Thermoelectric properties of Tl and I dual-doped Bi2Te3-based alloys

NASA Astrophysics Data System (ADS)

Wu, Fang; He, Qinglin; Tang, Mingsheng; Song, Hongzhang

2018-04-01

TlxBi2‑xTe3‑xIx (x = 0, 0.05, 0.1 and 0.2) flower-like nanopowders were prepared successfully by the hydrothermal method. Then, the synthesized nanoparticles were pressed into bulks by hot-pressing. The thermoelectric (TE) properties of the TlxBi2‑xTe3‑xIx bulk samples were investigated and discussed. The results showed that the influences of Tl doping on the electrical resistivity and Seebeck coefficients of the Bi2Te3 is over that of I doping. Thus, the power factors of the dual-doped bulks are all less than that of the Bi2Te3 bulk. The thermal conductivities of the TlxBi2‑xTe3‑xIx bulk samples also remain at lower values. As a result, the ZT value of the optimized doped bulk Tl0.1Bi1.9Te2.9I0.1 attains a value of 1.1 at 398 K.

The low temperature synthesis, characterization and properties of ferroelectrics

NASA Astrophysics Data System (ADS)

Xu, Jie

2000-10-01

PZT 50:50 xerogels prepared by two different sol-gel routes crystallized in a similar fashion to give a mixture of tetragonal and rhombohedral at high temperature (1000°C). Both the diffraction and EXAFS data suggest that the compositional inhomogeneity of the samples prepared by the two routes is similar. The crystallization of CZT gels is complicated. Crystalline CaCO 3 was always detected in the dry gels regardless of the sample composition and preparation methods. At intermediate temperatures a fluorite related phase was always formed and it transformed to perovskite at higher temperatures. The EXAFS data suggest that perovskite CZT samples prepared using alkoxide sol-gel chemistry may not be random solid solutions. All the solution processed ZrTiO4 materials crystallized in the range 600--700°C. The KTN samples prepared using a conventional alkoxide sol-gel route crystallized completely to perovskite at lower temperatures than those prepared using prehydrolyzed precursors. The EXAFS data for the KTN samples prepared using a conventional alkoxide sol-gel route are consistent with a random distribution of tantalum and niobium in the solid solution. However, materials prepared using the inhomogeneous sol-gel route and by the direct reaction of mixed oxides were shown to be compositionally inhomogeneous. The heterogeneity could not be removed by regrinding and heating the mixed oxide samples several times. K2Ta4-xNbxO11 (x = 0, 2, 4) samples were prepared using alkoxide sol-gel chemistry and their crystallization was examined by powder X-ray diffraction. A Rietveld structure analysis of the pyrochlore formed from a gel with bulk composition K2Ta 2Nb2O11 indicated that it was rich in potassium relative to the bulk sample. On heating to high temperatures tetragonal tungsten bronzes were formed. A Rietveld analysis was also performed for K2Ta 2Nb2O11 with tetragonal tungsten bronze structure. The defect pyrochlores "AgTaO3" and GaTaO 3 were synthesized by ion-exchange using pyrochlore KTaO3 as a starting material. The structures of the pyrochlores were examined using the Rietveld method. The pyrochlore-to-perovskite transformations were also explored.

Analysis of laboratory compaction methods of roller compacted concrete

NASA Astrophysics Data System (ADS)

Trtík, Tomáš; Chylík, Roman; Bílý, Petr; Fládr, Josef

2017-09-01

Roller-Compacted Concrete (RCC) is an ordinary concrete poured and compacted with machines typically used for laying of asphalt road layers. One of the problems connected with this technology is preparation of representative samples in the laboratory. The aim of this work was to analyse two methods of preparation of RCC laboratory samples with bulk density as the comparative parameter. The first method used dynamic compaction by pneumatic hammer. The second method of compaction had a static character. The specimens were loaded by precisely defined force in laboratory loading machine to create the same conditions as during static rolling (in the Czech Republic, only static rolling is commonly used). Bulk densities obtained by the two compaction methods were compared with core drills extracted from real RCC structure. The results have shown that the samples produced by pneumatic hammer tend to overestimate the bulk density of the material. For both compaction methods, immediate bearing index test was performed to verify the quality of compaction. A fundamental difference between static and dynamic compaction was identified. In static compaction, initial resistance to penetration of the mandrel was higher, after exceeding certain limit the resistance was constant. This means that the samples were well compacted just on the surface. Specimens made by pneumatic hammer actively resisted throughout the test, the whole volume was uniformly compacted.

Synthesis and characterization of Mn-Bi alloy

NASA Astrophysics Data System (ADS)

Mishra, Ashutosh; Patil, Harsha; Jain, G.; Mishra, N.

2012-06-01

High purity MnBi low temperature phase has been prepared and analyzed using X-ray diffraction, Lorentz-Polarization Factor and Fourier transforms infrared measurement. After synthesis of samples structural characterization has done on samples by X-ray diffraction, which shows that after making the bulk sample is in no single phase MnBi has been prepared by sintering Mn and Bi powders. By Lorentz-Polarization Factor is affecting the relative intensity of diffraction lines on a powder form. And by FTIR which shows absorption peaks of MnBi alloys.

Effect of layer thickness on the elution of bulk-fill composite components.

PubMed

Rothmund, Lena; Reichl, Franz-Xaver; Hickel, Reinhard; Styllou, Panorea; Styllou, Marianthi; Kehe, Kai; Yang, Yang; Högg, Christof

2017-01-01

An increment layering technique in a thickness of 2mm or less has been the standard to sufficiently convert (co)monomers. Bulk fill resin composites were developed to accelerate the restoration process by enabling up to 4mm thick increments to be cured in a single step. The aim of the present study is to investigate the effect of layer thickness on the elution of components from bulk fill composites. The composites ELS Bulk fill, SDR Bulk fill and Venus Bulkfill were polymerized according to the instruction of the manufacturers. For each composite three groups with four samples each (n=4) were prepared: (1) samples with a layer thickness of 2mm; (2) samples with a layer thickness of 4mm and (3) samples with a layer thickness of 6mm. The samples were eluted in methanol and water for 24h and 7 d. The eluates were analyzed by gas chromatography/mass spectrometry (GC/MS). A total of 11 different elutable substances have been identified from the investigated composites. Following methacrylates showed an increase of elution at a higher layer thickness: TEGDMA (SDR Bulk fill, Venus Bulk fill), EGDMA (Venus Bulk fill). There was no significant difference in the elution of HEMA regarding the layer thickness. The highest concentration of TEGDMA was 146μg/mL for SDR Bulk fill at a layer thickness of 6mm after 7 d in water. The highest HEMA concentration measured at 108μg/mL was detected in the methanol eluate of Venus Bulk fill after 7 d with a layer thickness of 6mm. A layer thickness of 4mm or more can lead to an increased elution of some bulk fill components, compared to the elution at a layer thickness of 2mm. Copyright © 2016 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Preparation and Thermoelectric Properties of Cu2Se Hot-Pressed from Hydrothermal Synthesis Nanopowders

NASA Astrophysics Data System (ADS)

Gao, F.; Leng, S. L.; Zhu, Z.; Li, X. J.; Hu, X.; Song, H. Z.

2018-04-01

The nanopowders of Cu2Se were synthesized by the hydrothermal method, and then were hot-pressed into bulk pellets. The effects of different preparation conditions on the structure and thermoelectric properties of Cu2Se nanocrystalline bulk alloys were investigated. The resistivity and Seebeck coefficients increase with the increment of hot-pressing temperatures, while they decrease with the increment of hot-pressing time, except for the Seebeck coefficients of the sample hot-pressed for 30 min. Based on the power factors and dimensionless thermoelectric figure-of-merit ( ZT) values, the optimum hot-pressing parameters are 700°C and 30 min.

Influence of Sm2O3 microalloying and Yb contamination on Y211 particles coarsening and superconducting properties of IG YBCO bulk superconductors

NASA Astrophysics Data System (ADS)

Vojtkova, L.; Diko, P.; Kovac, J.; Vojtko, M.

2018-06-01

Single grain YBa2Cu3O7‑x (YBCO or Y123) bulk superconductors were produced by an infiltration growth process. The solid phase precursor was prepared by solid state synthesis from Y2O3 + BaCuO2 powders. The influence of the addition of Sm2O3 and YB contamination from the substrate on the microstructure and superconducting properties was analyzed. The dependences of Yb concentration on the distance from the bottom of the samples measured by energy dispersive spectroscopy microanalysis used in conjunction with scanning electron microscopy confirmed the contamination of the samples during the melting stage of the sample preparation. It is shown that the addition of Sm in low concentration and its combination with Yb from the substrate modify the coarsening of the Y211 particles as well as lead to the appearance of a secondary peak effect in the field dependences of the critical current density.

Positron Lifetime Study on the As-Prepared Cd-Doped Pb-1212 Superconductive Oxides

NASA Astrophysics Data System (ADS)

Zhou, X. Y.; Zhou, X. Y.; Zhao, W. C.; Jin, H.; Cao, L. Z.; Zhai, L. H.; Han, R. D.

1997-12-01

The positron lifetime as a function of the Cd content x was measured for the as-prepared samples of (Pb1 - xCdx)Sr2(Y0.5Ca0.5)Cu2Oy. A constant long-lived lifetime was observed for all samples. The intensity of the long-lived lifetimes has an obvious decrease starting at x = 0.3 and indicated the existence of an impurity phase in the sample with x = 0.3. The monotonous decrease of the bulk lifetime for the single-phase samples implies that Cd mainly substitutes for Pb. The changes of the microstructure with Cd content were discussed.

An improved FIB sample preparation technique for site-specific plan-view specimens: A new cutting geometry.

PubMed

Li, Chen; Habler, Gerlinde; Baldwin, Lisa C; Abart, Rainer

2018-01-01

Focused ion beam (FIB) sample preparation technique in plan-view geometry allows direct correlations of the atomic structure study via transmission electron microscopy with micrometer-scale property measurements. However, one main technical difficulty is that a large amount of material must be removed underneath the specimen. Furthermore, directly monitoring the milling process is difficult unless very large material volumes surrounding the TEM specimen site are removed. In this paper, a new cutting geometry is introduced for FIB lift-out sample preparation with plan-view geometry. Firstly, an "isolated" cuboid shaped specimen is cut out, leaving a "bridge" connecting it with the bulk material. Subsequently the two long sides of the "isolated" cuboid are wedged, forming a triangular prism shape. A micromanipulator needle is used for in-situ transfer of the specimen to a FIB TEM grid, which has been mounted parallel with the specimen surface using a simple custom-made sample slit. Finally, the grid is transferred to the standard FIB grid holder for final thinning with standard procedures. This new cutting geometry provides clear viewing angles for monitoring the milling process, which solves the difficulty of judging whether the specimen has been entirely detached from the bulk material, with the least possible damage to the surrounding materials. With an improved success rate and efficiency, this plan-view FIB lift-out specimen preparation technique should have a wide application for material science. Copyright © 2017 The Authors. Published by Elsevier B.V. All rights reserved.

Low field magnetocaloric effect in bulk and ribbon alloy La(Fe0.88Si0.12)13

NASA Astrophysics Data System (ADS)

Vuong, Van-Hiep; Do-Thi, Kim-Anh; Nguyen, Duy-Thien; Nguyen, Quang-Hoa; Hoang, Nam-Nhat

2018-03-01

Low-field magnetocaloric effect occurred in itinerant metamagnetic materials is at core for magnetic cooling application. This works reports the magnetocaloric responses obtained at 1.35 T for the silicon-doped iron-based binary alloy La(Fe0.88Si0.12)13 in the bulk and ribbon form. Both samples possess a same symmetry but with different crystallite sizes and lattice parameters. The ribbon sample shows a larger maximum entropy change (nearly 8.5 times larger) and a higher Curie temperature (5 K higher) in comparison with that of the bulk sample. The obtained relative cooling power for the ribbon is also larger and very promising for application (RCP = 153 J/kg versus 25.2 J/kg for the bulk). The origin of the effect observed is assigned to the occurrence of negative magnetovolume effect in the ribbon structure with limit crystallization, caused by rapid cooling process at the preparation, which induced smaller crystallite size and large lattice constant at the overall weaker local crystal field.

Sampling hazelnuts for aflatoxin: uncertainty associated with sampling, sample preparation, and analysis.

PubMed

Ozay, Guner; Seyhan, Ferda; Yilmaz, Aysun; Whitaker, Thomas B; Slate, Andrew B; Giesbrecht, Francis

2006-01-01

The variability associated with the aflatoxin test procedure used to estimate aflatoxin levels in bulk shipments of hazelnuts was investigated. Sixteen 10 kg samples of shelled hazelnuts were taken from each of 20 lots that were suspected of aflatoxin contamination. The total variance associated with testing shelled hazelnuts was estimated and partitioned into sampling, sample preparation, and analytical variance components. Each variance component increased as aflatoxin concentration (either B1 or total) increased. With the use of regression analysis, mathematical expressions were developed to model the relationship between aflatoxin concentration and the total, sampling, sample preparation, and analytical variances. The expressions for these relationships were used to estimate the variance for any sample size, subsample size, and number of analyses for a specific aflatoxin concentration. The sampling, sample preparation, and analytical variances associated with estimating aflatoxin in a hazelnut lot at a total aflatoxin level of 10 ng/g and using a 10 kg sample, a 50 g subsample, dry comminution with a Robot Coupe mill, and a high-performance liquid chromatographic analytical method are 174.40, 0.74, and 0.27, respectively. The sampling, sample preparation, and analytical steps of the aflatoxin test procedure accounted for 99.4, 0.4, and 0.2% of the total variability, respectively.

Inhomogeneities and superconductivity in poly-phase Fe-Se-Te systems

NASA Astrophysics Data System (ADS)

Hartwig, S.; Schäfer, N.; Schulze, M.; Landsgesell, S.; Abou-Ras, D.; Blum, Ch. G. F.; Wurmehl, S.; Sokolowski, A.; Büchner, B.; Prokeš, K.

2018-02-01

The impact of synthesis conditions, post-preparation heating procedure, aging and influence of pressure on the superconducting properties of FeSe0.4Te0.6 crystals is reported. Two FeSe0.4Te0.6 single crystals were used in the study, prepared from stoichiometric melt but cooled down with very different cooling rates, and investigated using magnetic bulk and electrical-resistivity methods. The fast-cooled crystal contains large inclusions of Fe3Se2.1Te1.8 and exhibits bulk superconductivity in its as-prepared state, while the other is homogeneous and shows only traces of superconductivity. AC susceptibility measurements under hydrostatic pressure show that the superconducting transition temperature of the inhomogeneous crystal increases from 12.3 K at ambient pressure to Tsc = 17.9 K at 9 kbar. On the other hand, neither pressure nor mechanically-induced stress is sufficient to induce superconductivity in the homogeneous crystal. However, an additional heat treatment at 673 K followed by fast cooling down and/or long-term aging at ambient conditions leads to the appearance of bulk superconductivity also in the latter sample. This sample remains homogeneous on a scale down to few μm but shows an additional magnetic phase transition around 130 K suggesting that it must be inhomogeneous. For comparison also Fe3Se2.1Te1.8 polycrystals have been prepared and their magnetic properties have been studied. It appears that this phase is not superconducting by itself. It is concluded that nano-scale inhomogeneities that appear in the FeSexTe1-x system due to a spinodal decomposition in the solid state are necessary for bulk superconductivity, possibly due to minor changes in the crystal structure and microstructure. Macroscopic inclusions quenched by fast cooling from high temperatures lead obviously to strain and hence variations in the lattice constants, an effect that is further supported by application of pressure/stress.

