed laser treatment on the GCNSs was demonstrated by analyzing the Raman spectra of post irradiated samples.

  11. Structure investigation of three hydrazones Schiff's bases by spectroscopic, thermal and molecular orbital calculations and their biological activities

    NASA Astrophysics Data System (ADS)

    Belal, Arafa A. M.; Zayed, M. A.; El-Desawy, M.; Rakha, Sh. M. A. H.

    2015-03-01

    Three Schiff's bases AI (2(1-hydrazonoethyl)phenol), AII (2, 4-dibromo 6-(hydrazonomethyl)phenol) and AIII (2(hydrazonomethyl)phenol) were prepared as new hydrazone compounds via condensation reactions with molar ratio (1:1) of reactants. Firstly by reaction of 2-hydroxy acetophenone solution and hydrazine hydrate; it gives AI. Secondly condensation between 3,5-dibromo-salicylaldehyde and hydrazine hydrate gives AII. Thirdly condensation between salicylaldehyde and hydrazine hydrate gives AIII. The structures of AI-AIII were characterized by elemental analysis (EA), mass (MS), FT-IR and 1H NMR spectra, and thermal analyses (TG, DTG, and DTA). The activation thermodynamic parameters, such as, ΔE∗, ΔH∗, ΔS∗ and ΔG∗ were calculated from the TG curves using Coats-Redfern method. It is important to investigate their molecular structures to know the active groups and weak bond responsible for their biological activities. Consequently in the present work, the obtained thermal (TA) and mass (MS) practical results are confirmed by semi-empirical MO-calculations (MOCS) using PM3 procedure. Their biological activities have been tested in vitro against Escherichia coli, Proteus vulgaris, Bacillissubtilies and Staphylococcus aurous bacteria in order to assess their anti-microbial potential.

  12. Graphitic carbon nanospheres: A Raman spectroscopic investigation of thermal conductivity and morphological evolution by pulsed laser irradiation

    SciTech Connect

    Agarwal, Radhe; Sahoo, Satyaprakash E-mail: rkatiyar@hpcf.upr.edu; Chitturi, Venkateswara Rao; Katiyar, Ram S. E-mail: rkatiyar@hpcf.upr.edu

    2015-12-07

    Graphitic carbon nanospheres (GCNSs) were prepared by a unique acidic treatment of multi-walled nanotubes. Spherical morphology with a narrow size distribution was confirmed by transmission electron microscopy studies. The room temperature Raman spectra showed a clear signature of D- and G-peaks at around 1350 and 1591 cm{sup −1}, respectively. Temperature dependent Raman scattering measurements were performed to understand the phonon dynamics and first order temperature coefficients related to the D- and G-peaks. The temperature dependent Raman spectra in a range of 83–473 K were analysed, where the D-peak was observed to show a red-shift with increasing temperature. The relative intensity ratio of D- to G-peaks also showed a significant rise with increasing temperature. Such a temperature dependent behaviour can be attributed to lengthening of the C-C bond due to thermal expansion in material. The estimated value of the thermal conductivity of GCNSs ∼0.97 W m{sup −1} K{sup −1} was calculated using Raman spectroscopy. In addition, the effect of pulsed laser treatment on the GCNSs was demonstrated by analyzing the Raman spectra of post irradiated samples.

  13. Structure investigation of three hydrazones Schiff's bases by spectroscopic, thermal and molecular orbital calculations and their biological activities.

    PubMed

    Belal, Arafa A M; Zayed, M A; El-Desawy, M; Rakha, Sh M A H

    2015-03-01

    Three Schiff's bases AI (2(1-hydrazonoethyl)phenol), AII (2, 4-dibromo 6-(hydrazonomethyl)phenol) and AIII (2(hydrazonomethyl)phenol) were prepared as new hydrazone compounds via condensation reactions with molar ratio (1:1) of reactants. Firstly by reaction of 2-hydroxy acetophenone solution and hydrazine hydrate; it gives AI. Secondly condensation between 3,5-dibromo-salicylaldehyde and hydrazine hydrate gives AII. Thirdly condensation between salicylaldehyde and hydrazine hydrate gives AIII. The structures of AI-AIII were characterized by elemental analysis (EA), mass (MS), FT-IR and (1)H NMR spectra, and thermal analyses (TG, DTG, and DTA). The activation thermodynamic parameters, such as, ΔE(∗), ΔH(∗), ΔS(∗) and ΔG(∗) were calculated from the TG curves using Coats-Redfern method. It is important to investigate their molecular structures to know the active groups and weak bond responsible for their biological activities. Consequently in the present work, the obtained thermal (TA) and mass (MS) practical results are confirmed by semi-empirical MO-calculations (MOCS) using PM3 procedure. Their biological activities have been tested in vitro against Escherichia coli, Proteus vulgaris, Bacillissubtilies and Staphylococcus aurous bacteria in order to assess their anti-microbial potential. PMID:25437844

  14. Pillared and open-framework uranyl diphosphonates

    SciTech Connect

    Adelani, Pius O.; Albrecht-Schmitt, Thomas E.

    2011-09-15

    The hydrothermal reactions of uranium trioxide, uranyl acetate, or uranyl nitrate with 1,4-benzenebisphosphonic acid in the presence of very small amount of HF at 200 deg. C results in the formation of three different uranyl diphosphonate compounds, [H{sub 3}O]{sub 2}{l_brace}(UO{sub 2}){sub 6}[C{sub 6}H{sub 4}(PO{sub 3})(PO{sub 2}OH)]{sub 2}[C{sub 6}H{sub 4}(PO{sub 2}OH){sub 2}]{sub 2}[C{sub 6}H{sub 4}(PO{sub 3}){sub 2}]{r_brace}(H{sub 2}O){sub 2} (Ubbp-1), [H{sub 3}O]{sub 4}{l_brace}(UO{sub 2}){sub 4}[C{sub 6}H{sub 4}(PO{sub 3}){sub 2}]{sub 2}F{sub 4}{r_brace}.H{sub 2}O (Ubbp-2), and {l_brace}(UO{sub 2})[C{sub 6}H{sub 2}F{sub 2}(PO{sub 2}OH){sub 2}(H{sub 2}O){r_brace}{sub 2}.H{sub 2}O (Ubbp-3). The crystal structures of these compounds were determined by single crystal X-ray diffraction experiments. Ubbp-1 consists of UO{sub 7} pentagonal bipyramids that are bridged by the phosphonate moieties to form a three-dimensional pillared structure. Ubbp-2 is composed of UO{sub 5}F{sub 2} pentagonal bipyramids that are bridged through the phosphonate oxygen atoms into one-dimensional chains that are cross-linked by the phenyl spacers into a pillared structure. The structure of Ubbp-3 is a three-dimensional open-framework with large channels containing water molecules with internal dimensions of approximately 10.9x10.9 A. Ubbp-1 and Ubbp-2 fluoresce at room temperature. - Graphical Abstract: Illustration of the three-dimensional open-framework structure of {l_brace}(UO{sub 2})[C{sub 6}H{sub 2}F{sub 2}(PO{sub 2}OH){sub 2}(H{sub 2}O){r_brace}{sub 2}.H{sub 2}O viewed along the c-axis. The structure is constructed from UO{sub 7} units, pentagonal bipyramids=green, oxygen=red, phosphorus=magenta, carbon=black, hydrogen=white. Highlights: > The influence of the uranyl salt anions and pH were critically examined in relation to structural variation. > The acetate and nitrate counter ions of uranyl may be acting as structure directing agents. > The use of rigid phenyl spacer yield

  15. Synthesis and photocatalytic performances of the TiO2 pillared montmorillonite.

    PubMed

    Chen, Daimei; Zhu, Qian; Zhou, Fengsan; Deng, Xutao; Li, Fatang

    2012-10-15

    TiO(2) pillared clay materials were prepared by montmorillonite (Mt) and acidic solutions of hydrolyzed Ti alkoxides in the presence of high-molecular-weight polyoxypropylene (POP)-backboned di-quaternary salts (POP). The as-prepared materials were characterized by means of XRD, FTIR, TG-DTA, XRF, specific surface area and porosity determinations, TEM and SEM, respectively. The experiments showed that the resulting material was a porous delaminated structure containing pillared fragments and nano-scaled TiO(2) particles well dispersed among each other. Introducing polymer surfactant POP as an expanding agent of Mt cannot only promote the formation of the delaminated structure, but significantly improve the porosity and surface area of the composites. The resulting TiO(2) pillared Mt exhibited a good thermal stability as indicated by its surface area after calcination at 800 °C. No phase transformation from anatase to rutile was observed even under calcination at 900 °C. The grain size of anatase in as-prepared sample decreased with the increase of the POP concentration, but increased with the increment of calcination temperature. The photocatalytic performances of these new porous materials were evaluated by using methylene blue degradation. The composite solid exhibited superior photocatalyic property and the maximum removal efficiency was up to 98% within 90 min. PMID:22884731

  16. Iron oxide pillared clay with large gallery height: Synthesis and properties as a Fischer-Tropsch catalyst

    SciTech Connect

    Rightor, E.G.; Tsou, Mingshin; Pinnavaia, T.J. )

    1991-07-01

    New iron oxide pillared montmorillonites have been prepared by the reaction of Na{sup +} montmorillonite with base-hydrolyzed solutions of Fe{sup 3+} salts and subsequent thermal conversion of the intercalated polycations. Depending on the hydrolysis conditions used to generate the pillaring solutions, pillared products with basal spacings in the range 18 to 25 {angstrom} were obtained. Under optimum hydrolysis conditions (base/metal = 2.0 meq/mol, aging time = 23-147 hr) the pillared products contained 6.8-9.8 Fe{sup 3+} ions per O{sub 20}(OH){sub 4} unit cell and exhibited basal spacings of 25-29 {angstrom}. These latter spacings corresponded to exceptionally large gallery heights of 15-19 {angstrom}. Upon calcination at 300C, the spacings decreased to 23-27 {angstrom}. N{sub 2} BET surface areas after outgassing at 350C were in the range 270 to 350 m{sup 2}/g. The pillared products are active catalysts that have undergone Fischer-Tropsch synthesis of hydrocarbons at 275 C and 120 {minus}psi (CO:H{sub 2}=1:2). The hydrocarbon distribution in the C{sub 1}-C{sub 6} range (1.3% conversion) followed Anderson-Schulz-Flory statistics with a chain propagation probability of {alpha} = 0.49. X-ray energy dispersive analysis indicated that substantial amounts of the intercalated iron migrated to the edge sites of the clay particles under reaction conditions. The redistribution of iron resulted in a distribution of gallery heights sufficiently heterogeneous to preclude Bragg X-ray scattering along the 001 direction. Iron migration also occurred upon exposure of the pillared products to the ambient atmosphere for prolonged periods ({ge}3 months).

  17. Thermal stability of electron-irradiated poly(tetrafluoroethylene) - X-ray photoelectron and mass spectroscopic study

    NASA Technical Reports Server (NTRS)

    Wheeler, Donald R.; Pepper, Stephen V.

    1990-01-01

    Polytetrafluoroethylene (PTFE) was subjected to 3 keV electron bombardment and then heated in vacuum to 300 C. The behavior of the material as a function of radiation dose and temperature was studied by X-ray photoelectron spectroscopy (XPS) of the surface and mass spectroscopy of the species evolved. Lightly damaged material heated to 300 C evolved saturated fluorocarbon species, whereas unsaturated fluorocarbon species were evolved from heavily damaged material. After heating the heavily damaged material, those features in the XPS spectrum that were associated with damage diminished, giving the appearance that the radiation damage had annealed. The observations were interpreted by incorporating mass transport of severed chain fragments and thermal decomposition of severely damaged material into the branched and cross-linked network model of irradiated PTFE. The apparent annealing of the radiation damage was due to covering of the network by saturated fragments that easily diffused through the decomposed material to the surface region upon heating.

  18. Thermal and Electron Irradiation Processing of Outer SolarSystem Ice Simulants: Chemical and Spectroscopic Laboratory Characterization

    NASA Astrophysics Data System (ADS)

    Poston, Michael; Mahjoub, Ahmed; Hand, Kevin; Carlson, Robert; Brown, Mike; Blacksberg, Jordana; Eiler, John; Hodyss, Robert; Carey, Elizabeth; Ehlmann, Bethany

    2014-11-01

    Our team is examining the effects of energetic radiation and thermal cycling on pure and mixed solar system ices under ultra-high vacuum conditions. These ices are being examined in search of markers that are unique to a specific thermal or radiation history, with specific interest in simulating histories believed to be relevant to Jupiter Trojan asteroids and Kuiper Belt Objects. A key telescopic observation of the Trojan asteroids is that they have a bimodal distribution of spectral slopes in the visible and near infrared regions. One population exhibits very red spectral slopes, while the other moderately red slopes. This distribution may point to differing formation locations and dynamical histories between the two populations. The ices are deposited on a cryogenic stage at temperatures appropriate to outer solar system objects. Of specific interest are water, methanol, hydrogen sulfide, and ammonia, which are simple ice constituents that together contain the most common reactive elements found in ices. Electron irradiation has been conducted, with plans to irradiate with other particle sources as well. The ices are examined by reflectance spectroscopy in the visible through mid infrared while a quadrapole mass spectrometer monitors the vacuum chamber background for any desorbed or sputtered neutral products. All mixtures analyzed thus far have shown the appearance of new bands and disappearance of others during irradiation and formation of a residue that did not sublime upon heating to 300 Kelvin. This work has been supported by the Keck Institute for Space Studies (KISS). The research described here was carried out at the Jet Propulsion Laboratory, Caltech, under a contract with the National Aeronautics and Space Administration (NASA) and at the Caltech Division of Geological and Planetary Sciences.

  19. Synthesis, spectroscopic studies, thermal analyses, biological activity of tridentate coordinated transition metal complexes of bi(pyridyl-2-ylmethyl)amine]ligand

    NASA Astrophysics Data System (ADS)

    Abd El-Halim, Hanan F.; Mohamed, Gehad G.

    2016-01-01

    A new tridentate acyclic pincer ligand, [bi(pyridin-2-methyl)amine] (bpma, HL), was synthesized and reacted to form complexes with copper(II), nickel(II), iron(II), cobalt(II) and zinc(II) ions. Both the ligand and its complexes were characterized using elemental analysis, molar conductance, infrared, 1H-NMR-spectroscopy, mass and thermal analyses. According to the spectroscopic data, all of the complexes share the same coordination environment around the metal atoms, consisting two nitrogen-pyridine entities, one nitrogen-methylamine entity, one/two water molecules and/or one/two chloride or bromide ions. Complexes also showed molar conductivity according to the presence of two halide anions outer the coordination sphere except Co(II) and Zn(II) complexes are non electrolytes. Analysis indicates that the metal ions have trigonal bipyramidal structure. Cu(II), Ni(II), Fe(II), Co(II), and Zn(II) metal complexes were screened for their antibacterial activity against Bacillus subtilis, Staphylococcus aureus (G+) and Escherichia coli, and Pseudomonas aeruginosa (G-) bacteria. They showed remarkable antimicrobial activity.

  20. Synthesis, spectroscopic, thermal and antimicrobial studies of neodymium(III) and samarium(III) complexes derived from tetradentate ligands containing N and S donor atoms.

    PubMed

    Ain, Qurratul; Pandey, S K; Pandey, O P; Sengupta, S K

    2015-04-01

    Trivalent lanthanide complexes of the type [Ln(L)Cl(H2O)2] (where Ln=Nd(III) or Sm(III) and LH2=Schiff bases derived by the condensation of 3-(phenyl/substitutedphenyl)-4-amino-5-mercapto-1,2,4-triazole with diacetyl/benzil) have been synthesized by the reactions of anhydrous lanthanide(III) chloride with Schiff bases in methanol. The structures of the complexes have been proposed on the basis of elemental analysis, electrical conductance, magnetic moment, spectroscopic measurements (IR, 1H, 13C NMR and UV-vis spectra) and X-ray diffraction studies. The spectral data reveal that the Schiff base ligands behave as dibasic tetradentate chelating agents having coordination sites at two thiol sulfur atoms and two azomethine nitrogen atoms. The presence of coordinated water in metal complexes was confirmed by thermal and IR data of the complexes. All the Schiff bases and their metal complexes have also been screened for their antibacterial activity against Bacillus subtilis, Staphylococcus aureus and antifungal activities against Aspergillus niger, Curvularia pallescens and Colletotrichum capsici. PMID:25579799

  1. Synthesis, spectroscopic, thermal and antimicrobial studies of neodymium(III) and samarium(III) complexes derived from tetradentate ligands containing N and S donor atoms

    NASA Astrophysics Data System (ADS)

    Ain, Qurratul; Pandey, S. K.; Pandey, O. P.; Sengupta, S. K.

    2015-04-01

    Trivalent lanthanide complexes of the type [Ln(L)Cl(H2O)2] (where Ln = Nd(III) or Sm(III) and LH2 = Schiff bases derived by the condensation of 3-(phenyl/substitutedphenyl)-4-amino-5-mercapto-1,2,4-triazole with diacetyl/benzil) have been synthesized by the reactions of anhydrous lanthanide(III) chloride with Schiff bases in methanol. The structures of the complexes have been proposed on the basis of elemental analysis, electrical conductance, magnetic moment, spectroscopic measurements (IR, 1H, 13C NMR and UV-vis spectra) and X-ray diffraction studies. The spectral data reveal that the Schiff base ligands behave as dibasic tetradentate chelating agents having coordination sites at two thiol sulfur atoms and two azomethine nitrogen atoms. The presence of coordinated water in metal complexes was confirmed by thermal and IR data of the complexes. All the Schiff bases and their metal complexes have also been screened for their antibacterial activity against Bacillus subtilis, Staphylococcus aureus and antifungal activities against Aspergillus niger, Curvularia pallescens and Colletotrichum capsici.

  2. The interaction of a walking droplet and a pillar

    NASA Astrophysics Data System (ADS)

    Bush, John; Harris, Daniel; Brun, Pierre-Thomas

    2015-11-01

    Droplets may bounce on the surface of a vibrating fluid bath, propelled forward by their own pilot-wave field. With a view to better understanding the interaction of such walking droplets with boundaries, we consider their impact on a submerged circular pillar. While simple scattering events are the norm, as the Faraday threshold is approached, the drop departs the pillar along a path corresponding to a logarithmic spiral. An effective wave force resulting from the pillar is inferred from the spiral, and takes the form of the Coriolis force that would arise in a frame of reference rotating with the instantaneous angular momentum of the drop about the pillar. An electromagnetic analog is explored. Thanks to the NSF.

  3. 9. Partial elevation of west side showing pillar, central and ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    9. Partial elevation of west side showing pillar, central and southern sections, from San Antonio Highway Bridge. - Puente Ferroviario San Antonio, Spanning San Antonio Channel at PR-1, San Juan, San Juan Municipio, PR

  4. Preparation of silica or alumina pillared crystalline titanates

    SciTech Connect

    Udomsak, S.; Nge, R.; Dufner, D.C.; Anthony, R.G.; Lott, S.E.

    1994-05-01

    Layered crystalline titanates (CT) [Anthony and Dosch, US Patent 5 177 045 (1993)] are pillared with tetraethyl orthosilicate, 3-aminopropyltrimethoxysilane, and aluminum acetylacetonate to prepare porous and high surface area supports for sulfided NiMo catalyst. Tetra-ethyl orthosilicate or aluminum acetylacetonate intercalated CT are prepared by stepwise intercalation. First, the basal distance is increased by n-alkylammonium ions prior to intercalation with inorganic compounds. However, an aqueous solution of 3-aminopropyltrimethoxysilane could directly pillar CT without first swelling the titanate with n-alkylamine. The catalytic activities for hydrogenation of pyrene of sulfided NiMo supported silica or alumina pillared CT were higher than those of commercial catalysts (Shell324 and Amocat1C). The silicon and aluminum contents of the pillared CT, used as supports, have a considerable effect on the catalytic activities and physical properties of the supports.

  5. 16. LIGHTING AND PILLAR DETAIL VIEW ON HYPERION BOULEVARD VIADUCT ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    16. LIGHTING AND PILLAR DETAIL VIEW ON HYPERION BOULEVARD VIADUCT AT OVERCROSSING OF RIVERSIDE DRIVE. LOOKING NORTH. - Glendale-Hyperion Viaduct, Spanning Golden State Freeway (I-5) & Los Angeles River at Glendale Boulevard, Los Angeles, Los Angeles County, CA

  6. Transparent conductor-Si pillars heterojunction photodetector

    SciTech Connect

    Yun, Ju-Hyung; Kim, Joondong; Park, Yun Chang

    2014-08-14

    We report a high-performing heterojunction photodetector by enhanced surface effects. Periodically, patterned Si substrates were used to enlarge the photo-reactive regions and yield proportionally improved photo-responses. An optically transparent indium-tin-oxide (ITO) was deposited on a Si substrate and spontaneously formed an ITO/Si heterojunction. Due to an electrical conductive ITO film, ITO/Si heterojunction device can be operated at zero-bias, which effectively suppresses the dark current, resulting in better performances than those by a positive or a negative bias operation. This zero-bias operating heterojunction device exhibits a short response time (∼ 22.5 ms) due to the physical reaction to the incident light. We revealed that the location of the space charge region (SCR) is crucial for a specific photon-wavelength response. The SCR space has the highest collection efficiency of the photo-generated carriers. The photo-response can be maximized when we design the photodetector by superposing the SCR space over a corresponding photon-absorption length. The surface enhanced Si pillar devices significantly improved the photo-responses ratios from that of a planar Si device. According to this design scheme, a high photo-response ratio of 5560% was achieved at a wavelength of 600 nm. This surfaced-enhanced heterojunction design scheme would be a promising approach for various photoelectric applications.

  7. A comparative study of the acidity toward the aqueous phase and adsorptive properties of Al{sub 13}-pillared montmorillonite and Al{sub 13}-pillared saponite

    SciTech Connect

    Bergaoui, L.; Mrad, I.; Ghorbel, A.; Lambert, J.F.

    1999-04-15

    The selectivity of an Al{sub 13}-pillared saponite and an Al{sub 13}-pillared montmorillonite for Cd{sup 2+} and Cu{sup 2+} adsorption was studied. The quantity of metal adsorbed on both pillared clays depends on the pH of the solution and the pillars density. Adsorption equilibria are regulated by the protonation equilibria of the amphoteric sites on the pillars. Pillared clays adsorb more cadmium and copper than classic aluminum hydroxides which is simply attributable to a higher density of surface aluminum groups. Significant differences in behavior are observed between pillared montmorillonite and pillared saponite. Pillared montmorillonite appears to be more acidic, which is correlated with a more advanced degree of structural modification of the pillars on calcination. The authors propose a tentative, partial structural model of pillar transformation compatible with these differences. At the same time, both pillared clays have similar affinities for cadmium II at low pH (5--6), but pillared montmorillonite seems to be a more efficient cadmium trap at pH = 8 when its surface groups are negatively ionized. Thus, the nature of the clay layers conditions the structural modifications of the intercalated [Al{sub 13}] polycations, which in turn determine adsorptive behavior.

  8. Infrared spectroscopic study on the thermal decomposition of external and internal gelation products of simulated mixed oxide nuclear fuel.

    PubMed

    Kumar, K Suresh; Bhat, N P

    2004-02-01

    The thermal decomposition of urania-ceria gel corresponding to the composition U(0.7)Ce(0.3)O(2+x) obtained through external and internal gelation routes were studied using infrared spectroscopy (IR). In the case of externally gelated compound, the gel decomposes with the release of H2O and NH3 below 500 degrees C. A part of the NH3 released is entrapped in the solid and above 500 degrees C self reduction occurs in which U(VI) in the gel is reduced to U3O8. The decomposition products were identified to be U3O8 and CeO2. In the case of internally gelated compound, decomposition similar to the one for externally gelated compound occurred below 500 degrees C. Above 500 degrees C the carbon present in the gel reduced U(VI) to UO2 which formed solid solution with CeO2 around 650 degrees C. PMID:14747073

  9. Spectroscopic, optical, thermal, antimicrobial and density functional theory studies of 4-aminopyridinium 4-hydroxy benzoate hydrate crystal

    NASA Astrophysics Data System (ADS)

    Karthiga Devi, P.; Venkatachalam, K.; Poonkothai, M.

    2016-09-01

    The organic crystal 4-aminopyridinium 4-hydroxy benzoate hydrate was grown using slow evaporation method. Various characterization techniques such as single crystal X-ray diffraction, powder X-ray diffraction, FTIR, UV-visible-NIR spectroscopy and thermal analysis (TG-DSC) were employed to assay the structure and properties of the grown crystal. The antimicrobial evaluation of 4-aminopyridinium 4-hydroxy benzoate hydrate crystal was also performed against some bacteria and fungi. The minimum inhibitory concentration (MIC) values of 4-aminopyridinium 4-hydroxy benzoate hydrate were determined for bacterial and fungal strains. The assessment of optimized structure of the molecule and vibrational frequencies were done using DFT/B3LYP method with 6-31 G (d, p) basis set. The stability of the molecule, hyperconjugative interactions, delocalization of charges and intermolecular hydrogen bond were studied by applying natural bond orbital (NBO) analysis. TD-DFT method employing polarizable continuum model (PCM) was used to examine the electronic absorption spectrum. Evaluation of molecular electrostatic potential (MEP), Mulliken population charges and nonlinear optical (NLO) properties were also carried out. In addition, from the optimized geometry, frontier molecular orbitals analysis was executed.

  10. Synthesis, spectroscopic characterization, electrochemical behaviour and thermal decomposition studies of some transition metal complexes with an azo derivative

    NASA Astrophysics Data System (ADS)

    Sujamol, M. S.; Athira, C. J.; Sindhu, Y.; Mohanan, K.

    2010-01-01

    Complexes of manganese(II), cobalt(II), nickel(II), copper(II) and zinc(II) with a novel heterocyclic azo derivative, formed by coupling diazotized 2-amino-3-carbethoxy-4,5-dimethylthiophene with acetylacetone were synthesized and characterized on the basis of elemental analyses, molar conductance, magnetic susceptibility measurements, UV-vis, IR, 1H NMR and EPR spectral data. Spectral studies revealed that the ligand existed in an internally hydrogen bonded azo-enol form rather than the keto-hydrazone form and coordinated to the metal ion in a tridentate fashion. Analytical data revealed that all the complexes exhibited 1:1 metal-ligand ratio. On the basis of electronic spectral data and magnetic susceptibility measurements, suitable geometry was proposed for each complex. The nickel(II) complex has undergone facile transesterification reaction when refluxed in methanol for a long period. The ligand and the copper(II) complex were subjected to X-ray diffraction study. The electrochemical behaviour of copper(II) complex was investigated by cyclic voltammetry. The thermal behaviour of the same complex was also examined by thermogravimetry.

  11. Synthesis, spectroscopic characterization, electrochemical behaviour and thermal decomposition studies of some transition metal complexes with an azo derivative.

    PubMed

    Sujamol, M S; Athira, C J; Sindhu, Y; Mohanan, K

    2010-01-01

    Complexes of manganese(II), cobalt(II), nickel(II), copper(II) and zinc(II) with a novel heterocyclic azo derivative, formed by coupling diazotized 2-amino-3-carbethoxy-4,5-dimethylthiophene with acetylacetone were synthesized and characterized on the basis of elemental analyses, molar conductance, magnetic susceptibility measurements, UV-vis, IR, (1)H NMR and EPR spectral data. Spectral studies revealed that the ligand existed in an internally hydrogen bonded azo-enol form rather than the keto-hydrazone form and coordinated to the metal ion in a tridentate fashion. Analytical data revealed that all the complexes exhibited 1:1 metal-ligand ratio. On the basis of electronic spectral data and magnetic susceptibility measurements, suitable geometry was proposed for each complex. The nickel(II) complex has undergone facile transesterification reaction when refluxed in methanol for a long period. The ligand and the copper(II) complex were subjected to X-ray diffraction study. The electrochemical behaviour of copper(II) complex was investigated by cyclic voltammetry. The thermal behaviour of the same complex was also examined by thermogravimetry. PMID:19910244

  12. Band gap in tubular pillar phononic crystal plate.

    PubMed

    Shu, Fengfeng; Liu, Yongshun; Wu, Junfeng; Wu, Yihui

    2016-09-01

    In this paper, a phononic crystal (PC) plate with tubular pillars is presented and investigated. The band structures and mode displacement profiles are calculated by using finite element method. The result shows that a complete band gap opens when the ratio of the pillar height to the plate thickness is about 1.6. However, for classic cylinder pillar structures, a band gap opens when the ratio is equal or greater than 3. A tubular pillar design with a void room in it enhances acoustic multiple scattering and gives rise to the opening of the band gap. In order to verify it, a PC structure with double tubular pillars different in size (one within the other) is introduced and a more than 2times band gap enlargement is observed. Furthermore, the coupling between the resonant mode and the plate mode around the band gap is characterized, as well as the effect of the geometrical parameters on the band gap. The behavior of such structure could be utilized to design a pillar PC with stronger structural stability and to enlarge band gaps. PMID:27376841

  13. Planning and design for barrier pillar recovery: Three case histories

    SciTech Connect

    Newman, D.A.

    1995-11-01

    Barrier pillars created during mine development provide additional reserves during mine closure and can be the sole access to reserves previously abandoned because of mining height or out of seam dilution limitations. The safe and successful mining of barrier pillars requires a thorough knowledge of the magnitude and distribution of the vertical stress field in addition to the strength and physical properties of the coal, immediate roof, and immediate floor strata. Quantifying the vertical stress field is complicated by the combination of the overburden stress, abutment stresses transferred onto the barrier pillar from adjacent gob areas, and in multiple seam mining, stresses transferred from abandoned subjacent mines. These variables make the extraction and development of barrier pillar reserves a site specific consideration. Three case histories are presented in which barrier pillar development and extraction provides: (1) an access point and the means to ventilate a large area of low seam reserves left by a prior operator after developing only the thicker area of a multiple split reserve, (2) the means to increase total recovery of a deep, thick seam longwall reserve, and (3) opportunities for the development and retreat mining of a two mile long barrier pillar in thick seam reserves.