Understanding the effect of surface/bulk defects on the photocatalytic activity of TiO2: anatase versus rutile.

PubMed

Yan, Junqing; Wu, Guangjun; Guan, Naijia; Li, Landong; Li, Zhuoxin; Cao, Xingzhong

2013-07-14

The sole effect of surface/bulk defects of TiO2 samples on their photocatalytic activity was investigated. Nano-sized anatase and rutile TiO2 were prepared by hydrothermal method and their surface/bulk defects were adjusted simply by calcination at different temperatures, i.e. 400-700 °C. High temperature calcinations induced the growth of crystalline sizes and a decrease in the surface areas, while the crystalline phase and the exposed facets were kept unchanged during calcination, as indicated by the characterization results from XRD, Raman, nitrogen adsorption-desorption, TEM and UV-Vis spectra. The existence of surface/bulk defects in calcined TiO2 samples was confirmed by photoluminescence and XPS spectra, and the surface/bulk defect ratio was quantitatively analyzed according to positron annihilation results. The photocatalytic activity of calcined TiO2 samples was evaluated in the photocatalytic reforming of methanol and the photocatalytic oxidation of α-phenethyl alcohol. Based on the characterization and catalytic results, a direct correlation between the surface specific photocatalytic activity and the surface/bulk defect density ratio could be drawn for both anatase TiO2 and rutile TiO2. The surface defects of TiO2, i.e. oxygen vacancy clusters, could promote the separation of electron-hole pairs under irradiation, and therefore, enhance the activity during photocatalytic reaction.

The Influence of Sintering Temperature on the Microstructure and Thermoelectric Properties of n-Type Bi2Te3- x Se x Nanomaterials

NASA Astrophysics Data System (ADS)

Du, Y.; Cai, K. F.; Li, H.; An, B. J.

2011-05-01

Pure Bi2Te3 and Bi2Se3 nanopowders were hydrothermally synthesized, and n-type Bi2Te3- x Se x bulk samples were prepared by hot pressing a mixture of Bi2Te3 and Bi2Se3 nanopowders at 623 K, 648 K or 673 K and 80 MPa in vacuum. The phase composition of the powders and bulk samples were characterized by x-ray diffraction. The morphology of the powders was examined by transmission electron microscopy. The microstructure and composition of the bulk samples were characterized by field-emission scanning electron microscopy and energy-dispersive x-ray spectroscopy, respectively. The density of the samples increased with sintering temperature. The samples were somewhat oxidized, and the amount of oxide (Bi2TeO5) present increased with sintering temperature. The samples consisted of sheet-like grains with a thickness less than 100 nm. Seebeck coefficient, electrical conductivity, and thermal conductivity of the samples were measured from room temperature up to 573 K. Throughout the temperature range investigated, the sample sintered at 623 K had a higher power factor than the samples sintered at 648 K or 673 K.

Structural differences existing in bulk and nanoparticles of Y{sub 2}Sn{sub 2}O{sub 7}: Investigated by experimental and theoretical methods

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nigam, Sandeep, E-mail: snigam@barc.gov.in; Sudarsan, V., E-mail: vsudar@barc.gov.in; Majumder, C.

Present manuscript deals with the structural changes associated with transformation of bulk Y{sub 2}Sn{sub 2}O{sub 7} into nanoparticles of Y{sub 2}Sn{sub 2}O{sub 7}. Nanoparticles of Y{sub 2}Sn{sub 2}O{sub 7} both undoped and Eu{sup 3+} doped, were prepared at a relatively low temperature (700 °C) and investigated for their structural and luminescence properties and compared them with that of bulk Y{sub 2}Sn{sub 2}O{sub 7} sample prepared by the solid-state method at 1300 °C. Significant distortion in geometry and electron density distribution around Y{sup 3+}/Eu{sup 3+} ions in nanoparticles are confirmed from the Rietveld refinement of the powder X-ray diffraction patterns andmore » theoretical calculations based on the density functional theory (DFT). The SnO{sub 6} octahedron in Y{sub 2}Sn{sub 2}O{sub 7} is more expanded in nanoparticles compared to bulk. Iso-surface density distribution reveals that while bulk sample shows typical ionic feature in Y/Eu--O bonds, nanoparticle sample shows sharing of electron density along bond axis pertaining to covalent character. These inferences are further supported by the doped Eu{sup 3+} luminescence and calculated Ω{sub 2} and Ω{sub 4} parameters. - Graphical abstract: YO{sub 8} scalenohedron present in bulk and nanoparticles of Y{sub 2}Sn{sub 2}O{sub 7}.Variation of the electron density around Y{sup 3+} ions in YO{sub 8} polyhedron is also shown in bulk and nanoparticles of Y{sub 2}Sn{sub 2}O{sub 7}. The difference in the extent of ionic/covalent nature of the Y--O bond is clearly seen the contour plot of electron density. Highlights: ► YO{sub 8} scalenohedron is axially and equatorially distorted in Y{sub 2}Sn{sub 2}O{sub 7} nanoparticles. ► Enlargement of SnO{sub 6} octahedron in nanoparticles of Y{sub 2}Sn{sub 2}O{sub 7} compared to bulk. ► Less symmetric charge distribution around Y{sup 3+} ions in Y{sub 2}Sn{sub 2}O{sub 7} nanoparticles.« less

Elution of monomer from different bulk fill dental composite resins.

PubMed

Cebe, Mehmet Ata; Cebe, Fatma; Cengiz, Mehmet Fatih; Cetin, Ali Rıza; Arpag, Osman Fatih; Ozturk, Bora

2015-07-01

The purpose of this study was to evaluate the elution of Bis-GMA, TEGDMA, HEMA, and Bis-EMA monomers from six bulk fill composite resins over four different time periods, using HPLC. Six different composite resin materials were used in the present study: Tetric Evo Ceram Bulk Fill (Ivoclar Vivadent, Amherst, NY), X-tra Fill (VOCO, Cuxhaven, Germany), Sonic Fill (Kerr, Orange, CA, USA), Filtek Bulk Fill (3M ESPE Dental Product, St. Paul, MN), SDR (Dentsply, Konstanz, Germany), EQUIA (GC America INC, Alsip, IL). The samples (4mm thickness, 5mm diameter) were prepared and polymerized for 20s with a light emitted diode unit. After fabrication, each sample was immediately immersed in 75wt% ethanol/water solution used as extraction fluid and stored in the amber colored bottles at room temperature. Ethanol/water samples were taken (0.5mL) at predefined time intervals:10m (T1), 1h (T2), 24h (T3) and 30 days (T4). These samples were analyzed by HPLC. The obtained data were analyzed with one-way ANOVA and Tukey HSD at significance level of p<0.05. Amount of eluted Bis-EMA and Bis-GMA from Tetric Evo Ceram Bulk Fill and amount of eluted TEGDMA and HEMA from X-tra Fill higher than others composites (p<0.05). Residual monomers were eluted from bulk fill composite resins in all time periods and the amount of eluted monomers was increased with time. Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Effect of Ca substitution on some physical properties of nano-structured and bulk Ni-ferrite samples

NASA Astrophysics Data System (ADS)

Assar, S. T.; Abosheiasha, H. F.

2015-01-01

Nanoparticles of Ni1-xCaxFe2O4 (x=0.0, 0.02, 0.04, 0.06 and 0.10) were prepared by citrate precursor method. A part of these samples was sintered at 600 °C for 2 h in order to keep the particles within the nano-size while the other part was sintered at 1000 °C to let the particles to grow to the bulk size. The effect of Ca2+ ion substitution in nickel ferrite on some structural, magnetic, electrical and thermal properties was investigated. All samples were characterized by using X-ray diffraction (XRD), transmission electron microscope (TEM), Fourier transform infrared spectroscopy (FTIR) and vibrating sample magnetometer (VSM). A two probe method was used to measure the dc electrical conductivity whereas the photoacoustic (PA) technique was used to determine the thermal diffusivity of the samples. To interpret different experimental results for nano and bulk samples some cation distributions were assumed based on the VSM and XRD data. These suggested cation distributions give logical explanations for other experimental results such as the observed values of the absorption bands in FTIR spectra and the dc conductivity results. Finally, in the thermal measurements it was found that increasing the Ca2+ ion content causes a decrease in the thermal diffusivity of both nano and bulk samples. The explanation of this behavior is ascribed to the phonon-phonon scattering.

Evidence for pigmentary hematite on Mars based on optical, magnetic, and Moessbauer studies of superparamagnetic (nanocrystalline) hematite

NASA Technical Reports Server (NTRS)

Morris, Richard V.; Agresti, David G.; Newcomb, Jeffery A.; Shelfer, Tad D.; Lauer, Howard V., Jr.

1989-01-01

Samples containing variable amounts of superparamagnetic hematite (sp-Hm) were prepared by a method in which the sp-Hm particles were dispersed throughout larger particles of silica gel, and the optical and magnetic properties of these samples were compared with those of larger-diameter hematite (bulk-Hm). It is shown that the optical properties of sp-Hm are different from those of bulk-Hm. Implications of the results for mineralogical interpretations of spectral data for the Martian surface and its terrestrial analogues are discussed. It is concluded that features resulting from ferric iron in the Martian spectral data and the results of the Viking magnetic properties experiment are both consistent with hematite present as both sp-Hm and bulk-Hm; the hematite particles most likely occur in pigmentary form, i.e., as particles dispersed throughout the volume of a spectrally neutral material.

Electrical switching studies on Si15Te85-xCux bulk (1 ≤ x ≤ 5) glasses

NASA Astrophysics Data System (ADS)

Roy, Diptoshi; Nadig, Chinmayi H. S.; Krishnan, Aravindh; Karanam, Akshath; Abhilash, R.; Jagannatha K., B.; Das, Chandasree

2018-05-01

Bulk ingots of Si15Te85-xCux (1 ≤ x ≤ 5) glasses are concocted by typical melt quenching technique. XRD validate the non-crystalline feature of the prepared quenched sample. The samples are found to display threshold type of electrical switching behavior. The switching behavior on all the samples is noticed without any disturbances. Compositional dependence of threshold voltage of Si15Te85-xCux (1 ≤ x ≤ 5) glasses has been studied and it has been found that VT increases as the atomic percentage of dopant (copper) increases in the host matrix. The distinguished behavior has been envisaged and correlated to the improvement in network connectivity and rigidity with the addition of Cu.

Innovative Processing of Composites for Ultra-High Temperature Applications. Book 3

DTIC Science & Technology

1993-11-01

SiC Samples Prepared with Four Preceramic Polymer Infiltration / Pyrolysis (at 15750C) Cycles Figure 21 Scanning Electron...Micrograph of Large Pores near the Surface of Siliconized SIC Sample with Four Preceramic Polymer Infiltration / Pyrolysis (at 1575*C) Cycles II...In order to achieve dense, bulk composites with maximum SiC /Si ratio, two infiltration / pyrolysis cycles were used. S (4) After siliconization,

9 CFR 113.209 - Rabies Vaccine, Killed Virus.

Code of Federal Regulations, 2010 CFR

2010-01-01

... immunogenicity of vaccine prepared with virus at the highest passage from the Master Seed shall be established in... the availability of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov... observation period, the serial is unsatisfactory. (3) Potency test. Bulk or final container samples of...

The {alpha}-particle excited scintillation response of the liquid phase epitaxy grown LuAG:Ce thin films

DOE Office of Scientific and Technical Information (OSTI.GOV)

Prusa, P.; Cechak, T.; Mares, J. A.

2008-01-28

Liquid phase epitaxy grown Lu{sub 3}Al{sub 5}O{sub 12}:Ce (LuAG:Ce) 20 {mu}m thick films and plate cut from the bulk Czochralski-grown LuAG:Ce crystal were prepared for comparison of photoelectron yield (PhY) and PhY dependence on shaping time (0.5-10 {mu}s). {sup 241}Am ({alpha} particles) was used for excitation. At the 0.5 {mu}s shaping time, the best film shows comparable PhY with the bulk sample. PhY of bulk material increases noticeably more with shaping time than that of the films. Energy resolution of films is better. Influence of Pb{sup 2+} contamination in the films (from the flux) and antisite Lu{sub Al} defect inmore » bulk material is discussed.« less

Influence of addition of degassed water on bulk nanobubbles.

PubMed

Tuziuti, Toru; Yasui, Kyuichi; Kanematsu, Wataru

2018-05-01

The effects of the addition of degassed water on bulk nanobubbles (ultrafine bubbles) of air in liquid water were investigated by measuring the volumetric concentration and size distribution at different dissolved air degree of saturation (DOS) values. The proportion of degassed water mixed with water containing bulk nanobubbles was increased to prepare samples having lower DOS values. It was found that the volumetric concentration of nanobubbles mostly decreased and the average nanobubble size became larger as the DOS was decreased. In our proposed mechanism, smaller nanobubbles are selectively dissolved into the surrounding liquid by Laplace pressure due to surface tension as the DOS is reduced. These results demonstrate that stable bulk nanobubbles are present even in water undersaturated with gas. The role of nanobubble under an ultrasound is also discussed. Copyright © 2018 Elsevier B.V. All rights reserved.

Enhanced bulk heterojunction devices prepared by thermal and solvent vapor annealing processes

DOEpatents

Forrest, Stephen R.; Thompson, Mark E.; Wei, Guodan; Wang, Siyi

2017-09-19

A method of preparing a bulk heterojunction organic photovoltaic cell through combinations of thermal and solvent vapor annealing are described. Bulk heterojunction films may prepared by known methods such as spin coating, and then exposed to one or more vaporized solvents and thermally annealed in an effort to enhance the crystalline nature of the photoactive materials.

Highly Enhanced Thermoelectric Properties of Bi/Bi2S3 Nanocomposites.

PubMed

Ge, Zhen-Hua; Qin, Peng; He, DongSheng; Chong, Xiaoyu; Feng, Dan; Ji, Yi-Hong; Feng, Jing; He, Jiaqing

2017-02-08

Bismuth sulfide (Bi 2 S 3 ) has been of high interest for thermoelectric applications due to the high abundance of sulfur on Earth. However, the low electrical conductivity of pristine Bi 2 S 3 results in a low figure of merit (ZT). In this work, Bi 2 S 3 @Bi core-shell nanowires with different Bi shell thicknesses were prepared by a hydrothermal method. The core-shell nanowires were densified to Bi/Bi 2 S 3 nanocomposite by spark plasma sintering (SPS), and the structure of the nanowire was maintained as the nanocomposite due to rapid SPS processing and low sintering temperature. The thermoelectric properties of bulk samples were investigated. The electrical conductivity of a bulk sample after sintering at 673 K for 5 min using Bi 2 S 3 @Bi nanowire powders prepared by treating Bi 2 S 3 nanowires in a hydrazine solution for 3 h is 3 orders of magnitude greater than that of a pristine Bi 2 S 3 sample. The nanocomposite possessed the highest ZT value of 0.36 at 623 K. This represents a new strategy for densifying core-shell powders to enhance their thermoelectric properties.

Coagulase-negative Staphylococcus species in bulk milk: Prevalence, distribution, and associated subgroup- and species-specific risk factors.