  14. Parallel-plate submicron gap formed by micromachined low-density pillars for near-field radiative heat transfer

    SciTech Connect

    Ito, Kota; Miura, Atsushi; Iizuka, Hideo; Toshiyoshi, Hiroshi

    2015-02-23

    Near-field radiative heat transfer has been a subject of great interest due to the applicability to thermal management and energy conversion. In this letter, a submicron gap between a pair of diced fused quartz substrates is formed by using micromachined low-density pillars to obtain both the parallelism and small parasitic heat conduction. The gap uniformity is validated by the optical interferometry at four corners of the substrates. The heat flux across the gap is measured in a steady-state and is no greater than twice of theoretically predicted radiative heat flux, which indicates that the parasitic heat conduction is suppressed to the level of the radiative heat transfer or less. The heat conduction through the pillars is modeled, and it is found to be limited by the thermal contact resistance between the pillar top and the opposing substrate surface. The methodology to form and evaluate the gap promotes the near-field radiative heat transfer to various applications such as thermal rectification, thermal modulation, and thermophotovoltaics.

  15. Investigation of the Growth of Intermetallic Compounds Between Cu Pillars and Solder Caps

    NASA Astrophysics Data System (ADS)

    Lin, Jui-Ching; Qin, Yi; Woertink, Julia

    2014-11-01

    In flip chip applications, Cu pillars with solder caps are regarded as next-generation electronic interconnection technology, because of high input/output density. However, because of diffusion and reaction of Sn and Cu during the high-temperature reflow process, intermetallic compounds (IMC) are formed, and grow, at the interface between the cap and the pillar. Understanding the growth behavior of interfacial IMC is critical in the design of solder interconnections, because excessive growth of IMC can reduce the reliability of connections. In this study, the growth of IMC during thermal cycling, an accelerated method of testing the service environment of electronic devices, was studied by use of focused ion beam-scanning electron microscopy. Under alternating high and low-temperature extremes, growth of Cu6Sn5 ( η-phase) and Cu3Sn ( ɛ-phase) IMC was imaged and measured as a function of the number of cycles. The total IMC layer grew significantly thicker but became more uniform during thermal cycling. The Cu3Sn layer was initially thinner than the Cu6Sn5 layer but outgrew the Cu6Sn5 layer after 1000 cycles. It was found that, with limited Cu and Sn diffusion, consumption of Cu6Sn5 for growth of the Cu3Sn layer can result in a thinner Cu6Sn5 layer after thermal cycling.

  16. From Pillar[n]arene Scaffolds for the Preparation of Nanomaterials to Pillar[5]arene-containing Rotaxanes.

    PubMed

    Nierengarten, Iwona; Deschenaux, Robert; Nierengarten, Jean-François

    2016-01-01

    Pillar[n]arenes are a new class of macrocycles that are efficiently prepared from readily available building blocks. In this particular field, our research teams became interested in the use of a pillar[5]arene core as a compact scaffold for the synthesis of nanomaterials with a controlled distribution of functional groups on both rims of the macrocyclic framework. Such compounds have found applications in biology as multivalent ligands for specific lectines or as polycationic compounds for gene delivery. Liquid-crystalline derivatives have been prepared by grafting mesogenic subunits on the pillar[5]arene core. On the other hand, we also became interested in the preparation of pillar[5]arene-containing [2]rotaxanes. In particular, we have shown that pillar[5] arene-based [2]rotaxanes can be obtained from the reaction of amine stoppers with pseudo-rotaxanes resulting from the association of a pillar[5]arene derivative with a diacyl chloride reagent. Finally, amphiphilic [2]rotaxanes have been prepared and incorporated in thin ordered films at the air-water interface. PMID:26931219

  17. Optical emission spectroscopic diagnostics of a non-thermal atmospheric pressure helium-oxygen plasma jet for biomedical applications

    SciTech Connect

    Thiyagarajan, Magesh; Sarani, Abdollah; Nicula, Cosmina

    2013-06-21

    In this work, we have applied optical emission spectroscopy diagnostics to investigate the characteristics of a non-thermal atmospheric pressure helium plasma jet. The discharge characteristics in the active and afterglow region of the plasma jet, that are critical for biomedical applications, have been investigated. The voltage-current characteristics of the plasma discharge were analyzed and the average plasma power was measured to be around 18 W. The effect of addition of small fractions of oxygen at 0.1%-0.5% on the plasma jet characteristics was studied. The addition of oxygen resulted in a decrease in plasma plume length due to the electronegativity property of oxygen. Atomic and molecular lines of selected reactive plasma species that are considered to be useful to induce biochemical reactions such as OH transitions A{sup 2}{Sigma}{sup +}({nu}=0,1){yields}X{sup 2}{Pi}({Delta}{nu}=0) at 308 nm and A{sup 2}{Sigma}{sup +}({nu}=0,1){yields}X{sup 2}{Pi}({Delta}{nu}=1) at 287 nm, O I transitions 3p{sup 5}P{yields}3s{sup 5}S{sup 0} at 777.41 nm, and 3p{sup 3}P{yields}3s{sup 3}S{sup 0} at 844.6 nm, N{sub 2}(C-B) second positive system with electronic transition C{sup 3}{Pi}{sub u}{sup {yields}}B{sup 3}{Pi}{sub g}'' in the range of 300-450 nm and N{sub 2}{sup +}(B-X) first negative system with electronic transition B{sup 2}{Sigma}{sub u}{sup +}{yields}X{sup 2}{Sigma}{sub g}{sup +}({Delta}{nu}=0) at 391.4 nm have been studied. The atomic emission lines of helium were identified, including the He I transitions 3p{sup 3}P{sup 0}{yields}2s{sup 3}S at 388.8 nm, 3p{sup 1}P{sup 0}{yields} 2s{sup 1}S at 501.6 nm, 3d{sup 3}D{yields}2p{sup 3}P{sup 0} at 587.6 nm, 3d{sup 1}D{yields}2p{sup 1}P{sup 0} at 667.8 nm, 3s{sup 3}S{sup 1}{yields}2p{sup 3}P{sup 0} at 706.5 nm, 3s{sup 1}S{sup 0}{yields}2p{sup 1}P{sup 0} at 728.1 nm, and H{sub {alpha}} transition 2p-3d at 656.3 nm. Using a spectral fitting method, the OH radicals at 306-312 nm, the rotational and vibrational temperatures

  18. Nanoscale Structure and Elasticity of Pillared DNA Nanotubes.

    PubMed

    Joshi, Himanshu; Kaushik, Atul; Seeman, Nadrian C; Maiti, Prabal K

    2016-08-23

    We present an atomistic model of pillared DNA nanotubes (DNTs) and their elastic properties which will facilitate further studies of these nanotubes in several important nanotechnological and biological applications. In particular, we introduce a computational design to create an atomistic model of a 6-helix DNT (6HB) along with its two variants, 6HB flanked symmetrically with two double helical DNA pillars (6HB+2) and 6HB flanked symmetrically by three double helical DNA pillars (6HB+3). Analysis of 200 ns all-atom simulation trajectories in the presence of explicit water and ions shows that these structures are stable and well behaved in all three geometries. Hydrogen bonding is well maintained for all variants of 6HB DNTs. From the equilibrium bending angle distribution, we calculate the persistence lengths of these tubes. The measured persistence lengths of these nanotubes are ∼10 μm, which is 2 orders of magnitude larger than that of dsDNA. We also find a gradual increase of persistence length with an increasing number of pillars, in quantitative agreement with previous experimental findings. To have a quantitative understanding of the stretch modulus of these tubes, we carried out nonequilibrium steered molecular dynamics (SMD). The linear part of the force-extension plot gives a stretch modulus in the range 6500 pN for 6HB without pillars, which increases to 11 000 pN for tubes with three pillars. The values of the stretch modulus calculated using contour length distribution obtained from equilibrium MD simulations are similar to those obtained from nonequilibrium SMD simulations. The addition of pillars makes these DNTs very rigid. PMID:27400249

  19. Molecular dynamics study on the wettability of a hydrophobic surface textured with nanoscale pillars.

    PubMed

    Zhang, Zhengqing; Kim, Hyojeong; Ha, Man Yeong; Jang, Joonkyung

    2014-03-28

    Using molecular dynamics simulation, we studied the wetting properties of a surface textured with hydrophobic pillars, several nanometers in size. The drying transition of water confined between square or circular pillars was related to the Wenzel (WZ) to Cassie-Baxter (CB) transition of a water droplet deposited on periodic pillars. The inter-pillar spacing at which the drying occurs was compared to that predicted from the continuum theory. Such a comparison revealed that the line tension plays an important role in the drying behavior of the present nm-sized pillars. The water molecules near the pillar walls were layered and ordered in orientation. Our simulation showed a long-lived CB state which eventually turns into the WZ state. In this transition, water slowly penetrated down into the inter-pillar gap until it reached the half height of the pillar, and then quickly reached the base of the pillar. PMID:24513852

  20. Hybrid molecular simulation of methane storage inside pillared graphene

    NASA Astrophysics Data System (ADS)

    Hassani, Atieh; Hamed Mosavian, Mohammad Taghi; Ahmadpour, Ali; Farhadian, Nafiseh

    2015-06-01

    In this study, a hybrid molecular dynamics—grand canonical Monte Carlo simulation is carried out to investigate the storage capacity of methane in a new nanostructure adsorbent called pillared graphene. This new nanostructure is composed of graphene sheets in parallel with vertical carbon nanotubes (CNTs), which act as their holders. The adsorption ability of this new structure is compared to graphene sheets to evaluate its potential for methane storage. The results show that in a specific adsorbent volume, applying pillared graphene increases the number of adsorbed methane up to 22% in comparison to graphene sheets. Given the application of various isotherm models such as Langmuir, Freundlich, Sips, and Toth and calculation of their parameters, it is predicted that methane adsorption on pillared graphene displays a heterogeneous behavior. Furthermore, the effects of geometry parameters such as CNTs diameter, the number of CNTs, and graphene sheets layer spacing on the methane uptake are investigated. The results show that the pillared graphene containing 1 CNT per 30 nm2 graphene sheet areas provides the best configuration for methane adsorption. This optimum structure is characterized by a small diameter of about 0.938 nm and an optimal layer spacing of about 1.2 nm. Finally, our results show that this kind of pillared structure can be suitable for methane storage.

  1. Hybrid molecular simulation of methane storage inside pillared graphene.

    PubMed

    Hassani, Atieh; Hamed Mosavian, Mohammad Taghi; Ahmadpour, Ali; Farhadian, Nafiseh

    2015-06-21

    In this study, a hybrid molecular dynamics--grand canonical Monte Carlo simulation is carried out to investigate the storage capacity of methane in a new nanostructure adsorbent called pillared graphene. This new nanostructure is composed of graphene sheets in parallel with vertical carbon nanotubes (CNTs), which act as their holders. The adsorption ability of this new structure is compared to graphene sheets to evaluate its potential for methane storage. The results show that in a specific adsorbent volume, applying pillared graphene increases the number of adsorbed methane up to 22% in comparison to graphene sheets. Given the application of various isotherm models such as Langmuir, Freundlich, Sips, and Toth and calculation of their parameters, it is predicted that methane adsorption on pillared graphene displays a heterogeneous behavior. Furthermore, the effects of geometry parameters such as CNTs diameter, the number of CNTs, and graphene sheets layer spacing on the methane uptake are investigated. The results show that the pillared graphene containing 1 CNT per 30 nm(2) graphene sheet areas provides the best configuration for methane adsorption. This optimum structure is characterized by a small diameter of about 0.938 nm and an optimal layer spacing of about 1.2 nm. Finally, our results show that this kind of pillared structure can be suitable for methane storage. PMID:26093570

  2. Synthesis of SnO2 pillared carbon using long chain alkylamine grafted graphene oxide: an efficient anode material for lithium ion batteries

    NASA Astrophysics Data System (ADS)

    Reddy, M. Jeevan Kumar; Ryu, Sung Hun; Shanmugharaj, A. M.

    2015-12-01

    With the objective of developing new advanced composite materials that can be used as anodes for lithium ion batteries (LIBs), herein we describe the synthesis of SnO2 pillared carbon using various alkylamine (hexylamine; dodecylamine and octadecylamine) grafted graphene oxides and butyl trichlorotin precursors followed by its calcination at 500 °C for 2 h. While the grafted alkylamine induces crystalline growth of SnO2 pillars, thermal annealing of alkylamine grafted graphene oxide results in the formation of amorphous carbon coated graphene. Field emission scanning electron microscopy (FE-SEM) results reveal the successful formation of SnO2 pillared carbon on the graphene surface. X-ray diffraction (XRD), transmission electron microscopy (TEM) and Raman spectroscopy characterization corroborates the formation of rutile SnO2 crystals on the graphene surface. A significant rise in the BET surface area is observed for SnO2 pillared carbon, when compared to pristine GO. Electrochemical characterization studies of SnO2 pillared carbon based anode materials showed an enhanced lithium storage capacity and fine cyclic performance in comparison with pristine GO. The initial specific capacities of SnO2 pillared carbon are observed to be 1379 mA h g-1, 1255 mA h g-1 and 1360 mA h g-1 that decrease to 750 mA h g-1, 643 mA h g-1 and 560 mA h g-1 depending upon the chain length of grafted alkylamine on the graphene surface respectively. Electrochemical impedance spectral analysis reveals that the exchange current density of SnO2 pillared carbon based electrodes is higher, corroborating its enhanced electrochemical activity in comparison with GO based electrodes.With the objective of developing new advanced composite materials that can be used as anodes for lithium ion batteries (LIBs), herein we describe the synthesis of SnO2 pillared carbon using various alkylamine (hexylamine; dodecylamine and octadecylamine) grafted graphene oxides and butyl trichlorotin precursors

  3. Synthesis of SnO2 pillared carbon using long chain alkylamine grafted graphene oxide: an efficient anode material for lithium ion batteries.