PubMed

De Visscher, A; Piepers, S; Haesebrouck, F; Supré, K; De Vliegher, S

2017-01-01

Coagulase-negative staphylococci (CNS) have become the main pathogens causing bovine mastitis in recent years. A huge variation in species distribution among herds has been observed in several studies, emphasizing the need to identify subgroup- and species-specific herd-level factors to improve our understanding of the differences in ecological and epidemiological nature between species. The use of bulk milk samples enables the inclusion of a large(r) number of herds needed to identify herd-level risk factors and increases the likelihood of recovering enough isolates per species needed for conducting subgroup- and, eventually, species-specific analyses at the same time. This study aimed to describe the prevalence and distribution of CNS species in bulk milk samples and to identify associated subgroup- and species-specific herd-level factors. Ninety percent of all bulk milk samples yielded CNS. Staphylococcus equorum was the predominant species, followed by Staphylococcus haemolyticus and Staphylococcus epidermidis. A seasonal effect was observed for several CNS species. Bulk milk samples from herds with a loose-pack or a tiestall housing system were more likely to yield CNS species compared with herds with a freestall barn, except for S. epidermidis, Staphylococcus simulans, and Staphylococcus cohnii. In September, herds in which udders were clipped had lower odds of yielding Staphylococcus chromogenes, S. simulans, and Staphylococcus xylosus, the CNS species assumed to be most relevant for udder health, in their bulk milk than herds in which udder clipping was not practiced. Bulk milk of herds participating in a monthly veterinary udder health-monitoring program was more likely to yield these 3 CNS species. Herds always receiving their milk quality premium or predisinfecting teats before attachment of the milking cluster had lower odds of having S. equorum in their bulk milk. Herds not using a single dry cotton or paper towel for each cow during premilking udder preparation were more likely to have S. cohnii-positive bulk milk. Herds in which flushing with hot water or steam of the milking cluster after having milked a cow with a (sub)clinical mastitis was applied, were less likely to yield S. simulans, S. haemolyticus, and S. cohnii in their bulk milk. Always wearing gloves during milking decreased the odds of having Staphylococcus devriesei-positive bulk milk. Tap water from the public drinking system used as drinking water increased the odds of yielding S. simulans in the bulk milk. In conclusion, CNS are highly prevalent in bulk milk and might originate from the environment for some species (we hypothesize this is true for S. equorum or S. cohnii), or from within the udder (e.g., for S. simulans). Studies collecting bulk milk and quarter milk samples at the same time along with environmental samples are needed to determine the exact origin of the different (subgroups of) CNS species present in bulk milk using strain-typing techniques. Copyright © 2017 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

The effect of grain size and cement content on index properties of weakly solidified artificial sandstones

NASA Astrophysics Data System (ADS)

Atapour, Hadi; Mortazavi, Ali

2018-04-01

The effects of textural characteristics, especially grain size, on index properties of weakly solidified artificial sandstones are studied. For this purpose, a relatively large number of laboratory tests were carried out on artificial sandstones that were produced in the laboratory. The prepared samples represent fifteen sandstone types consisting of five different median grain sizes and three different cement contents. Indices rock properties including effective porosity, bulk density, point load strength index, and Schmidt hammer values (SHVs) were determined. Experimental results showed that the grain size has significant effects on index properties of weakly solidified sandstones. The porosity of samples is inversely related to the grain size and decreases linearly as grain size increases. While a direct relationship was observed between grain size and dry bulk density, as bulk density increased with increasing median grain size. Furthermore, it was observed that the point load strength index and SHV of samples increased as a result of grain size increase. These observations are indirectly related to the porosity decrease as a function of median grain size.

Preparation and Certification of Two New Bulk Welding Fume Reference Materials for Use in Laboratories Undertaking Analysis of Occupational Hygiene Samples

PubMed Central

Butler, Owen; Musgrove, Darren; Stacey, Peter

2014-01-01

Workers can be exposed to fume, arising from welding activities, which contain toxic metals and metalloids. Occupational hygienists need to assess and ultimately minimize such exposure risks. The monitoring of the concentration of particles in workplace air is one assessment approach whereby fume, from representative welding activities, is sampled onto a filter and returned to a laboratory for analysis. Inductively coupled plasma-atomic emission spectrometry and inductively coupled plasma-mass spectrometry are generally employed as instrumental techniques of choice for the analysis of such filter samples. An inherent difficulty, however, with inductively coupled plasma-based analytical techniques is that they typically require a sample to be presented for analysis in the form of a solution. The efficiency of the required dissolution step relies heavily upon the skill and experience of the analyst involved. A useful tool in assessing the efficacy of this dissolution step would be the availability and subsequent analysis of welding fume reference materials with stated elemental concentrations and matrices that match as closely as possible the matrix composition of welding fume samples submitted to laboratories for analysis. This article describes work undertaken at the Health and Safety Laboratory to prepare and certify two new bulk welding fume reference materials that can be routinely used by analysts to assess the performance of the digestion procedures they employ in their laboratories. PMID:24499055

Preparation and certification of two new bulk welding fume reference materials for use in laboratories undertaking analysis of occupational hygiene samples.

PubMed

Butler, Owen; Musgrove, Darren; Stacey, Peter

2014-01-01

Workers can be exposed to fume, arising from welding activities, which contain toxic metals and metalloids. Occupational hygienists need to assess and ultimately minimize such exposure risks. The monitoring of the concentration of particles in workplace air is one assessment approach whereby fume, from representative welding activities, is sampled onto a filter and returned to a laboratory for analysis. Inductively coupled plasma-atomic emission spectrometry and inductively coupled plasma-mass spectrometry are generally employed as instrumental techniques of choice for the analysis of such filter samples. An inherent difficulty, however, with inductively coupled plasma-based analytical techniques is that they typically require a sample to be presented for analysis in the form of a solution. The efficiency of the required dissolution step relies heavily upon the skill and experience of the analyst involved. A useful tool in assessing the efficacy of this dissolution step would be the availability and subsequent analysis of welding fume reference materials with stated elemental concentrations and matrices that match as closely as possible the matrix composition of welding fume samples submitted to laboratories for analysis. This article describes work undertaken at the Health and Safety Laboratory to prepare and certify two new bulk welding fume reference materials that can be routinely used by analysts to assess the performance of the digestion procedures they employ in their laboratories.

Results and analysis of saltstone cores taken from saltstone disposal unit cell 2A

DOE Office of Scientific and Technical Information (OSTI.GOV)

Reigel, M. M.; Hill, K. A.

2016-03-01

As part of an ongoing Performance Assessment (PA) Maintenance Plan, Savannah River Remediation (SRR) has developed a sampling and analyses strategy to facilitate the comparison of field-emplaced samples (i.e., saltstone placed and cured in a Saltstone Disposal Unit (SDU)) with samples prepared and cured in the laboratory. The primary objectives of the Sampling and Analyses Plan (SAP) are; (1) to demonstrate a correlation between the measured properties of laboratory-prepared, simulant samples (termed Sample Set 3), and the field-emplaced saltstone samples (termed Sample Set 9), and (2) to validate property values assumed for the Saltstone Disposal Facility (SDF) PA modeling. Themore » analysis and property data for Sample Set 9 (i.e. six core samples extracted from SDU Cell 2A (SDU2A)) are documented in this report, and where applicable, the results are compared to the results for Sample Set 3. Relevant properties to demonstrate the aforementioned objectives include bulk density, porosity, saturated hydraulic conductivity (SHC), and radionuclide leaching behavior.« less

Structural and superconducting features of Tl-1223 prepared at ambient pressure

DOE PAGES

Shipra, Fnu; Idrobo Tapia, Juan Carlos; Sefat, Athena Safa

2015-09-25

This study provides an account of the bulk preparation of TlBa 2Ca 2Cu 3O 9-δ (Tl-1223) superconductor at ambient pressure, and the Tc features under thermal-annealing conditions. The ‘as-prepared’ Tl-1223 (Tc =106 K) presents a significantly higher T c = 125 K after annealing the polycrystalline material in either flowing Ar+4% H 2, or N 2 gases. In order to understand the fundamental reasons for a particular Tc, we refined the average bulk structures using powder X-ray diffraction data. Although Ar+4%H2 annealed Tl- 1223 shows an increased ‘c’ lattice parameter, it shrinks by 0.03% (approximately unchanged) upon N2 anneal. Duemore » to such indeterminate conclusions on the average structural changes, local structures were investigated at using aberration-corrected scanning-transmission electron microscopy technique. Similar compositional changes in the atomic arrangements of both annealed-samples of Tl-1223 were detected in which the plane containing Ca atomic layer gives a non-uniform contrast, due to substitution of some heavier Tl. In this report, extensive bulk properties are summarized through temperature-dependent resistivity, and shielding and Meissner fractions of magnetic susceptibility results; the bulk and local structures are investigated to correlate to properties.« less

Phase-coexistence and thermal hysteresis in samples comprising adventitiously doped MnAs nanocrystals: programming of aggregate properties in magnetostructural nanomaterials.

PubMed

Zhang, Yanhua; Regmi, Rajesh; Liu, Yi; Lawes, Gavin; Brock, Stephanie L

2014-07-22

Small changes in the synthesis of MnAs nanoparticles lead to materials with distinct behavior. Samples prepared by slow heating to 523 K (type-A) exhibit the characteristic magnetostructural transition from the ferromagnetic hexagonal (α) to the paramagnetic orthorhombic (β) phase of bulk MnAs at Tp = 312 K, whereas those prepared by rapid nucleation at 603 K (type-B) adopt the β structure at room temperature and exhibit anomalous magnetic properties. The behavior of type-B nanoparticles is due to P-incorporation (up to 3%), attributed to reaction of the solvent (trioctylphosphine oxide). P-incorporation results in a decrease in the unit cell volume (∼1%) and shifts Tp below room temperature. Temperature-dependent X-ray diffraction reveals a large region of phase-coexistence, up to 90 K, which may reflect small differences in Tp from particle-to-particle within the nearly monodisperse sample. The large coexistence range coupled to the thermal hysteresis results in process-dependent phase mixtures. As-prepared type-B samples exhibiting the β structure at room temperature convert to a mixture of α and β after the sample has been cooled to 77 K and rewarmed to room temperature. This change is reflected in the magnetic response, which shows an increased moment and a shift in the temperature hysteresis loop after cooling. The proportion of α present at room temperature can also be augmented by application of an external magnetic field. Both doped (type-B) and undoped (type-A) MnAs nanoparticles show significant thermal hysteresis narrowing relative to their bulk phases, suggesting that formation of nanoparticles may be an effective method to reduce thermal losses in magnetic refrigeration applications.

Implications of PCR and ELISA results on the routes of bulk-tank contamination with Mycobacterium avium ssp. paratuberculosis.

PubMed

Beaver, A; Cazer, C L; Ruegg, P L; Gröhn, Y T; Schukken, Y H

2016-02-01

Mycobacterium avium ssp. paratuberculosis (MAP), the etiologic agent of Johne's disease in dairy cattle, may enter the bulk tank via environmental contamination or direct excretion into milk. Traditionally, diagnostics to identify MAP in milk target either MAP antibodies (by ELISA) or the organism itself (by culture or PCR). High ELISA titers may be directly associated with excretion of MAP into milk but only indirectly linked to environmental contamination of the bulk tank. Patterns of bulk-milk ELISA and bulk-milk PCR results could therefore provide insight into the routes of contamination and level of infection or environmental burden. Coupled with questionnaire responses pertaining to management, the results of these diagnostic tests could reveal correlations with herd characteristics or on-farm practices that distinguish herds with high and low environmental bulk-tank MAP contamination. A questionnaire on hygiene, management, and Johne's specific parameters was administered to 292 dairy farms in New York, Oregon, and Wisconsin. Bulk-tank samples were collected from each farm for evaluation by real-time PCR and ELISA. Before DNA extraction and testing of the unknown samples, bulk-milk template preparation was optimized with respect to parameters such as MAP fractionation patterns and lysis. Two regression models were developed to explore the relationships among bulk-tank PCR, ELISA, environmental predictors, and herd characteristics. First, ELISA optical density (OD) was designated as the outcome in a linear regression model. Second, the log odds of being PCR positive in the bulk tank were modeled using binary logistic regression with penalized maximum likelihood. The proportion of PCR-positive bulk tanks was highest for New York and for organic farms, providing a clue as to the geographical patterns of MAP-positive bulk-tank samples and relationship to production type. Bulk-milk PCR positivity was also higher for large relative to small herds. The models revealed that bulk-milk PCR result could predict ELISA OD, with PCR-positive results corresponding to high bulk-milk ELISA titers. Similarly, ELISA was a predictor of PCR result, although the association was stronger for organic farms. Despite agreement between high bulk-milk ELISA titers and positive PCR results, a large proportion of high ELISA farms had PCR-negative bulk tanks, suggesting that farms are able to maintain satisfactory hygiene and management despite a presence of MAP in these herds. Copyright © 2016 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Automated Clean Chemistry for Bulk Analysis of Environmental Swipe Samples - FY17 Year End Report

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ticknor, Brian W.; Metzger, Shalina C.; McBay, Eddy H.

Sample preparation methods for mass spectrometry are being automated using commercial-off-the-shelf (COTS) equipment to shorten lengthy and costly manual chemical purification procedures. This development addresses a serious need in the International Atomic Energy Agency’s Network of Analytical Laboratories (IAEA NWAL) to increase efficiency in the Bulk Analysis of Environmental Samples for Safeguards program with a method that allows unattended, overnight operation. In collaboration with Elemental Scientific Inc., the prepFAST-MC2 was designed based on COTS equipment. It was modified for uranium/plutonium separations using renewable columns packed with Eichrom TEVA and UTEVA resins, with a chemical separation method based on the Oakmore » Ridge National Laboratory (ORNL) NWAL chemical procedure. The newly designed prepFAST-SR has had several upgrades compared with the original prepFAST-MC2. Both systems are currently installed in the Ultra-Trace Forensics Science Center at ORNL.« less

Raman and dielectric studies of GdMnO3 bulk ceramics synthesized from nano powders

NASA Astrophysics Data System (ADS)

Samantaray, S.; Mishra, D. K.; Roul, B. K.

2017-05-01

Nanocrystalline GdMnO3 (GMO) powders has been synthesized by a simple chemical route i. e. pyrophoric reaction technique and then sintered in the form of bulk pellet at 850°C for 24 hours by adopting slow step sintering schedule. It is observed that by reducing the particles size, chemical route enhances the mixing process as well as decreasing the sintering temperature to get single phase material system in compared to the polycrystalline sample prepared directly from the micron sized commercial powder. Raman spectroscopic studies confirm that the sample is in single phase without any detectable impurity. Frequency dependent dielectric properties i.e., dielectric constant (K) and dielectric loss (tanδ) of GMO ceramics sintered at 850°C for 24 hours were studied at room temperature. The sample showed high K value (˜2736) in the frequency of 100 Hz at room temperature.

Laser-induced damage thresholds of bulk and coating optical materials at 1030  nm, 500  fs.