    PubMed

    Reddy, M Jeevan Kumar; Ryu, Sung Hun; Shanmugharaj, A M

    2016-01-01

    With the objective of developing new advanced composite materials that can be used as anodes for lithium ion batteries (LIBs), herein we describe the synthesis of SnO2 pillared carbon using various alkylamine (hexylamine; dodecylamine and octadecylamine) grafted graphene oxides and butyl trichlorotin precursors followed by its calcination at 500 °C for 2 h. While the grafted alkylamine induces crystalline growth of SnO2 pillars, thermal annealing of alkylamine grafted graphene oxide results in the formation of amorphous carbon coated graphene. Field emission scanning electron microscopy (FE-SEM) results reveal the successful formation of SnO2 pillared carbon on the graphene surface. X-ray diffraction (XRD), transmission electron microscopy (TEM) and Raman spectroscopy characterization corroborates the formation of rutile SnO2 crystals on the graphene surface. A significant rise in the BET surface area is observed for SnO2 pillared carbon, when compared to pristine GO. Electrochemical characterization studies of SnO2 pillared carbon based anode materials showed an enhanced lithium storage capacity and fine cyclic performance in comparison with pristine GO. The initial specific capacities of SnO2 pillared carbon are observed to be 1379 mA h g(-1), 1255 mA h g(-1) and 1360 mA h g(-1) that decrease to 750 mA h g(-1), 643 mA h g(-1) and 560 mA h g(-1) depending upon the chain length of grafted alkylamine on the graphene surface respectively. Electrochemical impedance spectral analysis reveals that the exchange current density of SnO2 pillared carbon based electrodes is higher, corroborating its enhanced electrochemical activity in comparison with GO based electrodes. PMID:26628211

  4. Effects of PCB Pad Metal Finishes on the Cu-Pillar/Sn-Ag Micro Bump Joint Reliability of Chip-on-Board (COB) Assembly

    NASA Astrophysics Data System (ADS)

    Kim, Youngsoon; Lee, Seyong; Shin, Ji-won; Paik, Kyung-Wook

    2016-06-01

    While solder bumps have been used as the bump structure to form the interconnection during the last few decades, the continuing scaling down of devices has led to a change in the bump structure to Cu-pillar/Sn-Ag micro-bumps. Cu-pillar/Sn-Ag micro-bump interconnections differ from conventional solder bump interconnections in terms of their assembly processing and reliability. A thermo-compression bonding method with pre-applied b-stage non-conductive films has been adopted to form solder joints between Cu pillar/Sn-Ag micro bumps and printed circuit board vehicles, using various pad metal finishes. As a result, various interfacial inter-metallic compounds (IMCs) reactions and stress concentrations occur at the Cu pillar/Sn-Ag micro bumps joints. Therefore, it is necessary to investigate the influence of pad metal finishes on the structural reliability of fine pitch Cu pillar/Sn-Ag micro bumps flip chip packaging. In this study, four different pad surface finishes (Thin Ni ENEPIG, OSP, ENEPIG, ENIG) were evaluated in terms of their interconnection reliability by thermal cycle (T/C) test up to 2000 cycles at temperatures ranging from -55°C to 125°C and high-temperature storage test up to 1000 h at 150°C. The contact resistances of the Cu pillar/Sn-Ag micro bump showed significant differences after the T/C reliability test in the following order: thin Ni ENEPIG > OSP > ENEPIG where the thin Ni ENEPIG pad metal finish provided the best Cu pillar/Sn-Ag micro bump interconnection in terms of bump joint reliability. Various IMCs formed between the bump joint areas can account for the main failure mechanism.

  5. Effects of PCB Pad Metal Finishes on the Cu-Pillar/Sn-Ag Micro Bump Joint Reliability of Chip-on-Board (COB) Assembly

    NASA Astrophysics Data System (ADS)

    Kim, Youngsoon; Lee, Seyong; Shin, Ji-won; Paik, Kyung-Wook

    2016-03-01

    While solder bumps have been used as the bump structure to form the interconnection during the last few decades, the continuing scaling down of devices has led to a change in the bump structure to Cu-pillar/Sn-Ag micro-bumps. Cu-pillar/Sn-Ag micro-bump interconnections differ from conventional solder bump interconnections in terms of their assembly processing and reliability. A thermo-compression bonding method with pre-applied b-stage non-conductive films has been adopted to form solder joints between Cu pillar/Sn-Ag micro bumps and printed circuit board vehicles, using various pad metal finishes. As a result, various interfacial inter-metallic compounds (IMCs) reactions and stress concentrations occur at the Cu pillar/Sn-Ag micro bumps joints. Therefore, it is necessary to investigate the influence of pad metal finishes on the structural reliability of fine pitch Cu pillar/Sn-Ag micro bumps flip chip packaging. In this study, four different pad surface finishes (Thin Ni ENEPIG, OSP, ENEPIG, ENIG) were evaluated in terms of their interconnection reliability by thermal cycle (T/C) test up to 2000 cycles at temperatures ranging from -55°C to 125°C and high-temperature storage test up to 1000 h at 150°C. The contact resistances of the Cu pillar/Sn-Ag micro bump showed significant differences after the T/C reliability test in the following order: thin Ni ENEPIG > OSP > ENEPIG where the thin Ni ENEPIG pad metal finish provided the best Cu pillar/Sn-Ag micro bump interconnection in terms of bump joint reliability. Various IMCs formed between the bump joint areas can account for the main failure mechanism.

  6. Dynamics of effusive and diffusive gas separation on pillared graphene.

    PubMed

    Wesołowski, Radosław P; Terzyk, Artur P

    2016-06-22

    Pillared graphene structures, from a practical viewpoint, are very interesting novel carbon materials. Combining the properties of graphene and nanotubes, such as durability, chemical purity and a controlled structure, they were proven to be effective membranes for noble gas separation processes. Here, we examine their possible use for other, more commercially useful gas mixture separation, i.e. air and coal gas. The mechanism of air gas transport through the pillar channels is studied, and the prospective application of 2-D pillared membranes in effusion-like processes provided. The separative abilities of hybrid systems consisting of membranes with different channel diameters in relation to coal gas are proven to be promising. PMID:27297664

  7. Piling Up Pillar[5]arenes To Self-Assemble Nanotubes.

    PubMed

    Nierengarten, Iwona; Guerra, Sebastiano; Ben Aziza, Haifa; Holler, Michel; Abidi, Rym; Barberá, Joaquín; Deschenaux, Robert; Nierengarten, Jean-François

    2016-04-25

    New liquid-crystalline pillar[5]arene derivatives have been prepared by grafting first-generation Percec-type poly(benzylether) dendrons onto the macrocyclic scaffold. The molecules adopt a disc-shaped structure perfectly suited for self-organization into a columnar liquid-crystalline phase. In this way, the pillar[5]arene cores are piled up, thus forming a nanotubular wire encased within a shell of peripheral dendrons. The capability of pillar[5]arenes to form inclusion complexes has been also exploited. Specifically, detailed binding studies have been carried out in solution with 1,6-dicyanohexane as the guest. Inclusion complexes have also been prepared in the solid state. Supramolecular organization into the Colh mesophase has been deduced from X-ray diffraction data and found to be similar to that observed within the crystal lattice of a model inclusion complex prepared from 1,4-dimethoxypillar[5]arene and 1,6-dicyanohexane. PMID:26888329

  8. Fabrication of Pillar Shaped Electrode Arrays for Artificial Retinal Implants

    PubMed Central

    Kim, Eui Tae; Seo, Jong-Mo; Woo, Se Joon; Zhou, Jing Ai; Chung, Hum; Kim, Sung June

    2008-01-01

    Polyimide has been widely applied to neural prosthetic devices, such as the retinal implants, due to its well-known biocompatibility and ability to be micropatterned. However, planar films of polyimide that are typically employed show a limited ability in reducing the distance between electrodes and targeting cell layers, which limits site resolution for effective multi-channel stimulation. In this paper, we report a newly designed device with a pillar structure that more effectively interfaces with the target. Electrode arrays were successfully fabricated and safely implanted inside the rabbit eye in suprachoroidal space. Optical Coherence Tomography (OCT) showed well-preserved pillar structures of the electrode without damage. Bipolar stimulation was applied through paired sites (6:1) and the neural responses were successfully recorded from several regions in the visual cortex. Electrically evoked cortical potential by the pillar electrode array stimulation were compared to visual evoked potential under full-field light stimulation.

  9. Gold-Tipped Elastomeric Pillars for Cellular Mechanotransduction

    PubMed Central

    Ghassemi, S.; Rossier, O.; Sheetz, M. P.; Wind, S. J.; Hone, J.

    2010-01-01

    We describe a technique for the fabrication of arrays of elastomeric pillars whose top surfaces are treated with selective chemical functionalization to promote cellular adhesion in cellular force transduction experiments. The technique involves the creation of a rigid mold consisting of arrays of circular holes into which a thin layer of Au is deposited while the top surface of the mold and the sidewalls of the holes are protected by a sacrificial layer of Cr. When an elastomer is formed in the mold, the Au adheres to the tops of the molded pillars. This can then be selectively functionalized with a protein that induces cell adhesion, while the rest of the surface is treated with a repellent substance. An additional benefit is that the tops of the pillars can be fluorescently labeled for improved accuracy in force transduction measurements. PMID:20526428

  10. Activation-Enabled Syntheses of Functionalized Pillar[5]arene Derivatives.

    PubMed

    Han, Jie; Hou, Xisen; Ke, Chenfeng; Zhang, Huacheng; Strutt, Nathan L; Stern, Charlotte L; Stoddart, J Fraser

    2015-07-01

    A series of regioselective di- and trifunctionalized pillar[5]arene derivatives have been synthesized by a deprotection-followed-by-activation strategy, and their constitutions have been established as a result of having access to their solid-state structures. De-O-methylation occurs in a stepwise manner at lower temperatures under kinetic control, affording the desired oligo-substituted pillar[5]arene derivatives. In addition, the regioisomers of these derivatives can be isolated by installing triflate groups on the free hydroxyl groups. PMID:26083303

  11. Pillared smectite clay coatings for ceramic-matrix composites

    SciTech Connect

    Jagota, S.; Harmer, M.A.; Lemon, M.F.; Jagota, A.; McCarron, E.M. III.

    1995-08-01

    This paper describes a novel route for the low-temperature formation of mullite, from pillared smectite clay precursors, for use as fiber coatings in ceramic-matrix composites. In particular, alumina-pillared bentonite converts in part to mullite at the unusually low temperature of about 800 C. The clay precursors display excellent film-forming capability and have been coated onto silicon carbide fibers. Mechanical tests on composites of the coated fibers and a borosilicate glass demonstrate their success as debond coatings, suggesting that this approach is a viable and simple route to oxide coatings for fibers.

  12. Quantum-dot-induced phase shift in a pillar microcavity

    SciTech Connect

    Young, A. B.; Hu, C. Y.; Rarity, J. G.; Oulton, R.; Thijssen, A. C. T.; Schneider, C.; Reitzenstein, S.; Kamp, M.; Hoefling, S.; Worschech, L.; Forchel, A.

    2011-07-15

    We perform high-resolution reflection spectroscopy of a quantum dot resonantly coupled to a pillar microcavity. We show the change in reflectivity as the quantum dot is tuned through the cavity resonance and measure the quantum-dot-induced phase shift using an ultrastable interferometer. The macroscopic phase shift we measure could be extended to the study of charged quantum dot pillar microcavity systems, where it could be exploited to realize a high-efficiency spin photon interface for hybrid quantum information schemes.

  13. Synthesis and characterization of TiO2 pillared montmorillonites: application for methylene blue degradation.

    PubMed

    Chen, Daimei; Du, Gaoxiang; Zhu, Qian; Zhou, Fengsan

    2013-11-01

    TiO2 pillared clay composites were prepared by modifying of montmorillonite (Mt) with cetyl-trimethyammoniumbromide (CTAB) and then using an acidic solution of hydrolyzed Ti alkoxide to intercalate into the interlayer space of the organic modified Mt. The as-prepared materials were characterized by XRD, FTIR, TEM, SEM TG-DTA, specific surface area and porosity measurements. The composites had a porous delaminated structure with pillared fragments and well dispersed TiO2 nanoparticles. Introduction of CTAB into the synthetic system accelerated the hydrolysis and condensation of the Ti source, which promoted TiO2 formation. In addition, the CTAB also significantly increased the porosity and surface area of the composites. A number of anatase particles, with crystal sizes of 5-10 nm, were homogenously distributed on the surface of the Mt as the result of the templating role of CTAB. The resultant TiO2 pillared Mt exhibited good thermal stability as indicated by its surface area after calcination at 800°C. No phase transformations from anatase to rutile were observed even under calcination at 900°C. The grain size of the anatase in prepared sample increased from 2.67 nm to 13.42 nm as the calcination temperature increased from 300°C to 900°C. The photocatalytic performance of these new porous materials was evaluated by using methylene blue degradation. The composite exhibited better photocatalytic property than P 25. The maximum removal efficiency of this composite was up to 99% within 60 min. PMID:23957927

  14. Eco-Friendly Magnetic Iron Oxide Pillared Montmorillonite for Advanced Catalytic Degradation of Dichlorophenol

    EPA Science Inventory

    Eco-friendly pillared montmorillonites, in which the pillars consist of iron oxide are expected to have interesting and unusual magnetic properties that are applicable for environmental decontamination. Completely “green” and effective composite was synthesized using mild reactio...

  15. Pillars of Progress. Lumina Foundation Focus. Spring 2008

    ERIC Educational Resources Information Center

    Powell, David S., Ed.

    2008-01-01

    Minority-Serving Institutions (MSIs) often go above and beyond the call of duty to encourage engagement and provide support to traditionally underrepresented students. This issue of Lumina Foundation Focus magazine, titled "Pillars of progress," examines MSIs and their efforts to maximize student success. Following the President's Message, In…

  16. Superhydrophobic Analyte Concentration Utilizing Colloid-Pillar Array SERS Substrates

    SciTech Connect

    Wallace, Ryan A.; Charlton, Jennifer J.; Kirchner, Teresa B.; Lavrik, Nickolay V.; Datskos, Panos G.; Sepaniak, Michael J.

    2014-11-04

    In order to detect a few molecules present in a large sample it is important to know the trace components in the medicinal and environmental sample. Surface enhanced Raman spectroscopy (SERS) is a technique that can be utilized to detect molecules at very low absolute numbers. However, detection at trace concentration levels in real samples requires properly designed delivery and detection systems. Moreover, the following work involves superhydrophobic surfaces that includes silicon pillar arrays formed by lithographic and dewetting protocols. In order to generate the necessary plasmonic substrate for SERS detection, simple and flow stable Ag colloid was added to the functionalized pillar array system via soaking. The pillars are used native and with hydrophobic modification. The pillars provide a means to concentrate analyte via superhydrophobic droplet evaporation effects. A 100-fold concentration of analyte was estimated, with a limit of detection of 2.9 10-12 M for mitoxantrone dihydrochloride. Additionally, analytes were delivered to the surface via a multiplex approach in order to demonstrate an ability to control droplet size and placement for scaled-up applications in real world applications. Finally, a concentration process involving transport and sequestration based on surface treatment selective wicking is demonstrated.

  17. Mine flooding and barrier pillar hydrology in the Pittsburgh basin

    SciTech Connect

    Leavitt, B.R.

    1999-07-01

    Pennsylvania began requiring barrier pillars between mines as early as 1930. The Ashley formula, resulting from a early commission on the problem, requires 20 feet of coal plus a thickness of coal equal to four times the seam height plus an additional thickness of coal equal to one tenth of the overburden thickness, or the maximum potential hydraulic head. For a 6-foot thick coal seam under 400 feet of cover, the barrier would be 20+24+40=84 feet. The Ashley formula is intended to protect coal miners from a catastrophic failure of a barrier pillar which has a high head of water impounded behind it. The paper gives several examples of flooded and unflooded mines and the performance of their barrier pillars with respect to acid mine drainage. It is concluded that for all practical purposes, barrier pillars designed with the Ashley formula are able to hydrologically isolate mines from one another. This hydrologic isolation promotes the inundation of closed mines. Inundation effectively stops acid formation, thus, fully inundated mines do not represent a perpetual source of acid mine drainage. Infiltrating ground water improves the mine water chemistry resulting in a net alkaline discharge which has greatly lowered iron concentrations. The best locations for acid mine drainage treatment plants is at the lowest surface elevation above the mine with mine flooded to near that elevation.