PubMed

Gallais, Laurent; Commandré, Mireille

2014-02-01

We report on extensive femtosecond laser damage threshold measurements of optical materials in both bulk and thin-film form. This study, which is based on published and new data, involved simple oxide and fluoride films, composite films made from a mixture of two dielectric materials, metallic films, and the surfaces of various bulk materials: oxides, fluorides, semiconductors, and ionic crystals. The samples were tested in comparable conditions at 1030 nm, 375 to 600 fs, under single-pulse irradiation. A large number of different samples prepared by different deposition techniques have been tested, involving classical materials used in the fabrication of optical thin film components (Ag, AlF3, Al2O3, HfO2, MgF2, Nb2O5, Pt, Sc2O3, SiO2, Ta2O5, Y2O3, and ZrO2) and their combination with codeposition processes. Their behaviors are compared with the surfaces of bulk materials (Al2O3, BaF2, CaF2, Ge, KBr, LiF, MgF2, NaCl, Quartz, Si, ZnS, ZnSe, and different silica glasses). Tabulated values of results are presented and discussed.

Microstructure and trapped field of YBCO bulk single-grain superconductors prepared by interior seeding

NASA Astrophysics Data System (ADS)

Radusovska, M.; Diko, P.; Piovarci, S.; Park, S.-D.; Jun, B.-H.; Kim, C.-J.

2017-10-01

The microstructural analyses of YBCO bulk single-grain superconductors grown by interior seeding with taller and shorter upper pellets have shown that a suitable upper pellet height can lower the porosity in the upper part of the sample, produce a more appropriate distribution of pinning centres in the form of Y-211 particles and suppress subgrain formation with a higher crystal misalignment in the c-growth sector (c-GS), which can lead to a higher measured trapped magnetic field and a more uniform cone of the trapped-field profile. The observed bulging of the sample surface at the c-GS can be explained by the edge melt distribution model, which shows that macroscopic mass transport to the growth sector occurs with higher growth rates.

Block Copolymer Adhesion Measured by Contact Mechanics Methods

NASA Astrophysics Data System (ADS)

Falsafi, A.; Bates, S.; Tirrell, M.; Pocius, A. V.

1997-03-01

Adhesion measurements for a series of polyolefin diblocks and triblocks are presented. These materials have poly(ethylene-propylene) or poly(ethyl-ethylene) rubbery block, and semicrystalline polyethylene block as physical crosslinker. The experiments consist of compression and decompression profiles of contact area between the samples as a function of normal load, analyzed by the JKR Theory. The samples are prepared either by formation of caps from the bulk material in melting and subsequent cooling, and/or coating them in thin films on surface modified elastic foundations of polydimethylsiloxane caps. The latter minimizes the viscoelastic losses which are dominant in the bulk of material. The effect of molecular architecture and microstructure on adhesion energy and dynamics of separation, obtained from decompression experiments, is discussed in view of their influence on molecular arrangements at the contacting surfaces.

Structural and transport properties of double perovskite Dy{sub 2}NiMnO{sub 6}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chanda, Sadhan, E-mail: sadhan.physics@gmail.com; Saha, Sujoy; Dutta, Alo

2015-02-15

Highlights: • Sol–gel citrate method is used to prepare the double perovskite Dy{sub 2}NiMnO{sub 6}. • Structure and dielectric relaxation of the sample are studied for nano and bulk phases. • The relaxation mechanism of the sample is modeled by Cole–Cole equation. • With increasing sintering temperature conductivity increases. • Electronic structures and magnetic properties have been studied by DFT calculations. - Abstract: The double perovskite oxide Dy{sub 2}NiMnO{sub 6} (DNMO) is synthesized in nano and bulk phase by the sol–gel citrate method. The Rietveld refinement of X-ray diffraction pattern of the sample at room temperature shows the monoclinic P2{submore » 1}/n phase. Dielectric relaxation of the sample is investigated in the impedance and electric modulus formalisms in the frequency range from 50 Hz to 1 MHz and in the temperature range from 253 to 415 K. The Cole–Cole model is used to explain the relaxation mechanism in DNMO. The frequency-dependent maxima in the imaginary part of impedance are found to obey an Arrhenius law with activation energy of 0.346 and 0.344 eV for nano and bulk DNMO, respectively. A significant increase in conductivity of bulk DNMO has been observed than that of the nanoceramic. Electronic structures and magnetic properties of DNMO have been studied by performing first principles calculation based on density functional theory.« less

Preparation by Poly(Acrylic Acid) Sol-Gel Method and Thermoelectric Properties of γ-Na x CoO2 Bulk Materials

NASA Astrophysics Data System (ADS)

Li, Xiaoyu; Zhang, Li; Tang, Xinfeng

2017-11-01

γ-Na x CoO2 single-phase powders have been synthesized by a poly(acrylic acid) (PAA) sol-gel (SG) method, and γ-Na x CoO2 bulk ceramic fabricated using spark plasma sintering. The effects of the PAA concentration on the sample phase composition and morphology were investigated. The thermoelectric properties of the γ-Na x CoO2 bulk ceramic were also studied. The results show that the PAA concentration did not significantly affect the crystalline phase of the product. However, agglomeration of γ-Na x CoO2 crystals was suppressed by the steric effect of PAA. The Na x CoO2 bulk ceramic obtained using the PAA SG method had higher crystallographic anisotropy, better chemical homogeneity, and higher density than the sample obtained by solid-state reaction (SSR), leading to improved thermoelectric performance. The PAA SG sample had power factor (in-plane PF = σS 2) of 0.61 mW m-1 K-2 and dimensionless figure of merit ( ZT) along the in-plane direction of 0.19 at 900 K, higher than for the SSR sample (in-plane PF = 0.51 mW m-1 K-2, in-plane ZT = 0.17). These results demonstrate that a simple and feasible PAA SG method can be used for synthesis of Na x CoO2 ceramics with improved thermoelectric properties.

Production and Characterization of Bulk MgB2 Material made by the Combination of Crystalline and Carbon Coated Amorphous Boron Powders

NASA Astrophysics Data System (ADS)

Hiroki, K.; Muralidhar, M.; Koblischka, M. R.; Murakami, M.

2017-07-01

The object of this investigation is to reduce the cost of bulk production and in the same time to increase the critical current performance of bulk MgB2 material. High-purity commercial powders of Mg metal (99.9% purity) and two types of crystalline (99% purity) and 16.5 wt% carbon-coated, nanometer-sized amorphous boron powders (98.5% purity) were mixed in a nominal composition of MgB2 to reduce the boron cost and to see the effect on the superconducting and magnetic properties. Several samples were produced mixing the crystalline boron and carbon-coated, nanometer-sized amorphous boron powders in varying ratios (50:50, 60:40, 70:30, 80:20, 90:10) and synthesized using a single-step process using the solid state reaction around 800 °C for 3 h in pure argon atmosphere. The magnetization measurements exhibited a sharp superconducting transition temperature with T c, onset around 38.6 K to 37.2 K for the bulk samples prepared utilizing the mixture of crystalline boron and 16.5% carbon-coated amorphous boron. The critical current density at higher magnetic field was improved with addition of carbon-coated boron to crystalline boron in a ratio of 80:20. The highest self-field Jc around 215,000 A/cm2 and 37,000 A/cm2 were recorded at 20 K, self-field and 2 T for the sample with a ratio of 80:10. The present results clearly demonstrate that the bulk MgB2 performance can be improved by adding carbon-coated nano boron to crystalline boron, which will be attractive to reduce the cost of bulk MgB2 material for several industrial applications.

Fabrication of single domain GdBCO bulk superconductors by a new modified TSIG technique

NASA Astrophysics Data System (ADS)

Yang, W. M.; Zhi, X.; Chen, S. L.; Wang, M.; Li, J. W.; Ma, J.; Chao, X. X.

2014-01-01

Single domain GdBCO bulk superconductors have been fabricated with new and traditional solid phases by a top seeded infiltration and growth (TSIG) process technique. In the conventional TSIG process, three types of powders, such as Gd2BaCuO5, GdBa2Cu3O7-x and Ba3Cu5O8, must be prepared, but in our new modified TSIG technique, only BaCuO2 powders are required during the fabrication of the single domain GdBCO bulk superconductors. The solid phase used in the conventional process is Gd2BaCuO5 instead of the solid phase (Gd2O3 + BaCuO2) utilized in the new process. The liquid phase used in the conventional process is a mixture of (GdBa2Cu3O7-x + Ba3Cu5O8), and the liquid phase in the new process is a mixture of (Gd2O3 + 10BaCuO2 + 6CuO). Single domain GdBCO bulk superconductors have been fabricated with the new solid and liquid phases. The levitation force of the GdBCO bulk samples fabricated by the new solid phase is 28 N, which is slightly higher than that of the samples fabricated using the conventional solid phases (26 N). The microstructure and the levitation force of the samples indicate that this new method can greatly simplify the fabrication process, introduce nanometer-sized flux centers, improve the levitation force and working efficiency, and greatly reduce the cost of fabrication of single domain GdBCO bulk superconductors by the TSIG process.

Bulk superhard B-C-N nanocomposite compact and method for preparing thereof

DOEpatents

Zhao, Yusheng; He, Duanwei

2004-07-06

Bulk, superhard, B-C-N nanocomposite compact and method for preparing thereof. The bulk, superhard, nanocomposite compact is a well-sintered compact and includes nanocrystalline grains of at least one high-pressure phase of B-C-N surrounded by amorphous diamond-like carbon grain boundaries. The bulk compact has a Vicker's hardness of about 41-68 GPa. It is prepared by ball milling a mixture of graphite and hexagonal boron nitride, encapsulating the ball-milled mixture, and sintering the encapsulated ball-milled mixture at a pressure of about 5-25 GPa and at a temperature of about 1000-2500 K.

Fabrication and Evaluation of Superconducting and Semiconducting Materials

DTIC Science & Technology

1993-09-01

Laboratory Material Physics Branch by conducting investigations into the properties of superconducting , magnetic , and other solid state materials. Studies...Physics Branch in conducting research into applied problems such as the design of magnetic shielding and superconducting quantum interference device...SQUID) magnetometry detection of magnetic anomalies. SFA provided research assistance in the areas of bulk ceramic sample preparation. conversion

Significantly enhanced critical current density in nano-MgB2 grains rapidly formed at low temperature with homogeneous carbon doping

NASA Astrophysics Data System (ADS)

Liu, Yongchang; Lan, Feng; Ma, Zongqing; Chen, Ning; Li, Huijun; Barua, Shaon; Patel, Dipak; Shahriar, M.; Hossain, Al; Acar, S.; Kim, Jung Ho; Xue Dou, Shi

2015-05-01

High performance MgB2 bulks using carbon-coated amorphous boron as a boron precursor were fabricated by Cu-activated sintering at low temperature (600 °C, below the Mg melting point). Dense nano-MgB2 grains with a high level of homogeneous carbon doping were formed in these MgB2 samples. This type of microstructure can provide a stronger flux pinning force, together with depressed volatility and oxidation of Mg owing to the low-temperature Cu-activated sintering, leading to a significant improvement of critical current density (Jc) in the as-prepared samples. In particular, the value of Jc for the carbon-coated (Mg1.1B2)Cu0.05 sample prepared here is even above 1 × 105 A cm-2 at 20 K, 2 T. The results herein suggest that the combination of low-temperature Cu-activated sintering and employment of carbon-coated amorphous boron as a precursor could be a promising technique for the industrial production of practical MgB2 bulks or wires with excellent Jc, as the carbon-coated amorphous boron powder can be produced commercially at low cost, while the addition of Cu is very convenient and inexpensive.

Physical properties of the Nankai inner accretionary prism sediments at Site C0002, IODP Expedition 348.

NASA Astrophysics Data System (ADS)

Kitamura, M.; Kitajima, H.; Henry, P.; Valdez, R. D., II; Josh, M.; Tobin, H. J.; Saffer, D. M.; Hirose, T.; Toczko, S.; Maeda, L.

2014-12-01

Integrated Ocean Drilling Program (IODP) Nankai Trough Seismogenic Zone Experiment (NanTroSEIZE) Expedition 348 focused on deepening the existing riser hole at Site C0002 to ~3000 meters below seafloor (mbsf) to access the deep interior of the Miocene inner accretionary prism. This unique tectonic environment, which has never before been sampled in situ by ocean drilling, was characterized through riser drilling, logging while drilling (LWD), mud gas monitoring and sampling, and cuttings and core analysis. Shipboard physical properties measurements including moisture and density (MAD), electrical conductivity, P-wave, natural gamma ray, and magnetic susceptibility measurements were performed mainly on cuttings samples from 870.5 to 3058.5 mbsf, but also on core samples from 2163 and 2204 mbsf. MAD measurements were conducted on seawater-washed cuttings ("bulk cuttings") in two size fractions of >4 mm and 1-4 mm from 870.5 to 3058.5 mbsf, and hand-picked intact cuttings from the >4 mm size fractions within 1222.5-3058.5 mbsf interval. The bulk cuttings show grain density of ~2.7 g/cm3, bulk density of 1.9 g/cm3 to 2.2 g/cm3, and porosity of 50% to 32%. Compared to the values on bulk cuttings, the intact cuttings show almost the same grain density, but higher bulk density and lower porosity, respectively. Combined with the MAD measurements on hand-picked intact cuttings and discrete core samples from previous expeditions, porosity generally decreases from ~60% to ~20% from the seafloor to 3000 mbsf at Site C0002. Electrical conductivity and P-wave velocity on discrete samples, which were prepared from both cuttings and core samples in the depth interval of 1745.5-3058.5 mbsf, range 0.15-0.9 S/m and 1.7-4.5 km/s, respectively. The electrical resistivity on discrete samples is higher than the LWD resistivity data but the overall depth trends are similar. The electrical conductivity and P-wave velocity on discrete samples corrected for in-situ pressure and temperature will be presented. The shipboard physical properties measurements on cuttings are very limited but can be useful with careful treatment and observation.

Influence of mixing conditions on the rheological properties and structure of capillary suspensions

PubMed Central

Bossler, Frank; Weyrauch, Lydia; Schmidt, Robert; Koos, Erin

2017-01-01

The rheological properties of a suspension can be dramatically altered by adding a small amount of a secondary fluid that is immiscible with the bulk liquid. These capillary suspensions exist either in the pendular state where the secondary fluid preferentially wets the particles or the capillary state where the bulk fluid is preferentially wetting. The yield stress, as well as storage and loss moduli, depends on the size and distribution of secondary phase droplets created during sample preparation. Enhanced droplet breakup leads to stronger sample structures. In capillary state systems, this can be achieved by increasing the mixing speed and time of turbulent mixing using a dissolver stirrer. In the pendular state, increased mixing speed also leads to better droplet breakup, but spherical agglomeration is favored at longer times decreasing the yield stress. Additional mixing with a ball mill is shown to be beneficial to sample strength. The influence of viscosity variance between the bulk and second fluid on the droplet breakup is excluded by performing experiments with viscosity-matched fluids. These experiments show that the capillary state competes with the formation of Pickering emulsion droplets and is often more difficult to achieve than the pendular state. PMID:28194044

Meteorite Dust and Health - A Novel Approach for Determining Bulk Compositions for Toxicological Assessments of Precious Materials

NASA Technical Reports Server (NTRS)

Vander Kaaden, K. E.; Harrington, A. D.; McCubbin, F. M.

2017-01-01

With the resurgence of human curiosity to explore planetary bodies beyond our own, comes the possibility of health risks associated with the materials covering the surface of these planetary bodies. In order to mitigate these health risks and prepare ourselves for the eventuality of sending humans to other planetary bodies, toxicological evaluations of extraterrestrial materials is imperative (Harrington et al. 2017). Given our close proximity, as well as our increased datasets from various missions (e.g., Apollo, Mars Exploration Rovers, Dawn, etc…), the three most likely candidates for initial human surface exploration are the Moon, Mars, and asteroid 4Vesta. Seven samples, including lunar mare basalt NWA 4734, lunar regolith breccia NWA 7611, martian basalt Tissint, martian regolith breccia NWA 7034, a vestian basalt Berthoud, a vestian regolith breccia NWA 2060, and a terrestrial mid-ocean ridge basalt, were examined for bulk chemistry, mineralogy, geochemical reactivity, and inflammatory potential. In this study, we have taken alliquots from these samples, both the fresh samples and those that underwent iron leaching (Tissint, NWA 7034, NWA 4734, MORB), and performed low pressure, high temperature melting experiments to determine the bulk composition of the materials that were previously examined.

Comparison of methods for measuring atmospheric deposition of arsenic, cadmium, nickel and lead.

PubMed

Aas, Wenche; Alleman, Laurent Y; Bieber, Elke; Gladtke, Dieter; Houdret, Jean-Luc; Karlsson, Vuokko; Monies, Christian

2009-06-01

A comprehensive field intercomparison at four different types of European sites (two rural, one urban and one industrial) comparing three different collectors (wet only, bulk and Bergerhoff samplers) was conducted in the framework of the European Committee for Standardization (CEN) to create an European standard for the deposition of the four elements As, Cd, Ni and Pb. The purpose was to determine whether the proposed methods lead to results within the uncertainty required by the EU's daughter directive (70%). The main conclusion is that a different sampling strategy is needed for rural and industrial sites. Thus, the conclusions on uncertainties and sample approach are presented separately for the different approaches. The wet only and bulk collector ("bulk bottle method") are comparable at wet rural sites where the total deposition arises mainly from precipitation, the expanded uncertainty when comparing these two types of sampler are below 45% for As, Cd and Pb, 67% for Ni. At industrial sites and possibly very dry rural and urban sites it is necessary to use Bergerhoff samplers or a "bulk bottle+funnel method". It is not possible to address the total deposition estimation with these methods, but they will give the lowest estimate of the total deposition. The expanded uncertainties when comparing the Bergerhoff and the bulk bottle+funnel methods are below 50% for As and Cd, and 63% for Pb. The uncertainty for Ni was not addressed since the bulk bottle+funnel method did not include a full digestion procedure which is necessary for sites with high loads of undissolved metals. The lowest estimate can however be calculated by comparing parallel Bergerhoff samplers where the expanded uncertainty for Ni was 24%. The reproducibility is comparable to the between sampler/method uncertainties. Sampling and sample preparation were proved to be the main factors in the uncertainty budget of deposition measurements.

Analysis of ultraviolet photo-response of ZnO nanostructures prepared by electrodeposition and atomic layer deposition

NASA Astrophysics Data System (ADS)

Makhlouf, Houssin; Karam, Chantal; Lamouchi, Amina; Tingry, Sophie; Miele, Philippe; Habchi, Roland; Chtourou, Radhouane; Bechelany, Mikhael

2018-06-01

In this work, ZnO nanowires (ZnO NWs) and urchin-like ZnO nanowires (U-ZnO NWs) based on self-assembled ordered polystyrene sphere (PS) were successfully prepared by combining atomic layer deposition (ALD) and electrochemical deposition (ECD) processes to build UV photosensors. The photo-response of the prepared samples was investigated and compared. The growth of the nanowires on self-assembled, ordered PS introduces a significant modification on the morphology, crystal orientation and grain size of U-ZnO NWs compared to randomly, vertically aligned ZnO NWs, and therefore improves the photo-response of U-ZnO NWs. The photocurrent may be produced by either a surface or bulk-related process. For ZnO NW-based photosensors, the photocurrent was monitored by a surface related process, whereas, it was mainly governed by a bulk related process for U-ZnO NWs, resulting in a higher and faster photo-response. The study of the rise and decay time constants for both materials showed that these parameters were strikingly sensitive to the optical properties.

On the measurement of austenite in supermartensitic stainless steel by X-ray diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tolchard, Julian Richard, E-mail: tolchard@material.ntnu.no; Sømme, Astri; Solberg, Jan Ketil

2015-01-15

Sections of a 13Cr supermartensitic stainless steel were investigated to determine the optimum sample preparation for measurement of the austenite content by X-ray diffraction. The surface of several samples was mechanically ground or polished using media of grit sizes in the range 1–120 μm. The strained surface layer was afterwards removed stepwise by electropolishing, and the austenite content measured at each step. It was found that any level of mechanical grinding or polishing results in a reduction of the measured austenite fraction relative to the true bulk value, and that coarser grinding media impart greater damage and greater reduction inmore » the measured austenite content. The results thus highlight the importance of the electropolishing step in preparation of such samples, but suggest that the American Society for Testing and Materials standard E975-03 substantially overestimates the amount of material which needs to be removed to recover the true “bulk” content. - Highlights: • Quantitative Rietveld analysis of austenite/martensite ratio in supermartensitic stainless steels • Critical evaluation of sample preparation for residual austenite measurements by X-ray diffraction • Highlighting of the importance of electropolishing as a final preparation step.« less

"One-sample concept" micro-combinatory for high throughput TEM of binary films.

PubMed

Sáfrán, György

2018-04-01

Phases of thin films may remarkably differ from that of bulk. Unlike to the comprehensive data files of Binary Phase Diagrams [1] available for bulk, complete phase maps for thin binary layers do not exist. This is due to both the diverse metastable, non-equilibrium or instable phases feasible in thin films and the required volume of characterization work with analytical techniques like TEM, SAED and EDS. The aim of the present work was to develop a method that remarkably facilitates the TEM study of the diverse binary phases of thin films, or the creation of phase maps. A micro-combinatorial method was worked out that enables both preparation and study of a gradient two-component film within a single TEM specimen. For a demonstration of the technique thin Mn x Al 1- x binary samples with evolving concentration from x = 0 to x = 1 have been prepared so that the transition from pure Mn to pure Al covers a 1.5 mm long track within the 3 mm diameter TEM grid. The proposed method enables the preparation and study of thin combinatorial samples including all feasible phases as a function of composition or other deposition parameters. Contrary to known "combinatorial chemistry", in which a series of different samples are deposited in one run, and investigated, one at a time, the present micro-combinatorial method produces a single specimen condensing a complete library of a binary system that can be studied, efficiently, within a single TEM session. That provides extremely high throughput for TEM characterization of composition-dependent phases, exploration of new materials, or the construction of phase diagrams of binary films. Copyright © 2018 Elsevier B.V. All rights reserved.

Fracture toughness, diametrical strength, and fractography of amalgam and of amalgam to amalgam bonds.

PubMed

Bapna, M S; Mueller, H J

1993-01-01

Chevron-notch fracture toughness, diametrical tensile strength and fractography were evaluated for bulk amalgams and for bonds formed between new and 1-day-old amalgams of the same type. Three types of bonded specimens were prepared: 1) by mechanically roughening the 1-day-old amalgam with 600-grit paper; 2) using a new mercury-rich amalgam; and 3) using a bonding resin, either 4-META or a phosphate ester monomer. Similar values in bond properties were obtained with all bonding techniques for two commercial dispersed-phase bonded amalgams, one of which contained palladium; however, bulk fracture toughness of the palladium-containing amalgam was significantly less than for the palladium-free amalgam. This result reveals that the bonding of amalgam to amalgam, at least for these two amalgams, is a surface-related phenomenon, and thus, the traditional reporting of bonding properties as a percentage of bulk properties loses meaning. Short-rod geometry was more representative of the interfacial bond properties since these samples fractured within the interfacial bonds, while diametrical strength samples often fractured slightly away from the interface. The use of bonding resins did not improve bond fracture toughness for either amalgam, while the diametrical strength improved for one of the amalgams. The use of mercury-rich amalgam significantly improved the fracture toughness over all other techniques for one amalgam while proving to be similar to a 600-grit preparation for the second amalgam.(ABSTRACT TRUNCATED AT 250 WORDS)

Effect of annealing ambience on the formation of surface/bulk oxygen vacancies in TiO2 for photocatalytic hydrogen evolution

NASA Astrophysics Data System (ADS)

Hou, Lili; Zhang, Min; Guan, Zhongjie; Li, Qiuye; Yang, Jianjun

2018-01-01

The surface and bulk oxygen vacancy have a prominent effect on the photocatalytic performance of TiO2. In this study, TiO2 possessing different types and concentration of oxygen vacancies were prepared by annealing nanotube titanic acid (NTA) at various temperatures in air or vacuum atmosphere. TiO2 with the unitary bulk single-electron-trapped oxygen vacancies (SETOVs) formed when NTA were calcined in air. Whereas, TiO2 with both bulk and surface oxygen vacancies were obtained when NTA were annealed in vacuum. The series of TiO2 with different oxygen vacancies were systematically characterized by TEM, XRD, PL, XPS, ESR, and TGA. The PL and ESR analysis verified that surface oxygen vacancies and more bulk oxygen vacancies could form in vacuum atmosphere. Surface oxygen vacancies can trap electron and hinder the recombination of photo-generated charges, while bulk SETOVs act as the recombination center. The surface or bulk oxygen vacancies attributed different roles on the photo-absorbance and activity, leading that the sample of NTA-A400 displayed higher hydrogen evolution rate under UV light, whereas NTA-V400 displayed higher hydrogen evolution rate under visible light because bulk SETOVs can improve visible light absorption because sub-band formed by bulk SETOVs prompted the secondary transition of electron excited.

Evaluation of residual uranium contamination in the dirt floor of an abandoned metal rolling mill.

PubMed

Glassford, Eric; Spitz, Henry; Lobaugh, Megan; Spitler, Grant; Succop, Paul; Rice, Carol

2013-02-01

A single, large, bulk sample of uranium-contaminated material from the dirt floor of an abandoned metal rolling mill was separated into different types and sizes of aliquots to simulate samples that would be collected during site remediation. The facility rolled approximately 11,000 tons of hot-forged ingots of uranium metal approximately 60 y ago, and it has not been used since that time. Thirty small mass (≈ 0.7 g) and 15 large mass (≈ 70 g) samples were prepared from the heterogeneously contaminated bulk material to determine how measurements of the uranium contamination vary with sample size. Aliquots of bulk material were also resuspended in an exposure chamber to produce six samples of respirable particles that were obtained using a cascade impactor. Samples of removable surface contamination were collected by wiping 100 cm of the interior surfaces of the exposure chamber with 47-mm-diameter fiber filters. Uranium contamination in each of the samples was measured directly using high-resolution gamma ray spectrometry. As expected, results for isotopic uranium (i.e., U and U) measured with the large-mass and small-mass samples are significantly different (p < 0.001), and the coefficient of variation (COV) for the small-mass samples was greater than for the large-mass samples. The uranium isotopic concentrations measured in the air and on the wipe samples were not significantly different and were also not significantly different (p > 0.05) from results for the large- or small-mass samples. Large-mass samples are more reliable for characterizing heterogeneously distributed radiological contamination than small-mass samples since they exhibit the least variation compared to the mean. Thus, samples should be sufficiently large in mass to insure that the results are truly representative of the heterogeneously distributed uranium contamination present at the facility. Monitoring exposure of workers and the public as a result of uranium contamination resuspended during site remediation should be evaluated using samples of sufficient size and type to accommodate the heterogeneous distribution of uranium in the bulk material.

Study of structural and magnetic properties of melt spun Nd2Fe13.6Zr0.4B ingot and ribbon

NASA Astrophysics Data System (ADS)

Amin, Muhammad; Siddiqi, Saadat A.; Ashfaq, Ahmad; Saleem, Murtaza; Ramay, Shahid M.; Mahmood, Asif; Al-Zaghayer, Yousef S.

2015-12-01

Nd2Fe13.6Zr0.4B hard magnetic material were prepared using arc-melting technique on a water-cooled copper hearth kept under argon gas atmosphere. The prepared samples, Nd2Fe13.6Zr0.4B ingot and ribbon are characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM) for crystal structure determination and morphological studies, respectively. The magnetic properties of the samples have been explored using vibrating sample magnetometer (VSM). The lattice constants slightly increased due to the difference in the ionic radii of Fe and that of Zr. The bulk density decreased due to smaller molar weight and low density of Zr as compared to that of Fe. Ingot sample shows almost single crystalline phase with larger crystallite sizes whereas ribbon sample shows a mixture of amorphous and crystalline phases with smaller crystallite sizes. The crystallinity of the material was highly affected with high thermal treatments. Magnetic measurements show noticeable variation in magnetic behavior with the change in crystallite size. The sample prepared in ingot type shows soft while ribbon shows hard magnetic behavior.

Investigation on charge transfer bands of Ce 4+ in Sr 2CeO 4 blue phosphor

NASA Astrophysics Data System (ADS)

Li, Ling; Zhou, Shihong; Zhang, Siyuan

2008-03-01

Bulk and nano-materials Sr2CeO4 were prepared by solid-state reaction and sol-gel technique, respectively. Photoluminescence shows that luminescence has the characteristic of a ligand-to-metal charge transfer (CT) emission. Compared with bulk Sr2CeO4, the nano-material exhibits stronger emission intensity, longer decay time, and higher CT excitation energy. Three CT excitation peaks were observed in both bulk and nano samples. Based on the theoretical calculations of the average energy gap of the chemical bond using the dielectric theory of complex crystal, the highest and the lowest energy CT bands were assigned to the transitions O1 → Ce4+ and O2 → Ce4+, respectively. The middle bands were due to the superposition of the transitions Ce-O1 and Ce-O2.

An EBIC study of dislocation networks in unprocessed and unprocessed web silicon ribbon. [for solar cells

NASA Technical Reports Server (NTRS)

Fieldler, F. S.; Ast, D.

1982-01-01

Experimental techniques for the preparation of electron beam induced current samples of Web-dentritic silicon are described. Both as grown and processed material were investigated. High density dislocation networks were found close to twin planes in the bulk of the material. The electrical activity of these networks is reduced in processed material.

High-Voltage Poling of a Bulk Sample of Disperse Red 1 Polymethylmethacrylate Guest-Host Polymer for U.S. Army Electro-optical Applications

DTIC Science & Technology

2008-12-01

attached DR1 to a tunable high glass transition temperatue (Tg) polymeric backbone prepared by ROMP. Figure 1. Standard and required poling...approximately 13-15 g of polymer. The remainder of the mixed polymer adhered to screw or barrel. Norbornyl-DR1 monomer (1). 5-norbornene-2- carboxylic acid

Effect of charcoal doping on the superconducting properties of MgB 2 bulk

NASA Astrophysics Data System (ADS)

Kim, N. K.; Tan, K. S.; Jun, B.-H.; Park, H. W.; Joo, J.; Kim, C.-J.