  18. Identification of markers closely linked to the peach "pillar" gene

    Technology Transfer Automated Retrieval System (TEKTRAN)

    In peach [Prunus persica (L.) Batsch], trees showing columnar (also termed "pillar" or "broomy") growth habit are of interest of high density production systems. However, in early breeding stages, the selection by this phenotype is very difficult, as the trait is recessively inherited and heterozyg...

  19. Rapid implantation of dissolving microneedles on an electrospun pillar array.

    PubMed

    Yang, Huisuk; Kim, Soyoung; Huh, Inyoung; Kim, Suyong; Lahiji, Shayan F; Kim, Miroo; Jung, Hyungil

    2015-09-01

    Dissolving microneedles (DMNs), designed to release drugs and dissolve after skin insertion, have been spotlighted as a novel transdermal delivery system due to their advantages such as minimal pain and tissue damage, ability to self-administer, and no associated hazardous residues. The drug delivery efficacy of DMNs, however, is limited by incomplete insertion and the extended period required for DMN dissolution. Here, we introduce a novel DMN delivery system, DMN on an electrospun pillar array (DEPA), which can rapidly implant DMNs into skin. DMNs were fabricated on a pillar array covered by a fibrous sheet produced by electrospinning PLGA solution (14%, w/v). DMNs were implanted into the skin by manual application (press and vibration for 10 s) by tearing of the fibers hung on the 300-μm pillars. Separation of DMNs from the fibrous sheet was dependent on both pillar height and the properties of the fibrous sheet. After evaluation of the implantation and dissolution of DMNs with diffusion of red dye by taking cross-sectional images of porcine skin, the hypoglycemic effect of insulin loaded DEPA was examined using a healthy mouse model. This DMN array overcomes critical issues associated with the low penetration efficiency of flat patch-based DMNs, and will allow realization of patient convenience with the desired drug efficacy. PMID:26117659

  20. A Novel Experimental Technique to Simulate Pillar Burst in Laboratory

    NASA Astrophysics Data System (ADS)

    He, M. C.; Zhao, F.; Cai, M.; Du, S.

    2015-09-01

    Pillar burst is one type of rockburst that occurs in underground mines. Simulating the stress change and obtaining insight into the pillar burst phenomenon under laboratory conditions are essential for studying the rock behavior during pillar burst in situ. To study the failure mechanism, a novel experimental technique was proposed and a series of tests were conducted on some granite specimens using a true-triaxial strainburst test system. Acoustic emission (AE) sensors were used to monitor the rock fracturing process. The damage evolution process was investigated using techniques such as macro and micro fracture characteristics observation, AE energy evolution, and b value analysis and fractal dimension analysis of cracks on fragments. The obtained results indicate that stepped loading and unloading simulated the pillar burst phenomenon well. Four deformation stages are divided as initial stress state, unloading step I, unloading step II, and final burst. It is observed that AE energy has a sharp increase at the initial stress state, accumulates slowly at unloading steps I and II, and increases dramatically at peak stress. Meanwhile, the mean b values fluctuate around 3.50 for the first three deformation stages and then decrease to 2.86 at the final stage, indicating the generation of a large amount of macro fractures. Before the test, the fractal dimension values are discrete and mainly vary between 1.10 and 1.25, whereas after failure the values concentrate around 1.25-1.35.

  1. Superhydrophobic Analyte Concentration Utilizing Colloid-Pillar Array SERS Substrates

    DOE PAGESBeta

    Wallace, Ryan A.; Charlton, Jennifer J.; Kirchner, Teresa B.; Lavrik, Nickolay V.; Datskos, Panos G.; Sepaniak, Michael J.

    2014-11-04

    In order to detect a few molecules present in a large sample it is important to know the trace components in the medicinal and environmental sample. Surface enhanced Raman spectroscopy (SERS) is a technique that can be utilized to detect molecules at very low absolute numbers. However, detection at trace concentration levels in real samples requires properly designed delivery and detection systems. Moreover, the following work involves superhydrophobic surfaces that includes silicon pillar arrays formed by lithographic and dewetting protocols. In order to generate the necessary plasmonic substrate for SERS detection, simple and flow stable Ag colloid was added tomore » the functionalized pillar array system via soaking. The pillars are used native and with hydrophobic modification. The pillars provide a means to concentrate analyte via superhydrophobic droplet evaporation effects. A 100-fold concentration of analyte was estimated, with a limit of detection of 2.9 10-12 M for mitoxantrone dihydrochloride. Additionally, analytes were delivered to the surface via a multiplex approach in order to demonstrate an ability to control droplet size and placement for scaled-up applications in real world applications. Finally, a concentration process involving transport and sequestration based on surface treatment selective wicking is demonstrated.« less

  2. Mechanical thinning pillar peach trees - second year results and observations

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Columnar (pillar) form peach trees were mechanically thinned at 50 days after full bloom during the pit hardening stage of development. A spike-drum mechanical shaker, which showed promise for peach fruit thinning, during preliminary tests in 2005 was used to remove the young fruits. The shaker wa...

  3. Extension of silicon emission model to silicon pillar oxidation

    NASA Astrophysics Data System (ADS)

    Kageshima, Hiroyuki; Shiraishi, Kenji; Endoh, Tetsuo

    2016-08-01

    Missing Si in the oxidation of Si pillar structures is investigated by extending the Si emission model to the oxidation of planar structures. The original Si emission model [H. Kageshima et al., Jpn. J. Appl. Phys. 38, L971 (1999)] assumes the emission of excess Si from the interface into the oxide during the oxidation process, the diffusion of the excess Si through the oxide, and the control of the oxidation rate by the concentration of remaining excess Si around the interface. By assuming the sublimation of the excess Si from the oxide surface in addition to the assumptions of the original Si emission model, the origin of the missing Si is consistently explained. It is suggested that the amount of the missing Si is enhanced by the geometrical effect of the pillar structure because the concentration of excess Si is inversely proportional to the radial position. This also suggests that the missing Si is inevitable for the thin pillar structures. Careful approaches to the oxidation process are recommended for pillar structures.

  4. The Sixth Pillar of Reading Instruction: Knowledge Development

    ERIC Educational Resources Information Center

    Cervetti, Gina N.; Hiebert, Elfrieda H.

    2015-01-01

    The National Reading Panel (NRP) identified five pillars, or essential components, of reading instruction that lead to the highest chance of reading success--phonemic awareness, phonics, fluency, vocabulary, and comprehension. A decade after the NRP's report, the majority of US states adopted the Common Core State Standards/English Language Arts…

  5. The calibration of photographic and spectroscopic films. Part 1: Film batch variations of reciprocity failure in IIaO film. Part 2: Thermal and aging effects in relationship to reciprocity failure. P art 3: Shifting of reciprocity failure points as a function of thermal and aging effects

    NASA Technical Reports Server (NTRS)

    Peters, Kevin A.; Atkinson, Pamela F.; Hammond, Ernest C., Jr

    1987-01-01

    Reciprocity failure was examined for IIaO spectroscopic film. Three separate experiments were performed in order to study film batch variations, thermal and aging effects in relationship to reciprocity failure, and shifting of reciprocity failure points as a function of thermal and aging effects. The failure was examined over ranges of time between 5 and 60 seconds. The variation to illuminance was obtained by using thirty neutral density filters. A standard sensitometer device imprinted the wedge pattern on the film as exposure time was subjected to variation. Results indicate that film batch differences, temperature, and aging play an important role in reciprocity failure of IIaO spectroscopic film. A shifting of the failure points was also observed in various batches of film.

  6. The calibration of photographic and spectroscopic films. 1: Film batch variations of reciprocity failure in IIaO film. 2: Thermal and aging effects in relationship to reciprocity failure. 3: Shifting of reciprocity failure points as a function of thermal and aging effects

    NASA Technical Reports Server (NTRS)

    Peters, K. A.; Atkinson, P. F.; Hammond, E. C., Jr.

    1986-01-01

    Reciprocity failure was examined for IIaO spectroscopic film. Three separate experiments were performed in order to study film batch variations, thermal and aging effects in relationship to reciprocity failure, and shifting of reciprocity failure points as a function of thermal and aging effects. The failure was examined over ranges of time between 5 and 60 seconds. The variation to illuminance was obtained by using thirty neutral density filters. A standard sensitometer device imprinted the wedge pattern on the film as exposure time was subjected to variation. The results indicate that film batch differences, temperature, and aging play an important role in reciprocity failure of IIaO spectroscopic film. A shifting of the failure points was also observed in various batches of film.

  7. Comparative case study of yielding and critical coal pillar designs in bump-prone strata

    SciTech Connect

    Koehler, J.R.; DeMarco, M.J.

    1995-11-01

    The failure of yield pillar-based gate road designs to provide adequate ground control performance is primarily related to the use of ``critically`` sized chain pillars. A ``critical`` pillar is one that falls into a range of pillar sizes that are too large to either yield nonviolently or yield before the roof and floor sustain permanent damage, but are to small to support full longwall abutment loads. To directly compare the in-mine performance of critical and yielding pillar designs, the US Bureau of Mines recently completed a field study in a tapering gate road at the Sunnyside No. 1 Mine, Sunnyside, UT. Extreme pillar stresses and associated coal bumps characterize the response to first panel mining of a 16.8-m-wide critical design. Significantly lower pillar stresses, early yielding of the pillar and adjacent panel rib, and an absence of coal bumps suggest that a narrower 12.2-m-wide design more closely approaches proper yield pillar dimensions. Probehole drilling of several 10.6-m-wide pillars revealed low stress levels and substantial pillar and panel rib yielding prior to abutment onset, suggesting a properly functioning yield pillar design.

  8. Intravascular pillars and pruning in the extraembryonic vessels of chick embryos.

    PubMed

    Lee, Grace S; Filipovic, Nenad; Lin, Miao; Gibney, Barry C; Simpson, Dinee C; Konerding, Moritz A; Tsuda, Akira; Mentzer, Steven J

    2011-06-01

    To investigate the local mechanical forces associated with intravascular pillars and vessel pruning, we studied the conducting vessels in the extraembryonic circulation of the chick embryo. During the development days 13-17, intravascular pillars and blood flow parameters were identified using fluorescent vascular tracers and digital time-series video reconstructions. The geometry of selected vessels was confirmed by corrosion casting and scanning electron microscopy. Computational simulations of pruning vessels suggested that serial pillars form along pre-existing velocity streamlines; blood pressure demonstrated no obvious spatial relationship with the intravascular pillars. Modeling a Reynolds number of 0.03 produced 4 pillars at approximately 20-μm intervals matching the observed periodicity. In contrast, a Reynolds number of 0.06 produced only 2 pillars at approximately 63-μm intervals. Our modeling data indicated that the combination of wall shear stress and gradient of shear predicted the location, direction, and periodicity of developing pillars. PMID:21448976

  9. Effects of various longwall chain pillar configurations on gate road stability

    SciTech Connect

    Listak, J.M.; Zelanko, J.C.; Barton, T.M.

    1988-01-01

    The Bureau of Mines conducted a field study to assess the performance of various chain pillar configurations in terms of gate road entry stability. This study is discussed in the book. Vibrating wire stressmeters (VWS's) were installed in four consecutive gate road chain pillars. Field data collected during panel retreat were analyzed to gain a better understanding of the mechanics of vertical load redistribution in gate road chain pillars as it relates to ground control problems. Several different pillar configurations were investigated including abutment-yield and yield-abutment-yield designs. VWS data indicate that average pillar loads were lower and appeared to stabilize when an abutment-yield pillar arrangement was utilized. Data analyses also support the occurrence of severe roof and pillar deterioration that was visually observed in the tailgate entries during panel extraction.

  10. Pave Pillar in-house research final report

    NASA Astrophysics Data System (ADS)

    Blair, Jesse L.; Powers, Philip

    The authors report on the concepts and technologies required to develop, integrate, and test the Pave Pillar architecture in an avionics system. Hardware and software issues relating to multiprocessing, multitasking, and real-time reconfiguration are discussed. The issues involved in developing and integrating the VHSIC avionic modular processors (VAMPs), high-speed data bus networks, and Ada software are examined. An avionic hot bench simulation was integrated to provide a closed-loop real-time test set-up called the integrated testbed (ITB) facility. The configuration and test setup for the common avionics modules were selected to provide a realistic environment and to be as close to the defined Pave Pillar architecture as possible.

  11. Process Development for Stamping Á-Pillar Covers with Aluminum

    SciTech Connect

    Choi, Jung-Pyung; Rohatgi, Aashish; Smith, Mark T.; Lavender, Curt A.

    2015-02-20

    In this work, performed in close collaboration with PACCAR and Magna International, a 6XXX series aluminum alloy was used for the development of A-Pillar cover for the cab of a typical heavy-duty Class-8 truck. The use of Al alloy for the A-pillar cover represents an approximately 40% weight savings over its steel or molded fiberglass composite counterpart. For the selected Al alloy, a small amount of cold work (5% tensile strain), following prior hot-forming, was found to significantly improve the subsequent age-hardening response. The role of solutionizing temperature and rate of cooling on the age-hardening response after paint-bake treatment were investigated. For the temperature range selected in this work, higher solutionizing temperature correlated with greater subsequent age-hardening and vice-versa. However, the age-hardening response was insensitive to the mode of cooling (water quench vs. air cooling). Finally, a two-step forming process was developed where, in the first step, the blank was heated to solutionizing temperature, quenched, and then partially formed at room temperature. For the second step, the pre-form was re-heated and quenched as in the first step, and the forming was completed at room temperature. The resulting A-pillars had sufficient residual ductility to be compatible with hemming and riveting

  12. Allowable pillar to diameter ratio for strategic petroleum reserve caverns.

    SciTech Connect

    Ehgartner, Brian L.; Park, Byoung Yoon

    2011-05-01

    This report compiles 3-D finite element analyses performed to evaluate the stability of Strategic Petroleum Reserve (SPR) caverns over multiple leach cycles. When oil is withdrawn from a cavern in salt using freshwater, the cavern enlarges. As a result, the pillar separating caverns in the SPR fields is reduced over time due to usage of the reserve. The enlarged cavern diameters and smaller pillars reduce underground stability. Advances in geomechanics modeling enable the allowable pillar to diameter ratio (P/D) to be defined. Prior to such modeling capabilities, the allowable P/D was established as 1.78 based on some very limited experience in other cavern fields. While appropriate for 1980, the ratio conservatively limits the allowable number of oil drawdowns and hence limits the overall utility and life of the SPR cavern field. Analyses from all four cavern fields are evaluated along with operating experience gained over the past 30 years to define a new P/D for the reserve. A new ratio of 1.0 is recommended. This ratio is applicable only to existing SPR caverns.