2008-09-01

The effect of charcoal doping on the superconducting properties of in situ processed MgB 2 bulk samples was investigated. To understand the size effect of the dopant the charcoal powder was attrition milled for 1 h, 3 h and 6 h using ZrO 2 balls. The milled charcoal powders were mixed with magnesium and boron powders to a nominal composition of Mg(B 0.975C 0.025) 2. The Mg(B 0.975C 0.025) 2 compacts were heat-treated at 900 °C for 0.5 h in flowing Ar atmosphere. Magnetic susceptibility for the samples showed that the superconducting transition temperature ( Tc) decreased as the size of the charcoal powder decreased. The critical current density ( Jc) of Mg(B 0.975C 0.025) 2 prepared using large size charcoal powder was lower than that of the undoped MgB 2. However, a crossover of Jc value was observed at high magnetic fields of about 4 T in Mg(B 0.975C 0.025) 2 prepared using small size charcoal powder. Carbon diffusion into the boron site was easier and gave the Jc increase effect when the small size charcoal was used as a dopant.

Crystallization kinetics and Avrami index of Sb-doped Se-Te-Sn chalcogenide glasses

NASA Astrophysics Data System (ADS)

Dwivedi, D. K.; Rao, Vandita; Mehta, N.; Chandel, N.

2018-05-01

Bulk amorphous samples of Sb-substituted Se78-xTe20Sn2Sbx (0 < x < 6) have been prepared using melt quench technique. The structure of Se78-xTe20Sn2Sbx (x = 0, 2, 4, 6) glassy alloys has been investigated using X-ray diffraction technique. Calorimetric studies of the prepared samples have been performed under non-isothermal conditions using differential scanning calorimetry (DSC) and glass transition temperature as well as crystallization temperature has been evaluated using DSC scans. The activation energy of crystallization kinetics (Ec) has been determined using model-free approaches such as Kissinger, Ozawa, Tang and Starink methods. The Avrami index (n) and frequency factor (Ko) have been calculated by Matusita and Augis-Benett method.

Fabrication Methods and Luminescent Properties of ZnO Materials for Light-Emitting Diodes

PubMed Central

Lee, Ching-Ting

2010-01-01

Zinc oxide (ZnO) is a potential candidate material for optoelectronic applications, especially for blue to ultraviolet light emitting devices, due to its fundamental advantages, such as direct wide band gap of 3.37 eV, large exciton binding energy of 60 meV, and high optical gain of 320 cm−1 at room temperature. Its luminescent properties have been intensively investigated for samples, in the form of bulk, thin film, or nanostructure, prepared by various methods and doped with different impurities. In this paper, we first review briefly the recent progress in this field. Then a comprehensive summary of the research carried out in our laboratory on ZnO preparation and its luminescent properties, will be presented, in which the involved samples include ZnO films and nanorods prepared with different methods and doped with n-type or p-type impurities. The results of ZnO based LEDs will also be discussed.

Effect of Zn addition on bulk microstructure of lead-free solder SN100C

NASA Astrophysics Data System (ADS)

Nur Nadirah M., K.; Nurulakmal M., S.

2017-12-01

This paper reports the effect of adding Zn (0.5 wt% Zn, 1.0 wt% Zn) to the bulk microstructure and intermetallic compound (IMC) formation of commercial SN100C (Sn-0.7Cu-0.05Ni+Ge) lead-free solder alloy. Solder alloys were prepared by melting SN100C ingot and Zn shots, and subsequently casted into steel mold. Samples were ground and polished for XRF, and polished samples were then etched for microstructure analysis. Microstructure of bulk solder and the IMC were observed using SEM equipped with EDX. SEM result showed the addition of 0.5 wt% Zn resulted in increased grain size of β-Sn matrix but further addition of Zn (1 wt%) reduced the size of β-Sn dendrites in the bulk solder. Several intermetallic compounds (IMCs) were observed distributed in the Sn matrix; Cu-Zn, Ni-Zn and Cu-Zn-Ni IMC but in relatively small percentage compared to Cu-Zn and Ni-Zn. These particles could be considered as effective nucleating agent that led to finer β-Sn grains. It is expected that the finer β-Sn will contribute towards higher solder strength and the various IMCs present could act as suppressant for Sn diffusion which will then tend to reduce the IMC growth during thermal aging.

Impact of Reservoir Fluid Saturation on Seismic Parameters: Endrod Gas Field, Hungary

NASA Astrophysics Data System (ADS)

El Sayed, Abdel Moktader A.; El Sayed, Nahla A.

2017-12-01

Outlining the reservoir fluid types and saturation is the main object of the present research work. 37 core samples were collected from three different gas bearing zones in the Endrod gas field in Hungary. These samples are belonging to the Miocene and the Upper - Lower Pliocene. These samples were prepared and laboratory measurements were conducted. Compression and shear wave velocity were measured using the Sonic Viewer-170-OYO. The sonic velocities were measured at the frequencies of 63 and 33 kHz for compressional and shear wave respectively. All samples were subjected to complete petrophysical investigations. Sonic velocities and mechanical parameters such as young’s modulus, rigidity, and bulk modulus were measured when samples were saturated by 100%-75%-0% brine water. Several plots have been performed to show the relationship between seismic parameters and saturation percentages. Robust relationships were obtained, showing the impact of fluid saturation on seismic parameters. Seismic velocity, Poisson’s ratio, bulk modulus and rigidity prove to be applicable during hydrocarbon exploration or production stages. Relationships among the measured seismic parameters in gas/water fully and partially saturated samples are useful to outline the fluid type and saturation percentage especially in gas/water transitional zones.

Crystal surface integrity and diffusion measurements on Earth and planetary materials

NASA Astrophysics Data System (ADS)

Watson, E. B.; Cherniak, D. J.; Thomas, J. B.; Hanchar, J. M.; Wirth, R.

2016-09-01

Characterization of diffusion behavior in minerals is key to providing quantitative constraints on the ages and thermal histories of Earth and planetary materials. Laboratory experiments are a vital source of the needed diffusion measurements, but these can pose challenges because the length scales of diffusion achievable in a laboratory time are commonly less than 1 μm. An effective strategy for dealing with this challenge is to conduct experiments involving inward diffusion of the element of interest from a surface source, followed by quantification of the resulting diffusive-uptake profile using a high-resolution depth-profiling technique such as Rutherford backscattering spectroscopy (RBS), nuclear reaction analysis (NRA), or ion microprobe (SIMS). The value of data from such experiments is crucially dependent on the assumption that diffusion in the near-surface of the sample is representative of diffusion in the bulk material. Historical arguments suggest that the very process of preparing a polished surface for diffusion studies introduces defects-in the form of dislocations and cracks-in the outermost micrometer of the sample that make this region fundamentally different from the bulk crystal in terms of its diffusion properties. Extensive indirect evidence suggests that, in fact, the near-surface region of carefully prepared samples is no different from the bulk crystal in terms of its diffusion properties. A direct confirmation of this conclusion is nevertheless clearly important. Here we use transmission electron microscopy to confirm that the near-surface regions of olivine, quartz and feldspar crystals prepared using careful polishing protocols contain no features that could plausibly affect diffusion. This finding does not preclude damage to the mineral structure from other techniques used in diffusion studies (e.g., ion implantation), but even in this case the role of possible structural damage can be objectively assessed and controlled. While all evidence points to the reliability of diffusivities obtained from in-diffusion experiments, we do not recommend experiments of this type using a powder source as a means of obtaining diffusant solubility or partitioning information for the mineral of interest.

In situ hydride formation in titanium during focused ion milling.

PubMed

Ding, Rengen; Jones, Ian P

2011-01-01

It is well known that titanium and its alloys are sensitive to electrolytes and thus hydrides are commonly observed in electropolished foils. In this study, focused ion beam (FIB) milling was used to prepare thin foils of titanium and its alloys for transmission electron microscopy. The results show the following: (i) titanium hydrides were observed in pure titanium, (ii) the preparation of a bulk sample in water or acid solution resulted in the formation of more hydrides and (iii) FIB milling aids the precipitation of hydrides, but there were never any hydrides in Ti64 and Ti5553.

Interface Shape and Growth Rate Analysis of Se/GaAs Bulk Crystals Grown in the NASA Crystal Growth Furnace (CGF)

NASA Technical Reports Server (NTRS)

Bly, J. M.; Kaforey, M. L.; Matthiesen, D. H.; Chait, A.

1997-01-01

Selenium-doped gallium arsenide, Se/GaAs, bulk crystals have been grown on earth using NASA's crystal growth furnace (CGF) in preparation for microgravity experimentation on the USML-2 spacelab mission. Peltier cooling pulses of 50 ms duration, 2040 A magnitude, and 0.0033 Hz frequency were used to successfully demark the melt-solid interface at known times during the crystal growth process. Post-growth characterization included interface shape measurement, growth rate calculation, and growth rate transient determinations. It was found that the interface shapes were always slightly concave into the solid. The curvature of the seeding interfaces was typically 1.5 mm for the 15 mm diameter samples. This was in agreement with the predicted interface shapes and positions relative to the furnace determined using a numerical model of the sample/ampoule/cartridge assembly (SACA).

Physical property characterization of Fe-tube encapsulated and vacuum annealed bulk MgB 2

NASA Astrophysics Data System (ADS)

Awana, V. P. S.; Rawat, Rajeev; Gupta, Anurag; Isobe, M.; Singh, K. P.; Vajpayee, Arpita; Kishan, H.; Takayama-Muromachi, E.; Narlikar, A. V.

2006-08-01

We report the phase formation, and present a detailed study of magnetization and resistivity under magnetic field of MgB 2 polycrystalline bulk samples prepared by the Fe-tube encapsulated and vacuum (10 -5 Torr) annealed (750 ∘C) route. Zero-field-cooled magnetic susceptibility (χ) measurements exhibited a sharp transition to the superconducting state with a sizeable diamagnetic signal at 39 K (Tc). The measured magnetization loops of the samples, despite the presence of flux jumps, exhibited a stable current density (Jc) of around 2.4×10 5 A/cm 2 in up to 2 T (Tesla) field and at temperatures (T) up to 10 K. The upper critical field is estimated from resistivity measurements in various fields and shows a typical value of 8 T at 21 K. Further, χ measurements at an applied field of 0.1 T reveal a paramagnetic Meissner effect (PME) that is briefly discussed.

Structure, optical and phonon properties of bulk and nanocrystalline Al2-xScx(WO4)3 solid solutions doped with Cr3+

NASA Astrophysics Data System (ADS)

Mączka, M.; Hermanowicz, K.; Pietraszko, A.; Yordanova, A.; Koseva, I.

2014-01-01

Pure and Cr3+ doped nanosized Al2-xScx(WO4)3 solid solutions were prepared by co-precipitation method as well as Al2-xScx(WO4)3 single crystals were grown by high-temperature flux method. The obtained samples were characterized by X-ray, Raman, IR, absorption and luminescence methods. Single crystal X-ray diffraction showed that AlSc(WO4)3 is orthorhombic at room temperature with space group Pnca and trivalent cations are statistically distributed. Raman and IR studies showed that Al2-xScx(WO4)3 solid solutions show "two mode" behavior. They also showed that vibrational properties of nanosized samples have been weakly modified in comparison with the bulk materials. The luminescence and absorption spectra revealed that chromium ions occupy two sites of weak and strong crystal field strength.

Effect of selenium deficiency on the thermoelectric properties of n -type In 4 Se 3 - x compounds

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhu, G. H.; Lan, Y. C.; Wang, H.

2011-03-01

Thermoelectric properties of dense bulk polycrystalline In 4 Se 3 - x ( x = 0, 0.25, 0.5, 0.65, and 0.8) compounds are investigated. A peak dimensionless thermoelectric figure of merit ( ZT ) of about 1 is achieved for x = 0.65 and 0.8. The peak ZT is about 50% higher than the previously reported highest value for polycrystalline In 4 Se 3 - x compounds. Our In 4 Se 3 - x samples were prepared by ball milling and hot pressing. We show that it is possible to effectively control the electrical conductivity and thermal conductivity by controllingmore » selenium (Se) deficiency x . The ZT enhancement is mainly attributed to the thermal conductivity reduction due to the increased phonon scattering by Se deficiency, defects, and nanoscale inclusions in the ball-milled and hot-pressed dense bulk In 4 Se 3 - x samples.« less

Effect of selenium deficiency on the thermoelectric properties of n-type In 4Se 3-x compounds

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhu, G H; Lan, Y C; Wang, H

2011-03-04

Thermoelectric properties of dense bulk polycrystalline In 4Se 3-x (x = 0, 0.25, 0.5, 0.65, and 0.8) compounds are investigated. A peak dimensionless thermoelectric figure of merit (ZT) of about 1 is achieved for x = 0.65 and 0.8. The peak ZT is about 50% higher than the previously reported highest value for polycrystalline In 4Se 3-x} compounds. Our In 4Se 3-x samples were prepared by ball milling and hot pressing. We show that it is possible to effectively control the electrical conductivity and thermal conductivity by controlling selenium (Se) deficiency x. The ZT enhancement is mainly attributed to themore » thermal conductivity reduction due to the increased phonon scattering by Se deficiency, defects, and nanoscale inclusions in the ball-milled and hot-pressed dense bulk In 4Se 3-x samples.« less

Process parameters, orientation, and functional properties of melt-processed bulk Y-Ba-Cu-O superconductors

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zakharchenko, I.V.; Terryll, K.M.; Rao, K.V.

1995-03-01

This study compared the microstructure, texturing, and functional properties (critical currents) of YBa{sub 2}Cu{sub 3}O{sub 7{minus}x}-based bulk pellets that were prepared by the quench-melt-growth-process (QMGP), melt-textured growth (MTG), and conventional solid-state reaction (SSR) approaches. Using two X-ray diffraction (XRD) methods, {theta}-2{theta}, and rocking curves, the authors found that the individual grains of two melt-processed pellets exhibited remarkable preferred orientational alignment (best rocking curve width = 3.2{degree}). However, the direction of the preferred orientation among the grains was random. Among the three types of bulk materials studied, the QMGP sample was found to have the best J{sub c} values, {approx} 4,500more » A/cm{sup 2} at 77 K in a field of 2 kG, as determined from SQUID magnetic data.« less

Efficient sample preparation method based on solvent-assisted dispersive solid-phase extraction for the trace detection of butachlor in urine and waste water samples.