  13. Hydroconversion reactions catalyzed by highly stable pillared clays

    SciTech Connect

    Gomez, S.A.; Mosqueira, L.; Espinosa, J.; Fuentes, G.A.

    1993-12-31

    Al-pillared clays (Al-PILC) and Al-X-PILC (X = Ga, Ni), structurally stable at high temperature - in the case of Ga above 800{degrees}C-have been synthesized by controlling intercalation steps and stabilization procedures. New bidimensional materials with an interlaminar distance about 10-12{angstrom} and with different chemical reactivities in the pillars have thus been produced. The analytical techniques employed to characterize the materials and the processes involved during stabilization include N{sub 2} adsorption, AA, XRD, NH{sub 3}-TPD, TGA-DTA, HR- and MAS-NMR (Al, Si, and Ga) and in-situ IR and DRIFTS. Chemical characterization using high pressure reactions with probe molecules such as diphenylmethane and tert-butylbenzene shows selectivity patterns than can be clearly associated with the microstructure of the PILC used, as well as an effect due to the composition of the pillars. Similar studies with zeolites give patterns that differ from those of PILC, probably because of the change in dimensionality of the internal structure. Poisoning studies with metal porphyrins prove that PLIC have improved resistance compared to standard catalysts. Hydrotreatment of Maya crude results a significant reduction in total sulfur under conditions suitable for commercial operation.

  14. Phosphonium pillar[5]arenes as a new class of efficient biofilm inhibitors: importance of charge cooperativity and the pillar platform.

    PubMed

    Joseph, Roymon; Kaizerman, Dana; Herzog, Ido M; Hadar, Maya; Feldman, Mark; Fridman, Micha; Cohen, Yoram

    2016-08-23

    Biofilm formation, which frequently occurs in microbial infections and often reduces the efficacy of antibiotics, also perturbs many industrial and domestic processes. We found that a new class of water soluble pillar[5]arenes bearing phosphonium moieties (1, 2) and their respective ammonium analogues (3, 4) inhibit biofilm formation with IC50 values in the range of 0.67-1.66 μM. These compounds have no antimicrobial activity, do not damage red blood cell membranes, and do not affect mammalian cell viability in culture. Comparison of the antibiofilm activities of the phosphonium-decorated pillar[5]arene derivatives 1 and 2 with their respective ammonium counterparts 3 and 4 and their monomers 5 and 6, demonstrate that while positive charges, charge cooperativity and the pillararene platform are essential for the observed antibiofilm activity the nature of the charges is not. PMID:27503150

  15. Amine-pillared Nanosheet Adsorbents for CO2 Capture Applications

    NASA Astrophysics Data System (ADS)

    Jiang, Hui

    Amine-functionalized solid adsorbents have gained attention within the last decade for their application in carbon dioxide capture, due to their many advantages such as low energy cost for regeneration, tunable structure, elimination of corrosion problems, and additional advantages. However, one of the challenges facing this technology is to accomplish both high CO 2 capture capacity along with high CO2 diffusion rates concurrently. Current amine-based solid sorbents such as porous materials similar to SBA-15 have large pores diffusion entering molecules; however, the pores become clogged upon amine inclusion. To meet this challenge, our group's solution involves the creation of a new type of material which we are calling-amino-pillared nanosheet (APN) adsorbents which are generated from layered nanosheet precursors. These materials are being proposed because of their unique lamellar structure which exhibits ability to be modified by organic or inorganic pillars through consecutive swelling and pillaring steps to form large mesoporous interlayer spaces. After the expansion of the layer space through swelling and pillaring, the large pore space can be functionalized with amine groups. This selective functionalization is possible by the choice of amine group introduced. Our choice, large amine molecules, do not access the micropore within each layer; however, either physically or chemically immobilized onto the surface of the mesoporous interlayer space between each layer. The final goal of the research is to investigate the ability to prepare APN adsorbents from a model nanoporous layered materials including nanosheets precursor material MCM-22(P) and nanoporous layered silicate material AMH-3. MCM-22(P) contains 2-dimensional porous channels, 6 membered rings (MB) openings perpendicular to the layers and 10 MB channels in the plane of the layers. However, the transport limiting openings (6 MB) to the layers is smaller than CO2 gas molecules. In contrast, AMH-3 has

  16. Stress Changes and Deformation Monitoring of Longwall Coal Pillars Located in Weak Ground

    NASA Astrophysics Data System (ADS)

    Yu, Bin; Zhang, Zhenyu; Kuang, Tiejun; Liu, Jinrong

    2016-08-01

    Coal pillar stability is strongly influenced by the site-specific geological and geotechnical conditions. Many geological structures such as faults, joints, or rock intrusions can be detrimental to mining operations. In order to evaluate the performance of coal pillars under weak roof degraded by igneous rock intrusion, stress and deformation monitoring was conducted in the affected tailgate areas of Nos. 8208 and 8210 longwalls in Tashan coal mine, Shanxi Province, China. The measurements in the 8208 longwall tailgate showed that the mining-induced stresses in 38-m-wide coal chain pillars under the overburden depth of 300-500 m started to increase at about 100 m ahead of the 8208 longwall working face and reached its peak level at approximately 50 m ahead of the longwall face. The peak stress of 9.16 MPa occurred at the depth of 8-9 m into the pillar from the tailgate side wall. In comparison, disturbance of the headgate block pillar area was negligible, indicating the difference of abutment pressure distribution between the tailgate and headgate sites where the adjacent unmined longwall block carried most of the overburden load. However, when the longwall face passed the headgate monitoring site by 360-379 m, the pillar stress increased to a peak value of 21.4 MPa at the pillar depth of 13 m from the gob side mainly due to stress redistribution in the chain pillar. In contrast to the headgate, at the tailgate side, the adjacent goaf was the dominant triggering factor for high stress concentrations in the chain pillar. Convergence measurements in the tailgate during longwall mining further indicated the evolution characteristics of coal pillar deformation, clearly showing that the gateroad deformation is mainly induced by the longwall extraction it serves. When predicting the future pillar loads from the monitored data, two stress peaks appeared across the 38-m-wide tailgate coal pillar, which are separated by the lower stress area within the pillar center. This

  17. IR spectroscopic and thermal desorption studies of the interaction of the SO2 + O2 mixture with the 9% Ni-Cu-Cr/2% Ce/(θ + α)-Al2O3 catalyst

    NASA Astrophysics Data System (ADS)

    Dosumov, K.; Popova, N. M.; Umbetkaliev, A. K.; Brodskii, A. R.; Tungatarova, S. A.; Zheksenbaeva, Z. T.

    2012-10-01

    Data on the formation of surface structures during the adsorption of sulfur dioxide on alumina-supported metal and oxide catalysts in the presence of oxygen were reviewed. The results of our IR spectroscopic and thermal desorption studies of the interaction of the SO2+O2 mixture with the 9% Ni-Cu-Cr/2% Ce/(θ + α)-Al2O3 catalyst are presented. At 673 K chemisorption of SO2 takes place (absorption band 1165 cm-1, T {des/m} = 673 K), and SO2 is oxidized to form sulfate structures (absorption bands 1235, 1140, 1100, 985, and 615 cm-1, T {des/m} = 973 K), which decompose into SO2 and O2 at 973 K and decay when reduced in H2.

  18. Synthesis and characterization of mixed Fe-Cr oxide pillared {alpha}-zirconium phosphate materials

    SciTech Connect

    Perez-Reina, F.J.; Olivera-Pastor, P.; Rodriguez-Castellon, E.; Jimenez-Lopez, A.

    1996-02-15

    Mixed Fe/Cr hydroxyacetate oligomers ranging in composition from 90/10 to 10/90 have been prepared by mixing Fe{sup 3+} and Cr{sup 3+} nitrate solutions and then adding n-propylammonium acetate up to an acetate/Cr{sup 3+} ratio of 2.8 and pH 4. The oligomers were intercalated into colloidal {alpha}-zirconium phosphate or precipitated with excess n-propylamine. The precipitates are all amorphous and show differential thermal behavior in comparison with the intercalates. Upon calcination in air, the precipitates become crystalline, showing the characteristic XRD peaks of mixed Fe/Cr oxides. These mixed oxides present unusually high BET surface areas (up to 276 m {sup 2}{center_dot}g{sup {minus}1}), especially those with low Fe/Cr ratios. The intercalates are poorly crystalline or amorphous at room temperature and upon calcination at 400{degrees}C in air or under N{sub 2}, which indicates that there is no oxide segregation from the interlayers. From these results it is suggested that mixed Fe/Cr oxides are cross-linked to the phosphate layer, forming a pillared structure. Significantly, the mixed oxides segregated from the phosphate surface at 1000{degrees}C present XRD patterns identical to the mixed oxides obtained from the precipitates with the same Fe/Cr ratios. The pillared materials show high BET surface areas, from 200 to 306 m{sup 2}/g, and narrow pore size distributions with pore radius ranging from 8.5 to 13.8 {Angstrom}. XPS analysis reveals a higher affinity of the phosphate surface for Cr{sup 3+} at high Fe/Cr ratios from 70/30 to 90/10. In these samples the partial oxidation of Cr(III) to Cr(VI) was observed in the XPS spectra, in spite of the materials being calcined under N{sub 2}.

  19. Rib pillar extraction - An alternative to longwalling and shortwalling

    SciTech Connect

    Habenicht, H.; Urschitz, E.

    1987-06-01

    Three mining methods for full extraction in flat coal seams - i.e., longwall (LW), shortwall (SW), and rib pillar extraction (RPE) - are compared with each other in view of the introduction of a mechanized, self-advancing roof support. Features are shown according to which RPE appears most attractive under certain conditions. In this presentation, the mining methods are outlined and discussed. The new support (Alpine Breaker Line Support, ABLS) is described, and its employment is explained. A trial operation in RPE using the ABLS has been conducted successfully in a South African coal mine. The results and improvements are stated.

  20. The calibration of photographic and spectroscopic films: Reciprocity failure and thermal responses of IIaO film at liquid nitrogen temperatures

    NASA Technical Reports Server (NTRS)

    Hammond, E. C., Jr.; Peters, K. A.; Gunther, S. O.; Cunningham, L. M.; Wright, D. D.

    1985-01-01

    Reciprocity failure was examined for IIaO spectroscopic film. The results indicate reciprocity failure occurs at three distinct minimum points in time; 15 min, 30 min and 90 min. The results are unique because theory suggests only one minimum reciprocity failure point should occur. When incubating 70mm IIaO film for 15 and 30 min at temperatures of 30, 40, 50, and 60 C and then placing in a liquid nitrogen bath at a temperature of -190 C the film demonstrated an increase of the optical density when developed at a warm-up time of 30 min. Longer warm-up periods of 1, 2 and 3 hrs yield a decrease in optical density of the darker wedge patterns; whereas, shorter warm-up times yield an overall increase in the optical densities.

  1. Syntheses, crystal structures and properties of two unusual pillared-layer 3d-4f Ln-Cu heterometallic coordination polymers

    SciTech Connect

    Fan Leqing; Wu Jihuai; Huang Yunfang

    2011-09-15

    Two unusual pillared-layer 3d-4f Ln-Cu heterometallic coordination polymers, {l_brace}[Ln{sub 2}Cu{sub 5}Br{sub 4}(IN){sub 7}(H{sub 2}O){sub 6}].H{sub 2}O{r_brace}{sub n} (Ln=Eu (1) and Gd (2), HIN=isonicotinic acid), have been synthesized under hydrothermal conditions, and characterized by elemental analysis, IR, thermal analysis and single-crystal X-ray diffraction. The structure determination reveals that 1 and 2 are isostructural and feature a novel three-dimensional pillared-layer hetrometallic structure built upon the linkages of one-dimensional (1D) linear Ln-carboxylate chains, zero-dimensional (0D) Ln-carboxylate Ln{sub 2}(IN){sub 8} dimers, rare 1D zigzag [Cu{sub 5}Br{sub 4}]{sub n} inorganic chains and IN{sup -} pillars. In both 3D structures, there are Ln-carboxylate layers resulted from the connections of 1D Ln-carboxylate chains and 0D Ln{sub 2}(IN){sub 8} dimers through O-H...O hydrogen bondings. The luminescent properties of 1 have been investigated. The magnetic properties of 1 and 2 have also been studied. - Graphical abstract: Two unusual pillared-layer Eu (Gd)-Cu heterometallic coordination polymers have been hydrothermally synthesized. The luminescent properties of Eu-Cu compound and magnetic properties of both compounds are investigated. Highlights: > Two unusual 3D pillared-layer Eu (Gd)-Cu heterometallic coordination polymers have been synthesized. > 1D and 0D Ln-carboxylate motifs construct layers by O-H...O hydrogen bondings. > In both the structures, there are rare 1D zigzag Cu/Br inorganic chains. > Luminescent properties of Eu-Cu compound and magnetic properties of both the compounds are investigated.

  2. Length scale selects directionality of droplets on vibrating pillar ratchet

    SciTech Connect

    Agapov, Rebecca L.; Boreyko, Jonathan B.; Briggs, Dayrl P.; Srijanto, Bernadeta R.; Retterer, Scott T.; Collier, C. Patrick; Lavrik, Nickolay V.

    2014-09-22

    Directional control of droplet motion at room temperature is of interest for applications such as microfluidic devices, self-cleaning coatings, and directional adhesives. Here, arrays of tilted pillars ranging in height from the nanoscale to the microscale are used as structural ratchets to directionally transport water at room temperature. Water droplets deposited on vibrating chips with a nanostructured ratchet move preferentially in the direction of the feature tilt while the opposite directionality is observed in the case of microstructured ratchets. This remarkable switch in directionality is consistent with changes in the contact angle hysteresis. To glean further insights into the length scale dependent asymmetric contact angle hysteresis, the contact lines formed by a nonvolatile room temperature ionic liquid placed onto the tilted pillar arrays were visualized and analyzed in situ in a scanning electron microscope. As a result, the ability to tune droplet directionality by merely changing the length scale of surface features all etched at the same tilt angle would be a versatile tool for manipulating multiphase flows and for selecting droplet directionality in other lap-on-chip applications.

  3. Length scale selects directionality of droplets on vibrating pillar ratchet

    DOE PAGESBeta

    Agapov, Rebecca L.; Boreyko, Jonathan B.; Briggs, Dayrl P.; Srijanto, Bernadeta R.; Retterer, Scott T.; Collier, C. Patrick; Lavrik, Nickolay V.

    2014-09-22

    Directional control of droplet motion at room temperature is of interest for applications such as microfluidic devices, self-cleaning coatings, and directional adhesives. Here, arrays of tilted pillars ranging in height from the nanoscale to the microscale are used as structural ratchets to directionally transport water at room temperature. Water droplets deposited on vibrating chips with a nanostructured ratchet move preferentially in the direction of the feature tilt while the opposite directionality is observed in the case of microstructured ratchets. This remarkable switch in directionality is consistent with changes in the contact angle hysteresis. To glean further insights into the lengthmore » scale dependent asymmetric contact angle hysteresis, the contact lines formed by a nonvolatile room temperature ionic liquid placed onto the tilted pillar arrays were visualized and analyzed in situ in a scanning electron microscope. As a result, the ability to tune droplet directionality by merely changing the length scale of surface features all etched at the same tilt angle would be a versatile tool for manipulating multiphase flows and for selecting droplet directionality in other lap-on-chip applications.« less

  4. Interactions of Monovalent Organic Cations with Pillared Clays.

    PubMed

    Mishael; Rytwo; Nir; Crespin; Annabi-Bergaya; Van Damme H

    1999-01-01

    Interactions between an acid-activated pillared clay and several organic cations including dyes (methylene blue, MB; crystal violet, CV; acriflavin, AF) and benzyl derivatives (benzyltrimethylammonium, BTMA; benzyltriethylammonium, BTEA) were studied by adsorption measurements and X-ray diffraction. When the dyes were adsorbed from low ionic strength solutions, adsorption was irreversible but saturated at levels below the cation exchange capacity (CEC) of the clay (0.6 meq/g). The difference with CEC value was largest for CV. This mode of adsorption was interpreted in terms of interlayer adsorption with steric hindrance in the pillared galleries. On the other hand, when the dyes were adsorbed from high ionic strength solutions, adsorption levels well beyond the CEC of the clay could be reached, in particular for MB and CV. This was interpreted in terms of a second adsorption mode, involving formation of molecular aggregates on the outer surface of the clay, as evidenced by X-ray diffraction. The behavior of the cationic benzyl derivatives was markedly different, with an adsorption level always below the CEC and a decrease of adsorption as the ionic strength was increased, as expected for non-complex-forming cations. Copyright 1999 Academic Press. PMID:9878144

  5. Two new barium sulfonates with pillared layered structures

    NASA Astrophysics Data System (ADS)

    Yang, Jin; Li, Li; Ma, Jian-Fang; Liu, Ying-Ying; Ma, Ji-Cheng

    2006-08-01

    The reactions of BaCl 2·2H 2O with NaHL a and K 3L b (H 2L a=4-hydroxybenzenesulfonic acid, H 3L b=4-hydroxy-5-nitro-1,3-benzenedisulfonic acid) gave two pillared layered coordination polymers: Ba(HL a)(Cl) 1 and KBaL b(H 2O) 32, respectively. The crystal structures were determined by X-ray diffraction method and refined by full-matrix least-squares methods to R=0.0509 and wR=0.1216 using 1455 reflections with I>2 σ( I) for 1; and R=0.0288 and wR=0.0727 using 2661 reflections with I>2 σ( I) for 2. The interesting feature of compound 1 is the coordination actions of chloride anions, which help to form the polymeric layers by bridging barium cations. In compound 2 the Lb3- anion acts as an unusual dodecadente ligand to form a coordination polymer with pillared layered structure.

  6. Two new barium sulfonates with pillared layered structures

    NASA Astrophysics Data System (ADS)

    Yang, Jin; Li, Li; Ma, Jian-Fang; Liu, Ying-Ying; Ma, Ji-Cheng

    2006-05-01

    The reactions of BaCl 2·2H 2O with NaHL a and K 3L b (H 2L a=4-hydroxybenzenesulfonic acid, H 3L b=4-hydroxy-5-nitro-1,3-benzenedisulfonic acid) gave two pillared layered coordination polymers: Ba(HL a)(Cl) 1 and KBaL b(H 2O) 32, respectively. The crystal structures were determined by X-ray diffraction method and refined by full-matrix least-squares methods to R=0.0509 and wR=0.1216 using 1455 reflections with I>2 σ( I) for 1; and R=0.0288 and wR=0.0727 using 2661 reflections with I>2 σ( I) for 2. The interesting feature of compound 1 is the coordination actions of chloride anions, which help to form the polymeric layers by bridging barium cations. In compound 2 the Lb3- anion acts as an unusual dodecadente ligand to form a coordination polymer with pillared layered structure.

  7. Removal of rhodamine B using iron-pillared bentonite.

    PubMed

    Hou, Mei-Fang; Ma, Cai-Xia; Zhang, Wei-De; Tang, Xiao-Yan; Fan, Yan-Ning; Wan, Hong-Fu

    2011-02-28

    The iron-pillared bentonite (Fe-Ben) was prepared by ion-exchange using the natural bentonite (GZ-Ben) from Gaozhou, China, at room temperature without calcination. Both Fe-Ben and GZ-Ben were characterized by X-ray diffraction, N(2) adsorption and Fourier transform infrared spectroscopy. The results show that the d(001) value and surface area of the bentonite material increased after iron pillaring. Fe-Ben adsorbed much more Rhodamine B (RhB) than GZ-Ben, which can be ascribed to the special surface properties and large surface area of Fe-Ben. The optimum pH value for the adsorption of RhB on Fe-Ben is 5.0. The adsorption of RhB onto Fe-Ben can be well described by the pseudo-second-order kinetic model and the intraparticle diffusion kinetic model. The adsorption isotherm of RhB onto Fe-Ben matches well with the Langmuir model. PMID:21168960

  8. Interaction of vanadium (IV) solvates (L) with second-generation fluoroquinolone antibacterial drug ciprofloxacin: spectroscopic, structure, thermal analyses, kinetics and biological evaluation (L=An, DMF, Py and Et3N).

    PubMed

    Zordok, Wael A

    2014-08-14

    The preparation and characterization of the new solid complexes [VO(CIP)2L]SO4⋅nH2O, where L=aniline (An), dimethylformamide (DMF), pyridine (Py) and triethylamine (Et3N) in the reaction of ciprofloxacin (CIP) with VO(SO4)2·2H2O in ethanol. The isolated complexes have been characterized with their melting points, elemental analysis, IR spectroscopy, magnetic properties, conductance measurements, UV-Vis. and (1)H NMR spectroscopic methods and thermal analyses. The results supported the formation of the complexes and indicated that ciprofloxacin reacts as a bidentate ligand bound to the vanadium ion through the pyridone oxygen and one carboxylato oxygen. The activation energies, E(*); entropies, ΔS(*); enthalpies, ΔH(*); Gibbs free energies, ΔG(*), of the thermal decomposition reactions have been derived from thermo gravimetric (TGA) and differential thermo gravimetric (DTG) curves, using Coats-Redfern and Horowitz-Metzeger methods. The lowest energy model structure of each complex has been proposed by using the density functional theory (DFT) at the B3LYP/CEP-31G level of theory. The ligand and their metal complexes were also evaluated for their antibacterial activity against several bacterial species, such as Bacillus Subtilis (B. Subtilis), Staphylococcus aureus (S. aureus), Nesseria Gonorrhoeae (N. Gonorrhoeae), Pseudomonas aeruginosa (P. aeruginosa) and Escherichia coli (E. coli). PMID:24762540

  9. Interaction of vanadium (IV) solvates (L) with second-generation fluoroquinolone antibacterial drug ciprofloxacin: Spectroscopic, structure, thermal analyses, kinetics and biological evaluation (L = An, DMF, Py and Et3N)

    NASA Astrophysics Data System (ADS)

    Zordok, Wael A.

    2014-08-01

    The preparation and characterization of the new solid complexes [VO(CIP)2L]SO4ṡnH2O, where L = aniline (An), dimethylformamide (DMF), pyridine (Py) and triethylamine (Et3N) in the reaction of ciprofloxacin (CIP) with VO(SO4)2·2H2O in ethanol. The isolated complexes have been characterized with their melting points, elemental analysis, IR spectroscopy, magnetic properties, conductance measurements, UV-Vis. and 1H NMR spectroscopic methods and thermal analyses. The results supported the formation of the complexes and indicated that ciprofloxacin reacts as a bidentate ligand bound to the vanadium ion through the pyridone oxygen and one carboxylato oxygen. The activation energies, E*; entropies, ΔS*; enthalpies, ΔH*; Gibbs free energies, ΔG*, of the thermal decomposition reactions have been derived from thermo gravimetric (TGA) and differential thermo gravimetric (DTG) curves, using Coats-Redfern and Horowitz-Metzeger methods. The lowest energy model structure of each complex has been proposed by using the density functional theory (DFT) at the B3LYP/CEP-31G level of theory. The ligand and their metal complexes were also evaluated for their antibacterial activity against several bacterial species, such as Bacillus Subtilis (B. Subtilis), Staphylococcus aureus (S. aureus), Nesseria Gonorrhoeae (N. Gonorrhoeae), Pseudomonas aeruginosa (P. aeruginosa) and Escherichia coli (E. coli).

  10. Highly thermostable anatase titania-pillared clay for the photocatalytic degradation of airborne styrene.

    PubMed

    Lim, Melvin; Zhou, Yan; Wood, Barry; Wang, Lian Zhou; Rudolph, Victor; Lu, Gao Qing

    2009-01-15

    Airborne styrene is a suspected human carcinogen, and traditional ways of mitigation include the use of adsorption technologies (activated carbon or zeolites) or thermal destruction. These methods presenttheir own shortcomings, i.e., adsorbents need to be regenerated or replaced regularly, and relatively large energy inputs are required in thermal treatment. Photocatalysis offers a potentially sustainable and clean means of controlling such fugitive emissions of styrene in air. The present study demonstrates a new type of well-characterized, highly thermostable titania-pillared clay photocatalysts for airborne styrene decomposition in a custom-designed fluidized-bed photoreactor. This photocatalytic system is found to be capable of destroying up to 87% of 300 ppmV airborne styrene in the presence of ultraviolet (UV) irradiation. The effects of relative humidity (RH: 0 or 20%) are also studied, together with the arising physical structures (in terms of porosity and surface characteristics) of the catalysts when subjected to relatively high calcination temperatures of 1000-1200 degrees C. Such a temperature range may be encountered, e.g., in flue gas emissions (1). It is found that relative humidity levels of 20% retard the degradation efficiencies of airborne styrene when using highly porous catalysts. PMID:19238991

  11. Spectroscopic studies of non-thermal plasma jet at atmospheric pressure formed in low-current nonsteady-state plasmatron for biomedical applications

    NASA Astrophysics Data System (ADS)

    Demkin, V. P.; Melnichuk, S. V.; Demkin, O. V.; Kingma, H.; Van de Berg, R.

    2016-04-01

    The optical and electrophysical characteristics of the nonequilibrium low-temperature plasma formed by a low-current nonsteady-state plasmatron are experimentally investigated in the present work. It is demonstrated that experimental data on the optical diagnostics of the plasma jet can provide a basis for the construction of a self-consistent physical and mathematical plasma model and for the creation of plasma sources with controllable electrophysical parameters intended for the generation of the required concentration of active particles. Results of spectroscopic diagnostics of plasma of the low-current nonsteady-state plasmatron confirm that the given source is efficient for the generation of charged particles and short-wavelength radiation—important plasma components for biomedical problems of an increase in the efficiency of treatment of biological tissues by charged particles. Measurement of the spatial distribution of the plasma jet potential by the probe method has demonstrated that a negative space charge is formed in the plasma jet possibly due to the formation of electronegative oxygen ions.

  12. Thermal infrared (2.5-13.5 μm) spectroscopic remote sensing of igneous rock types on particulate planetary surfaces

    USGS Publications Warehouse

    Salisbury, John W.; Walter, Louis S.

    1989-01-01

    Fundamental molecular vibration bands are significantly diminished by scattering. Thus such bands in spectra of fine particulate regoliths (i.e., dominated by <5-μm particles), or regoliths displaying a similar scale of porosity, are difficult to use for mineralogical or rock type identification. Consequently, other spectral features have been sought that may be more useful in spectroscopic remote sensing of composition. We find that mineralogical information is retained in overtones and combination tones of the fundamental molecular vibrations in the 3.0- to 7.0-μm region, but that relatively few minerals have a sufficiently distinctive band structure to be unambiguously identified with currently available techniques. More significantly, identification of general rock type, as defined by the SCFM chemical index (SCFM = SiO2/SiO2 + CaO + FeO + MgO), is possible using spectral features associated with the principal Christiansen frequency and with a region of relative transparency between the Si-O stretching and bending bands. However, environmental factors may affect the appearance and wavelengths of these features. Finally, prominent absorption bands may result from the presence of relatively small amounts of water, hydroxyl or carbonate, because absorption bands exhibited by these materials in the 2.7- to 4.0-μm region, where silicate spectra are otherwise featureless, increase strongly in spectral contrast with decreasing particle size. Such materials are thus detectable in very small amounts in a particulate regolith composed predominantly of silicate minerals.

  13. The Sloan-C Pillars: Towards a Balanced Approach to Measuring Organizational Learning

    ERIC Educational Resources Information Center

    Yeo, Kee Meng; Mayadas, A. Frank

    2010-01-01

    The Sloan Pillars have set the standard for university-wide online learning program assessment for more than a dozen years. In this paper, the authors propose the extension of the Pillars to corporate e-learning, offering an alternative to traditional enterprise learning assessments. Claiming that conventional methods stress individual courses or…

  14. New Soft Rock Pillar Strength Formula Derived Through Parametric FEA Using a Critical State Plasticity Model

    NASA Astrophysics Data System (ADS)

    Rastiello, Giuseppe; Federico, Francesco; Screpanti, Silvio

    2015-09-01

    Many abandoned room and pillar mines have been excavated not far from the surface of large areas of important European cities. In Rome, these excavations took place at shallow depths (3-15 m below the ground surface) in weak pyroclastic soft rocks. Many of these cavities have collapsed; others appear to be in a stable condition, although an appreciable percentage of their structural components (pillars, roofs, etc.) have shown increasing signs of distress from both the morphological and mechanical points of view. In this study, the stress-strain behaviour of soft rock pillars sustaining systems of cavities under vertical loads was numerically simulated, starting from the in situ initial conditions due to excavation of the cavities. The mechanical behaviour of the constituent material of the pillar was modelled according to the Modified Cam-Clay constitutive law (elasto-plastic with strain hardening). The influence of the pillar geometry (cross-section area, shape, and height) and mechanical parameters of the soft rock on the ultimate compressive strength of the pillar as a whole was parametrically investigated first. Based on the numerical results, an original relationship for pillar strength assessment was developed. Finally, the estimated pillar strengths according to the proposed formula and well-known formulations in the literature were compared.

  15. Building Training on the Pillars: Applying Total Quality in the Classroom.

    ERIC Educational Resources Information Center

    Gallagher, Jo D.; And Others

    This paper focuses on the application of total quality management (TQM) in human resources development. It analyzes writings of five leading total quality authors from which four basic principles, or pillars, are derived as the basis for the application of total quality within the instructional setting. The pillars are: (1) customer satisfaction;…

  16. Dimeric and polymeric mercury(II) complexes of 1-methyl-1,2,3,4-tetrazole-5-thiol: Synthesis, crystal structure, spectroscopic characterization, and thermal analyses

    NASA Astrophysics Data System (ADS)

    Taheriha, Mohammad; Ghadermazi, Mohammad; Amani, Vahid

    2016-03-01

    Two-dimensional coordination polymer of [Hg(μ3-mmtz)2]n (1) and centrosymmetric dinuclear complexes of {[H2en][Hg2(mmtz)4(μ-Br)2]} (2) and {[H2en][Hg2(mmtz)4(μ-I)2]} (3) (where Hmmtz is 1-methyl-1,2,3,4-tetrazole-5-thiol and en is ethylene diamine) were synthesized from the reaction of Hmmtz and en with HgCl2, HgBr2 and HgI2, respectively, in CH3OH. Complex 1 was also synthesized from the reaction of Hmmtz and en with HgX2 (X = OAc and SCN) in CH3OH. These three complexes were thoroughly characterized by elemental analysis (CHN), thermal gravimetric analysis (TGA), differential thermal analyses (DTA), infrared, UV-vis, 1H NMR, and luminescence spectroscopy, and their structures were determined by single-crystal X-ray diffraction.