PubMed

Aladaghlo, Zolfaghar; Fakhari, Alireza; Behbahani, Mohammad

2016-10-01

In this work, an efficient sample preparation method termed solvent-assisted dispersive solid-phase extraction was applied. The used sample preparation method was based on the dispersion of the sorbent (benzophenone) into the aqueous sample to maximize the interaction surface. In this approach, the dispersion of the sorbent at a very low milligram level was achieved by inserting a solution of the sorbent and disperser solvent into the aqueous sample. The cloudy solution created from the dispersion of the sorbent in the bulk aqueous sample. After pre-concentration of the butachlor, the cloudy solution was centrifuged and butachlor in the sediment phase dissolved in ethanol and determined by gas chromatography with flame ionization detection. Under the optimized conditions (solution pH = 7.0, sorbent: benzophenone, 2%, disperser solvent: ethanol, 500 μL, centrifuged at 4000 rpm for 3 min), the method detection limit for butachlor was 2, 3 and 3 μg/L for distilled water, waste water, and urine sample, respectively. Furthermore, the preconcentration factor was 198.8, 175.0, and 174.2 in distilled water, waste water, and urine sample, respectively. Solvent-assisted dispersive solid-phase extraction was successfully used for the trace monitoring of butachlor in urine and waste water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Physical properties of the Nankai inner accretionary prism at Site C0002, IODP Expedition 348

NASA Astrophysics Data System (ADS)

Kitamura, Manami; Kitajima, Hiroko; Henry, Pierre; Valdez, Robert; Josh, Matthew

2014-05-01

Integrated Ocean Drilling Program (IODP) Nankai Trough Seismogenic Zone Experiment (NanTroSEIZE) Expedition 348 focused on deepening the existing riser hole at Site C0002 to ~3000 meters below seafloor (mbsf) to access the deep interior of the Miocene inner accretionary prism. This unique tectonic environment, which has never before been sampled in situ by ocean drilling, was characterized through riser drilling, logging while drilling (LWD), mud gas monitoring and sampling, and cuttings and core analysis. Shipboard physical properties measurements including moisture and density (MAD), electrical conductivity, P-wave, natural gamma ray, and magnetic susceptibility measurements were performed mainly on cuttings samples from 870.5 to 3058.5 mbsf, but also on core samples from 2163 and 2204 mbsf. MAD measurements were conducted on seawater-washed cuttings ("bulk cuttings") in two size fractions of >4 mm and 1-4 mm from 870.5 to 3058.5 mbsf, and hand-picked intact cuttings from the >4 mm size fractions within 1222.5-3058.5 mbsf interval. The bulk cuttings show grain density of 2.68 g/cm3 and 2.72 g/cm3, bulk density of 1.9 g/cm3 to 2.2 g/cm3, and porosity of 50% to 32%. Compared to the values on bulk cuttings, the intact cuttings show almost the same grain density (2.66-2.70 g/cm3), but higher bulk density (2.05-2.41 g/cm3) and lower porosity (37-18%), respectively. The grain density agreement suggests that the measurements on both bulk cuttings and intact cuttings are of good quality, and the differences in porosity and density are real, but the values from the bulk cuttings are affected strongly by artifacts of the drilling process. Thus, the bulk density and porosity data on handpicked cuttings are better representative of formation properties. Combined with the MAD measurements on hand-picked intact cuttings and discrete core samples from previous expeditions, porosity generally decreases from ~60% to ~20% from the seafloor to 3000 mbsf at Site C0002. Electrical conductivity and P-wave velocity on discrete samples, which were prepared from both cuttings and core samples in the depth interval of 1745.5-3058.5 mbsf, range 0.15-0.9 S/m and 1.7-4.5 km/s, respectively. The electrical resistivity (a reciprocal of conductivity) on discrete samples is generally higher than the LWD resistivity data but the overall depth trends are similar. On the other hand, the P-wave velocity on discrete samples is lower than the LWD P-wave velocity between 2200 mbsf and 2600 mbsf, while the P-wave velocity on discrete samples and LWD P-wave velocity are in a closer agreement below 2600 mbsf. The electrical conductivity and P-wave velocity on discrete samples corrected for in-situ pressure and temperature will be presented. The shipboard physical properties measurements on cuttings are very limited but can be useful with careful treatment and observation.

Laser-induced particle size tuning and structural transformations in germanium nanoparticles prepared by stain etching and colloidal synthesis route

DOE Office of Scientific and Technical Information (OSTI.GOV)

Karatutlu, Ali, E-mail: a.karatutlu@qmul.ac.uk, E-mail: ali.karatutlu@bou.edu.tr; Electrical and Electronics Engineering, Bursa Orhangazi University, 16310 Yıldırım/Bursa; Little, William

In this study, with the aid of Raman measurements, we have observed transformations in small (∼3 nm and ∼10 nm) free-standing Ge nanoparticles under laser light exposure. The nanoparticles were obtained by the chemical stain etching of a monocrystalline Ge wafer and of Ge powder and by colloidal synthesis route. We found that the transformation path depends on laser power and exposure time. At relatively low values of the laser power (2 mW) over a period of 100 min, the Raman signal indicates transformation of the sample from a nanocrystaline to bulk-like state, followed by partial oxidation and finally a conversion of themore » entire sample into alpha-quartz type GeO{sub 2}. However, when the laser power is set at 60 mW, we observed a heat release during an explosive crystallization of the nanocrystalline material into bulk Ge without noticeable signs of oxidation. Together with the transmission electron microscopy measurements, these results suggest that the chemical stain etching method for the preparation of porous Ge may not be a top-down process as has been widely considered, but a bottom up one. Systematic studies of the laser exposure on Ge nanoparticles prepared by colloidal synthesis results in the fact that the explosive crystallisation is common for H-terminated and partially disordered Ge nanoparticles regardless of its particle size. We suggest possible bio-medical applications for the observed phenomena.« less

Optically active single-walled carbon nanotubes

NASA Astrophysics Data System (ADS)

Peng, Xiaobin; Komatsu, Naoki; Bhattacharya, Sumanta; Shimawaki, Takanori; Aonuma, Shuji; Kimura, Takahide; Osuka, Atsuhiro

2007-06-01

The optical, electrical and mechanical properties of single-walled carbon nanotubes (SWNTs) are largely determined by their structures, and bulk availability of uniform materials is vital for extending their technological applications. Since they were first prepared, much effort has been directed toward selective synthesis and separation of SWNTs with specific structures. As-prepared samples of chiral SWNTs contain equal amounts of left- and right-handed helical structures, but little attention has been paid to the separation of these non-superimposable mirror image forms, known as optical isomers. Here, we show that optically active SWNT samples can be obtained by preferentially extracting either right- or left-handed SWNTs from a commercial sample. Chiral `gable-type' diporphyrin molecules bind with different affinities to the left- and right-handed helical nanotube isomers to form complexes with unequal stabilities that can be readily separated. Significantly, the diporphyrins can be liberated from the complexes afterwards, to provide optically enriched SWNTs.

Results From The Salt Disposition Project Next Generation Solvent Demonstration Plan

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peters, T. B.; Fondeur, F. F.; Taylor-Pashow, K. M.L.

2014-04-02

Strip Effluent Hold Tank (SEHT), Decontaminated Salt Solution Hold Tank (DSSHT), Caustic Wash Tank (CWT) and Solvent Hold Tank (SHT) samples were taken throughout the Next Generation Solvent (NGS) Demonstration Plan. These samples were analyzed and the results are reported. SHT: The solvent behaved as expected, with no bulk changes in the composition over time, with the exception of the TOA and TiDG. The TiDG depletion is higher than expected, and consideration must be taken on the required rate of replenishment. Monthly sampling of the SHT is warranted. If possible, additional SHT samples for TiDG analysis (only) would help SRNLmore » refine the TiDG degradation model. CWT: The CWT samples show the expected behavior in terms of bulk chemistry. The 137Cs deposited into the CWT varies somewhat, but generally appears to be lower than during operations with the BOBCalix solvent. While a few minor organic components were noted to be present in the Preliminary sample, at this time these are thought to be artifacts of the sample preparation or may be due to the preceding solvent superwash. DSSHT: The DSSHT samples show the predicted bulk chemistry, although they point towards significant dilution at the front end of the Demonstration. The 137Cs levels in the DSSHT are much lower than during the BOBCalix operations, which is the expected observation. SEHT: The SEHT samples represent the most different output of all four of the outputs from MCU. While the bulk chemistry is as expected, something is causing the pH of the SEHT to be higher than what would be predicted from a pure stream of 0.01 M boric acid. There are several possible different reasons for this, and SRNL is in the process of investigating. Other than the pH issue, the SEHT is as predicted. In summary, the NGS Demonstration Plan samples indicate that the MCU system, with the Blend Solvent, is operating as expected. The only issue of concern regards the pH of the SEHT, and SRNL is in the process of investigating this. SRNL results support the transition to routine operations.« less

Comparison of Grab, Air, and Surface Results for Radiation Site Characterization

NASA Astrophysics Data System (ADS)

Glassford, Eric Keith

2011-12-01

The use of proper sampling methods and sample types for evaluating sites believed to be contaminated with radioactive materials is necessary to avoid misrepresenting conditions at the site. This study was designed to investigate if the site characterization, based upon uranium contamination measured in different types of samples, is dependent upon the mass of the sample collected. A bulk sample of potentially contaminated interior dirt was collected from an abandoned metal processing mill that rolled uranium between 1948 and 1956. The original mill dates from 1910 and has a dirt floor. The bulk sample was a mixture of dirt, black and yellow particles of metal dust, and small fragments of natural debris. Small mass (approximately 0.75 grams (g)) and large mass (approximately 70g) grab samples were prepared from the bulk sample material to simulate collection of a "grab" type sample. Air sampling was performed by re-suspending a portion of the bulk sample material using a vibration table to simulate airborne contamination that might be present during site remediation. Additionally, samples of removable contaminated surface dust were collected on 47 mm diameter filter paper by wiping the surfaces of the exposure chamber used to resuspend the bulk material. Certified reference materials, one containing a precisely known quantity of U 3O8 and one containing a known quantity of natural uranium, were utilized to calibrate the gamma spectrometry measurement system. Non-destructive gamma spectrometry measurements were used to determine the content of uranium-235 (235U) at 185 keV and 143 keV, thorium-234 (234Th) at 63 keV, and protactinium-234m (234mPa) at 1001 keV in each sample. Measurement of natural uranium in small, 1 g samples is usually accomplished by radiochemical analysis in order to measure alpha particles emitted by 238U, 235U, and 234U. However, uranium in larger bulk samples can also be measured non-destructively using gamma spectrometry to detect the low energy photons from 234Th and 234mPa, the short-lived decay products of 238U, and 235U. Two sided t-tests and coefficient of variation were used to compare sampling types. The large grab samples had the lowest calculated coefficient of variation results for activity and atom percentage. The wipe samples had the highest calculated coefficient of variation of mean specific activity (dis/sec/g) for all three energies. The air filter samples had the highest coefficient of variation calculation for mean atom percentage, for both uranium isotopes examined. The data indicated that the large mass sample was the most effective at characterizing the rolling mill radioactive site conditions, since this would indicate which samples had the smallest variations compared to the mean. Additionally, measurement results of natural uranium in the samples indicate that the distribution of radioactive contamination at the sampling location is most likely non-homogeneous and that the size of the sample collected and analyzed must be sufficiently large to insure that the analytical results are truly representative of the activity present.

Evaluation of dredged material proposed for ocean disposal from Hudson River, New York

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gardiner, W.W.; Barrows, E.S.; Antrim, L.D.

1996-09-01

The Hudson River (Federal Project No. 41) was one of seven waterways that the U.S. Army Corps of Engineers-New York District (USACE-NYD) requested the Battelle Marine Sciences Laboratory (MSL) to sample and evaluate for dredging and disposal in March 1994. Sediment samples were collected from the Hudson River. Tests and analyses were conducted on Hudson River sediment core samples. The evaluation of proposed dredged material from the Hudson River included bulk sediment chemical analyses, chemical analyses of site water and elutriate, water-column and benthic acute toxicity tests, and bioaccumulation studies. Individual sediment core samples collected from Hudson River were analyzedmore » for grain size, moisture content, and total organic carbon (TOC). A composite sediment sample, representing the entire area proposed for dredging, was analyzed for bulk density, specific gravity, metals, chlorinated pesticides, polychlorinated biphenyl (PCB) congeners, polynuclear aromatic hydrocarbons (PAH), and 1,4-dichlorobenzene. Site water and elutriate water, prepared from the suspended-particulate phase (SPP) of Hudson River sediment, were analyzed for metals, pesticides, and PCBS. Water-column or SPP toxicity tests were performed with three species. Benthic acute toxicity tests were performed. Bioaccumulation tests were also conducted.« less

Thermal Stress Effect on Density Changes of Hemp Hurds Composites

NASA Astrophysics Data System (ADS)

Schwarzova, Ivana; Cigasova, Julia; Stevulova, Nadezda

2016-12-01

The aim of this article is to study the behavior of prepared biocomposites based on hemp hurds as a filling agent in composite system. In addition to the filler and water, an alternative binder, called MgO-cement was used. For this objective were prepared three types of samples; samples based on untreated hemp hurds as a referential material and samples based on chemically (with NaOH solution) and physically (by ultrasonic procedure) treated hemp hurds. The thermal stress effect on bulk density changes of hemp hurds composites was monitored. Gradual increase in temperature led to composites density reduction of 30-40 %. This process is connected with mass loss of the adsorbed moisture and physically bound water and also with degradation of organic compounds present in hemp hurds aggregates such as pectin, hemicelluloses and cellulose. Therefore the changes in the chemical composition of treated hemp hurds in comparison to original sample and its thermal decomposition were also studied.

Buried oxide and defects in oxygen implanted Si monitored by positron annihilation

NASA Astrophysics Data System (ADS)

Kruseman, A. C.; van Veen, A.; Schut, H.; Mijnarends, P. E.; Fujinami, M.

2001-08-01

One- and two-detector Doppler broadening measurements performed on low (˜1014 to 1015O+/cm2) and high dose (˜1017 to 1018O+/cm2) oxygen-irradiated Si using variable-energy slow positrons are analyzed in terms of S and W parameters. After annealing the low-dose samples at 800 °C, large VxOy complexes are formed at depths around 400 nm. These complexes produce a clear-cut signature when the ratio of S to that of defect-free bulk Si is plotted. Similar behavior is found for samples irradiated with 2 and 4×1017O+/cm2 and annealed at 1000 °C. After irradiation with 1.7×1018O+/cm2 and anneal at 1350 °C a 170 nm thick almost-bulk-quality Si surface layer is formed on top of a 430 nm thick buried oxide layer. This method of preparation is called separation by implantation of oxygen. S-W measurements show that the surface layer contains electrically inactive VxOy complexes not seen by electron microscopy. A method is presented to decompose the Doppler broadening line shape into contributions of the bulk, surface, and defect.

SOLID-STATE SYNTHESIS AND SOME PROPERTIES OF MAGNESIUM-DOPED COPPER ALUMINUM OXIDES

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Chang; Ren, Fei; Wang, Hsin

2010-01-01

Copper aluminum oxide (CuAlO2) with delafossite structure is a promising candidate for high temperature thermoelectric applications because of its modest band gap, high stability and low cost. We investigate magnesium doping on the aluminum site as a means of producing higher electrical conductivity and optimized Seebeck coefficient. Powder samples were synthesized using solid-state reaction and bulk samples were prepared using both cold-pressing and hot-pressing techniques. Composition analysis, microstructural examination and transport property measurements were performed, and the results suggest that while hot-pressing can achieve high density samples, secondary phases tend to form and lower the performance of the materials.

Bulk Al-Al3Zr composite prepared by mechanical alloying and hot extrusion for high-temperature applications

NASA Astrophysics Data System (ADS)

Pourkhorshid, E.; Enayati, M. H.; Sabooni, S.; Karimzadeh, F.; Paydar, M. H.

2017-08-01

Bulk Al/Al3Zr composite was prepared by a combination of mechanical alloying (MA) and hot extrusion processes. Elemental Al and Zr powders were milled for up to 10 h and heat treated at 600°C for 1 h to form stable Al3Zr. The prepared Al3Zr powder was then mixed with the pure Al powder to produce an Al-Al3Zr composite. The composite powder was finally consolidated by hot extrusion at 550°C. The mechanical properties of consolidated samples were evaluated by hardness and tension tests at room and elevated temperatures. The results show that annealing of the 10-h-milled powder at 600°C for 1 h led to the formation of a stable Al3Zr phase. Differential scanning calorimetry (DSC) results confirmed that the formation of Al3Zr began with the nucleation of a metastable phase, which subsequently transformed to the stable tetragonal Al3Zr structure. The tension yield strength of the Al-10wt%Al3Zr composite was determined to be 103 MPa, which is approximately twice that for pure Al (53 MPa). The yield stress of the Al/Al3Zr composite at 300°C is just 10% lower than that at room temperature, which demonstrates the strong potential for the prepared composite to be used in high-temperature structural applications.