  17. Characterization of the physico-chemical properties of polymeric materials for aerospace flight. [differential thermal and atomic absorption spectroscopic analysis of nickel cadmium batteries

    NASA Technical Reports Server (NTRS)

    Rock, M.

    1981-01-01

    Electrodes and electrolytes of nickel cadmium sealed batteries were analyzed. Different thermal analysis of negative and positive battery electrodes was conducted and the temperature ranges of occurrence of endotherms indicating decomposition of cadmium hydroxide and nickel hydroxide are identified. Atomic absorption spectroscopy was used to analyze electrodes and electrolytes for traces of nickel, cadmium, cobalt, and potassium. Calibration curves and data are given for each sample analyzed. Instrumentation and analytical procedures used for each method are described.

  18. Synthesis, crystal structure, and spectroscopic and thermal properties of the polymeric compound catena-poly[[bis(2,4-dichlorobenzoato)zinc(II)]-μ-isonicotinamide].

    PubMed

    Homzová, Katarína; Györyová, Katarína; Koman, Marián; Melník, Milan; Juhászová, Žofia

    2015-09-01

    Zinc(II) carboxylates with O-, S- and N-donor ligands are interesting for their structural features, as well as for their antibacterial and antifungal activities. The one-dimensional zinc(II) coordination complex catena-poly[[bis(2,4-dichlorobenzoato-κO)zinc(II)]-μ-isonicotinamide-κ(2)N(1):O], [Zn(C7H3Cl2O2)2(C6H6N2O)]n, has been prepared and characterized by IR spectroscopy, single-crystal X-ray analysis and thermal analysis. The tetrahedral ZnO3N coordination about the Zn(II) cation is built up by the N atom of the pyridine ring, an O atom of the carbonyl group of the isonicotinamide ligand and two O atoms of two dichlorobenzoate ligands. Isonicotinamide serves as a bridge between tetrahedra, with a Zn···Zn distance of 8.8161 (7) Å. Additionally, π-π interactions between the planar benzene rings contribute to the stabilization of the extended structure. The structure is also stabilized by intermolecular hydrogen bonds between the amino and carboxylate groups of the ligands, forming a two-dimensional network. During thermal decomposition of the complex, isonicotinamide, dichlorobenzene and carbon dioxide were evolved. The final solid product of the thermal decomposition heated up to 1173 K was metallic zinc. PMID:26322615

  19. Stress Distribution on Blasting Gallery Barrier Pillar due to Goaf Formation During Extraction

    NASA Astrophysics Data System (ADS)

    Kumar Reddy, Sandi; Sastry, Vedala Rama

    2015-09-01

    Semi-mechanised blasting gallery mining is a sustainable option to achieve higher production and productivity from underground thick coal seams. Judicious design of underground blasting gallery panel requires understanding of stress distribution on barrier pillars during different stages of extraction. This paper presents a study of stress distribution in and around barrier pillar for the different stages of extraction in the blasting gallery panel. Finite difference analysis taken up for final excavation (depillaring) in the panel with different stages of extraction. Analysis revealed that the stress transferred on barrier pillar increased as progress of excavation increased. Maximum stress was observed at a distance of 10 and 12 m from the pillar edge for virgin and goaved out panel sideby respectively, which gradually decreased towards centre of the pillar.

  20. Spectroscopic and thermal investigations on the charge transfer interaction between risperidone as a schizophrenia drug with some traditional π-acceptors: Part 2

    NASA Astrophysics Data System (ADS)

    El-Habeeb, Abeer A.; Al-Saif, Foziah A.; Refat, Moamen S.

    2013-03-01

    The focus of present investigation was to assess the utility of non-expensive techniques in the evaluation of risperidone (Ris) in solid and solution states with different traditional π-acceptors and subsequent incorporation of the analytical determination into pharmaceutical formulation for a faster release of risperidone. Charge-transfer complexes (CTC) of risperidone with picric acid (PA), 2,3-dichloro-5,6-dicyano-p-benzoquinon (DDQ), tetracyanoquinodimethane (TCNQ), tetracyano ethylene (TCNE), tetrabromo-p-quinon (BL) and tetrachloro-p-quinon (CL) have been studied spectrophotometrically in absolute methanol at room temperature. The stoichiometries of the complexes were found to be 1:1 ratio by the photometric molar ratio between risperidone and the π-acceptors. The equilibrium constants, molar extinction coefficient (ɛCT) and spectroscopic-physical parameters (standard free energy (ΔGo), oscillator strength (f), transition dipole moment (μ), resonance energy (RN) and ionization potential (ID)) of the complexes were determined upon the modified Benesi-Hildebrand equation. Risperidone in pure form was applied in this study. The results indicate that the formation constants for the complexes depend on the nature of electron acceptors and donor, and also the spectral studies of the complexes were determined by (infrared, Raman, and 1H NMR) spectra and X-ray powder diffraction (XRD). The most stable mono-protonated form of Ris is characterized by the formation of +Nsbnd H (pyrimidine ring) intramolecular hydrogen bonded. In the high-wavenumber spectral region ˜3400 cm-1, the bands of the +Nsbnd H stretching vibrations and of the pyrimidine nitrogen atom could be potentially useful to discriminate the investigated forms of Ris. The infrared spectra of both Ris complexes are confirming the participation of +Nsbnd H pyrimidine ring in the donor-acceptor interaction.

  1. Design of coal mine roof support and yielding pillars for longwall mining in the Appalachian coalfield

    SciTech Connect

    Newman, D.A.

    1985-01-01

    In this thesis, the existing Geomechanics Classification (Bieniawski, 1979) was modified for use in underground coal mines through the introduction of adjustment modifiers for strata weathering, horizontal stress, and roof support. Sixty-two roof case histories were collected from two mines exploiting the Pittsburgh and Lower Kittanning coal seams. Geologic and material property variables were examined with respect to supported stand-up time, while survival and regression analyses were used in deriving the adjustment multipliers. Guidelines for roofspan selection and roof support design were an integral facet of the modified classification scheme. Tentative design guidelines for chain pillars are provided on the basis of a field investigation and numerical modeling of longwall chain pillar behavior. A longwall chain pillar was instrumented with vibrating wire stressmeters to quantify the change in stress distribution as longwall mining proceeded out by the pillar. A sonic probe was used to conduct a velocity profile across the pillar before and after mining to delineate the failed and stable regions of the pillar. Velocity profiles across the pillar were supplemented by an examination of changes in the dynamic modulus and the shear wave frequency. The main contributions of the research lies in: (i) modifications introduced to the Geomechanics Classification (RMR System), (ii) the correlation between changes in pillar stress and the extent of the yield zone surrounding a longwall chain pillar, and (iii) the proposal of design procedures involving coal mine roof support and chain pillars. Numerical examples obtained from mine case histories are provided to illustrate the use of the design procedures.

  2. Nanophononic Metamaterial: Thermal Conductivity Reduction by Local Resonance

    NASA Astrophysics Data System (ADS)

    Davis, Bruce L.; Hussein, Mahmoud I.

    2014-02-01

    We present the concept of a locally resonant nanophononic metamaterial for thermoelectric energy conversion. Our configuration, which is based on a silicon thin film with a periodic array of pillars erected on one or two of the free surfaces, qualitatively alters the base thin-film phonon spectrum due to a hybridization mechanism between the pillar local resonances and the underlying atomic lattice dispersion. Using an experimentally fitted lattice-dynamics-based model, we conservatively predict the metamaterial thermal conductivity to be as low as 50% of the corresponding uniform thin-film value despite the fact that the pillars add more phonon modes to the spectrum.

  3. Assessment of historical masonry pillars reinforced by CFRP strips

    NASA Astrophysics Data System (ADS)

    Fedele, Roberto; Rosati, Giampaolo; Biolzi, Luigi; Cattaneo, Sara

    2014-10-01

    In this methodological study, the ultimate response of masonry pillars strengthened by externally bonded Carbon Fiber Reinforced Polymer (CFRP) was investigated. Historical bricks were derived from a XVII century rural building, whilst a high strength mortar was utilized for the joints. The conventional experimental information, concerning the overall reaction force and relative displacements provided by "point" sensors (LVDTs and clip gauge), were herein enriched with no-contact, full-field kinematic measurements provided by 2D Digital Image Correlation (2D DIC). Experimental information were critically compared with prediction provided by an advanced three-dimensional models, based on nonlinear finite elements under the simplifying assumption of perfect adhesion between the reinforcement and the support.

  4. Evaporation-driven clustering of microscale pillars and lamellae

    NASA Astrophysics Data System (ADS)

    Kim, Tae-Hong; Kim, Jungchul; Kim, Ho-Young

    2016-02-01

    As a liquid film covering an array of micro- or nanoscale pillars or lamellae evaporates, its meniscus pulls the elastic patterns together because of capillary effects, leading to clustering of the slender microstructures. While this elastocapillary coalescence may imply various useful applications, it is detrimental to a semiconductor manufacturing process called the spin drying, where a liquid film rinses patterned wafers until drying. To understand the transient mechanism underlying such self-organization during and after liquid evaporation, we visualize the clustering dynamics of polymer micropatterns. Our visualization experiments reveal that the patterns clumped during liquid evaporation can be re-separated when completely dried in some cases. This restoration behavior is explained by considering adhesion energy of the patterns as well as capillary forces, which leads to a regime map to predict whether permanent stiction would occur. This work does not only extend our understanding of micropattern stiction, but also suggests a novel path to control and prevent pattern clustering.

  5. Pillared Interlayered Clays as Adsorbents of Gases and Vapors

    NASA Astrophysics Data System (ADS)

    Pires, J.; Pinto, M. L.

    This chapter reviews recent works where porous materials prepared from clays, particularly pillared interlayered clays (PILCs), were studied as gas phase adsorbents. It also includes the cases which used the adsorption of gases and vapors for the nanotextural characterization of the materials, other than the usual low temperature nitrogen adsorption. This is, for instance, the case of the adsorption of molecules of volatile organic compounds (VOCs), with various dimensions and shapes, which can be used as probe molecules for the characterization of the porosity or concerning the topic of the VOCs abatement. A similar situation occurs with water adsorption, whose results can be informative not only on the desiccant properties of the materials but also on their surface chemistry. A more recent line of studies of adsorption by materials prepared from clays, namely, the hydrocarbon purification from natural gas or biogas, was also addressed.

  6. Subsidence vulnerability in shallow room-and-pillar mines

    SciTech Connect

    Missavage, R.

    1985-07-01

    Concern over mining-related subsidence is inhibiting the development of surface land uses in previously mined areas and is constraining the recovery of coal resources in areas with established land uses that might be impacted by subsequent subsidence. The determination of subsidence vulnerability of mined-out areas (especially abandoned mine areas) can be a useful tool in the design and location of surface structures. A model has been developed for assessing subsidence vulnerability in shallow room-and-pillar mines based on the flexural rigidity and strength characteristics of the overlying strata. The model does not predict the subsidence profile or when the subsidence will occur. It only predicts those areas that are likely to subside. This paper briefly describes the model and its testing.

  7. The Surface Photovoltage Mechanism of a Silicon Nanoporous Pillar Array

    NASA Astrophysics Data System (ADS)

    Hu, Zhen-Gang; Tian, Yong-Tao; Li, Xin-Jian

    2013-08-01

    The surface photovoltage (SPV) mechanism of a silicon nanoporous pillar array (Si-NPA) is investigated by using SPV spectroscopy in different external electric fields. Through comparisons with the SPV spectrum of single crystal silicon (sc-Si), the silicon nano-crystallite (nc-Si)/SiOx nanostructure of Si-NPA is proved to be capable of producing obvious SPV in the wavelength range 300-580 nm. The SPV for the sc-Si layer and the nc-Si/SiOx nanostructure has shown certain contrary characters in different external electric fields. Through analysis, the localized states in the amorphous SiOx matrix are believed to dominate the SPV for the nc-Si/SiOx nanostructure.

  8. Spectroscopic, thermal and voltammetric studies of crystalline complex trans- N, N'-bis(salicylidene)-1',2'-cyclohexanediamine with Cu(II)

    NASA Astrophysics Data System (ADS)

    Aslantas, Mehmet; Tümer, Mehmet; Şahin, Ertan

    2008-11-01

    The dimeric complex, [C 20H 20CuN 2O 2] 2, has been prepared and characterized by thermal analysis, IR spectroscopy and single-crystal X-ray diffraction techniques. The Cu atom in the binuclear complex exists in a distorted square-pyramidal configuration, defined by three O atoms and two N atoms. The crystal structure is stabilized by intermolecular C-H⋯O hydrogen bonding interaction. The electrochemical property of the complex was investigated in CH 2Cl 2 by cyclic voltammetry at 100 mV s -1 scan rate.

  9. Cultural Values and Social Differentiation: The Catholic Pillar and Its Education System in Belgium and The Netherlands.

    ERIC Educational Resources Information Center

    Vanderstraeten, Raf

    2002-01-01

    Discusses research on Catholic pillarization. Argues that some European countries are internally divided into blocks of different religions and political persuasions. Outlines the success of the pillars in the areas of education and healthcare. Stresses that other social sectors which function impersonally are not influenced by the pillars. (CAJ)

  10. Supercritical hydrothermal synthesis of Cu{sub 2}O(SeO{sub 3}): Structural characterization, thermal, spectroscopic and magnetic studies

    SciTech Connect

    Larranaga, Aitor

    2009-01-08

    Cu{sub 2}O(SeO{sub 3}) has been synthesized in supercritical hydrothermal conditions, using an externally heated steel reactor with coupled hydraulic pump for the application of high pressure. The compound crystallizes in the P2{sub 1}3 cubic space group. The unit cell parameter is a = 9.930(1) A with Z = 12. The crystal structure has been refined by the Rietveld method. The limit of thermal stability is, approximately, 490 deg. C. Above this temperature the compound decomposes to SeO{sub 2}(g) and CuO(s). The IR spectrum shows the characteristic bands of the (SeO{sub 3}){sup 2-} oxoanion. In the diffuse reflectance spectrum two intense absorptions characteristic of the Cu(II) cations in five-coordination are observed. The ESR spectra are isotropic from room temperature to 5 K, with g = 2.11(2). The thermal evolution of the intensity and line width of the signals suggest a ferromagnetic transition in the 50-45 K range. Magnetic measurements, at low temperatures, confirm the existence of a ferromagnetic transition with a critical temperature of 55 K.