Studies of doped LaMnO3 samples prepared by citrate combustion process

NASA Astrophysics Data System (ADS)

Dimri, M. Chandra; Khanduri, H.; Mere, A.; Stern, R.

2018-04-01

La0.95A0.05MnO3 (where A=Na, Sr, Er, Dy and Ce) powder samples were synthesized by chemical solution route and the magnetic and structural properties are reported in this paper. The pervoskite structure was confirmed from X-ray diffraction patterns and Raman spectra at room temperature in all of these doped samples. Curie transition temperatures in doped LaMnO3 bulk samples were around 250K, which are much higher than the ideal value (˜140 K) in undoped samples. The increase in the magnetic transition temperatures can be related to non-stoichiometry and cation vacancies created due to higher valence substitutions for the univalent La1+ ions.

Silver-modified mobile phase for normal-phase liquid chromatographic determination of prostaglandins and their 5,6-trans isomers in prostaglandin bulk drugs and triacetin solutions.

PubMed

Kissinger, L D; Robins, R H

1985-03-15

A silver-modified, normal-phase, high-performance liquid chromatographic system has been developed for prostaglanding bulk drugs and triacetin solutions. Silver nitrate present in the mobile phase results in high selectivity for cis/trans isomers with conventional silica columns. Prostaglandins were esterified with alpha-bromo-2'-acetonaphthone prior to chromatography to provide high detectability at 254 nm. For dilute triacetin solutions, a sample preparation scheme based on gravity-flow chromatography with silica columns was developed to isolate the prostaglandin from triacetin prior to derivatization. The analytical technique was applied to triacetin solutions containing as little as 10 micrograms/ml arbaprostil [15-(R)-methyl-PGE2].

Bubble template synthesis of Sn2Nb2O7 hollow spheres for enhanced visible-light-driven photocatalytic hydrogen production.

PubMed

Zhou, Chao; Zhao, Yufei; Bian, Tong; Shang, Lu; Yu, Huijun; Wu, Li-Zhu; Tung, Chen-Ho; Zhang, Tierui

2013-10-28

Hierarchical Sn2Nb2O7 hollow spheres were prepared for the first time via a facile hydrothermal route using bubbles generated in situ from the decomposition of urea as soft templates. The as-obtained hollow spheres with a large specific surface area of 58.3 m(2) g(-1) show improved visible-light-driven photocatalytic H2 production activity in lactic acid aqueous solutions, about 4 times higher than that of the bulk Sn2Nb2O7 sample prepared by a conventional high temperature solid state reaction method.

Rotary bulk solids divider

DOEpatents

Maronde, Carl P.; Killmeyer, Jr., Richard P.

1992-01-01

An apparatus for the disbursement of a bulk solid sample comprising, a gravity hopper having a top open end and a bottom discharge end, a feeder positioned beneath the gravity hopper so as to receive a bulk solid sample flowing from the bottom discharge end, and a conveyor receiving the bulk solid sample from the feeder and rotating on an axis that allows the bulk solid sample to disperse the sample to a collection station.

ROTARY BULK SOLIDS DIVIDER

DOEpatents

Maronde, Carl P.; Killmeyer JR., Richard P.

1992-03-03

An apparatus for the disbursement of a bulk solid sample comprising, a gravity hopper having a top open end and a bottom discharge end, a feeder positioned beneath the gravity hopper so as to receive a bulk solid sample flowing from the bottom discharge end, and a conveyor receiving the bulk solid sample from the feeder and rotating on an axis that allows the bulk solid sample to disperse the sample to a collection station.

Chemical composition separation of a propylene-ethylene random copolymer by high temperature solvent gradient interaction chromatography.

PubMed

Liu, Yonggang; Phiri, Mohau Justice; Ndiripo, Anthony; Pasch, Harald

2017-11-03

A propylene-ethylene random copolymer was fractionated by preparative temperature rising elution fractionation (TREF). The structural heterogeneity of the bulk sample and its TREF fractions was studied by high temperature liquid chromatography with a solvent gradient elution from 1-decanol to 1,2,4-trichlorobenzene. HPLC alone cannot resolve those propylene-ethylene copolymers with high ethylene content in the bulk sample, due to their low weight fractions in the bulk sample and a small response factor of these components in the ELSD detector, as well as their broad chemical composition distribution. These components can only be detected after being separated and enriched by TREF followed by HPLC analysis. Chemical composition separations were achieved for TREF fractions with average ethylene contents between 2.1 and 22.0mol%, showing that copolymers with higher ethylene contents were adsorbed stronger in the Hypercarb column and eluted later. All TREF fractions, except the 40°C fraction, were relatively homogeneous in both molar mass and chemical composition. The 40°C fraction was rather broad in both molar mass and chemical composition distributions. 2D HPLC showed that the molar masses of the components containing more ethylene units were getting lower for the 40°C fraction. HPLC revealed and confirmed that co-crystallization influences the separation in TREF of the studied propylene-ethylene copolymer. Copyright © 2017 Elsevier B.V. All rights reserved.

Raman study of supported molybdenum disulfide single layers

NASA Astrophysics Data System (ADS)

Durrer, William; Manciu, Felicia; Afanasiev, Pavel; Berhault, Gilles; Chianelli, Russell

2008-10-01

Owing to the increasing demand for clean transportation fuels, highly dispersed single layer transition metal sulfides such as MoS2-based catalysts play an important role in catalytic processes for upgrading and removing sulfur from heavy petroleum feed. In its crystalline bulk form, MoS2 is chemically rather inactive due to a strong tendency to form highly stacked layers, but, when dispersed as single-layer nanoclusters on a support, the MoS2 becomes catalytically active in the hydrogenolysis of sulphur and nitrogen from organic compounds (hydrotreating catalysis). In the present studies alumina-supported MoS2 samples were analyzed by confocal Raman spectroscopy. Evidence of peaks at 152 cm-1, 234 cm-1, and 336 cm-1, normally not seen in the Raman spectrum of the standard bulk crystal, confirms the formation of single layers of MoS2. Furthermore, the presence of the 383 cm-1 Raman line suggests the trigonal prismatic coordination of the formed MoS2 single layers. Depending on the sample preparation method, a restacking of MoS2 layers is also observed, mainly for ex-thiomolybdate samples sulfided at 550 C.

Mechanical and thermal properties of bulk ZrB2

NASA Astrophysics Data System (ADS)

Nakamori, Fumihiro; Ohishi, Yuji; Muta, Hiroaki; Kurosaki, Ken; Fukumoto, Ken-ichi; Yamanaka, Shinsuke

2015-12-01

ZrB2 appears to have formed in the fuel debris at the Fukushima Daiichi nuclear disaster site, through the reaction between Zircaloy cladding materials and the control rod material B4C. Since ZrB2 has a high melting point of 3518 K, the ceramic has been widely studied as a heat-resistant material. Although various studies on the thermochemical and thermophysical properties have been performed for ZrB2, significant differences exist in the data, possibly due to impurities or the porosity within the studied samples. In the present study, we have prepared a ZrB2 bulk sample with 93.1% theoretical density by sintering ZrB2 powder. On this sample, we have comprehensively examined the thermal and mechanical properties of ZrB2 by the measurement of specific heat, ultrasonic sound velocities, thermal diffusivity, and thermal expansion. Vickers hardness and fracture toughness were also measured and found to be 13-23 GPa and 1.8-2.8 MPa m0.5, respectively. The relationships between these properties were carefully examined in the present study.

Properties of the exotic metastable ST12 germanium allotrope

PubMed Central

Zhao, Zhisheng; Zhang, Haidong; Kim, Duck Young; Hu, Wentao; Bullock, Emma S.; Strobel, Timothy A.

2017-01-01

The optical and electronic properties of semiconducting materials are of great importance to a vast range of contemporary technologies. Diamond-cubic germanium is a well-known semiconductor, although other ‘exotic' forms may possess distinct properties. In particular, there is currently no consensus for the band gap and electronic structure of ST12-Ge (tP12, P43212) due to experimental limitations in sample preparation and varying theoretical predictions. Here we report clear experimental and theoretical evidence for the intrinsic properties of ST12-Ge, including the first optical measurements on bulk samples. Phase-pure bulk samples of ST12-Ge were synthesized, and the structure and purity were verified using powder X-ray diffraction, transmission electron microscopy, Raman and wavelength/energy dispersive X-ray spectroscopy. Optical measurements indicate that ST12-Ge is a semiconductor with an indirect band gap of 0.59 eV and a direct optical transition at 0.74 eV, which is in good agreement with electrical transport measurements and our first-principles calculations. PMID:28045027

Properties of the exotic metastable ST12 germanium allotrope

DOE PAGES

Zhao, Zhisheng; Zhang, Haidong; Kim, Duck Young; ...

2017-01-03

The optical and electronic properties of semiconducting materials are of great importance to a vast range of contemporary technologies. Diamond-cubic germanium is a well-known semiconductor, although other ‘exotic’ forms may possess distinct properties. In particular, there is currently no consensus for the band gap and electronic structure of ST12-Ge (tP12, P4 32 12) due to experimental limitations in sample preparation and varying theoretical predictions. Here we report clear experimental and theoretical evidence for the intrinsic properties of ST12-Ge, including the first optical measurements on bulk samples. Phase-pure bulk samples of ST12-Ge were synthesized, and the structure and purity were verifiedmore » using powder X-ray diffraction, transmission electron microscopy, Raman and wavelength/energy dispersive X-ray spectroscopy. Lastly, optical measurements indicate that ST12-Ge is a semiconductor with an indirect band gap of 0.59 eV and a direct optical transition at 0.74 eV, which is in good agreement with electrical transport measurements and our first-principles calculations.« less

Quantitative comparison of organic photovoltaic bulk heterojunction photostability under laser illumination

DOE PAGES

Lesoine, Michael D.; Bobbitt, Jonathan M.; Carr, John A.; ...

2014-11-20

The photostability of bulk heterojunction organic photovoltaic films containing a polymer donor and a fullerene-derivative acceptor was examined using resonance Raman spectroscopy and controlled laser power densities. The polymer donors were poly(3-hexylthiophene-2,5-diyl) (P3HT), poly[[9-(1-octylnonyl)-9H-carbazole-2,7-diyl]-2,5-thiophenediyl-2,1,3-benzothiadiazole-4,7-diyl-2,5-thiophenediyl] (PCDTBT), or poly({4,8-bis[(2-ethylhexyl)oxy]benzo[1,2-b:4,5-b']dithiophene-2,6-diyl}{3-fluoro-2-[(2-ethylhexyl)carbonyl]thieno[3,4-b]thiophenediyl}) (PTB7). Four sample preparation methods were studied: (i) thin or (ii) thick films with fast solvent evaporation under nitrogen, (iii) thick films with slow solvent evaporation under nitrogen, and (iv) thin films dried under nitrogen followed by thermal annealing. Polymer order was assessed by monitoring a Raman peak’s full width at half-maximum and location as a function of illumination time and laser powermore » densities from 2.5 × 10 3 to 2.5 × 10 5 W cm –2. Resonance Raman spectroscopy measurements show that before prolonged illumination, PCDTBT and PTB7 have the same initial order for all preparation conditions, while P3HT order improves with slow solvent drying or thermal annealing. All films exhibited changes to bulk heterojunction structure with 2.5 × 10 5 Wcm –2 laser illumination as measured by resonance Raman spectroscopy, and atomic force microscopy images show evidence of sample heating that affects the polymer over an area greater than the illumination profile. Furthermore, photostability data are important for proper characterization by techniques involving illumination and the development of devices suitable for real-world applications.« less

Effect of gamma irradiation on physicochemical properties of stored pigeon pea (Cajanus cajan) flour

PubMed Central

Bamidele, Oluwaseun P; Akanbi, Charles T

2013-01-01

The effect of gamma irradiation at various doses (5, 10, 15, 20 kGy) was observed on pigeon pea flour stored for 3 months on proximate composition, functional properties, and peroxide value. Sensory evaluation was also carried out on bean cake (moinmoin) made from nonirradiated and irradiated pigeon pea flour. The results showed that stored gamma-irradiated samples had significantly lower (P < 0.05) value of protein and little or no effect on moisture content. There were slight decreases in crude fiber and ash content of the irradiated samples compared with the control sample. The result of functional properties of the irradiated flours showed slight increase in water absorption capacity, swelling capacity and bulk density. The peroxide value of crude oil increased significantly with dose increases for the period of storage. The sensory evaluation of moinmoin samples prepared from irradiated pigeon pea flour showed no significant difference from the moinmoin sample prepared from nonirradiated flour. It can be concluded that gamma irradiation can extend the shelf life of pigeon pea flour. PMID:24804044

Effect of gamma irradiation on physicochemical properties of stored pigeon pea (Cajanus cajan) flour.

PubMed

Bamidele, Oluwaseun P; Akanbi, Charles T

2013-09-01

The effect of gamma irradiation at various doses (5, 10, 15, 20 kGy) was observed on pigeon pea flour stored for 3 months on proximate composition, functional properties, and peroxide value. Sensory evaluation was also carried out on bean cake (moinmoin) made from nonirradiated and irradiated pigeon pea flour. The results showed that stored gamma-irradiated samples had significantly lower (P < 0.05) value of protein and little or no effect on moisture content. There were slight decreases in crude fiber and ash content of the irradiated samples compared with the control sample. The result of functional properties of the irradiated flours showed slight increase in water absorption capacity, swelling capacity and bulk density. The peroxide value of crude oil increased significantly with dose increases for the period of storage. The sensory evaluation of moinmoin samples prepared from irradiated pigeon pea flour showed no significant difference from the moinmoin sample prepared from nonirradiated flour. It can be concluded that gamma irradiation can extend the shelf life of pigeon pea flour.

The relationship between Vickers microhardness and compressive strength of functional surface geopolymers

NASA Astrophysics Data System (ADS)

Subaer, Ekaputri, Januari Jaya; Fansuri, Hamzah; Abdullah, Mustafa Al Bakri

2017-09-01

An experimental study to investigate the relationship between Vickers microhardness and compressive strength of geopolymers made from metakaolin has been conducted. Samples were prepared by using metakaolin activated with a sodium silicate solution at a different ratio of Si to Al and Na to Al and cured at 70°C for one hour. The resulting geopolymers were stored in an open air for 28 days before conducting any measurement. Bulk density and apparent porosity of the samples were measured by using Archimedes's method. Vickers microhardness measurements were performed on a polished surface of geopolymers with a load ranging from 0.3 - 1.0 kg. The topographic of indented samples were examined by using scanning electron microscopy (SEM). Compressive strength of the resulting geopolymers was measured on the cylindrical samples with a ratio of height to the diameter was 2:1. The results showed that the molar ratios of geopolymers compositions play important roles in the magnitude of bulk density, porosity, Vickers's microhardness as well as the compressive strength. The porosity reduced exponentially the magnitude of the strength of geopolymers. It was found that the relationship between Vickers microhardness and compressive strength was linear.

The influence of surface roughness and high pressure torsion on the growth of anodic titania nanotubes on pure titanium

NASA Astrophysics Data System (ADS)

Hu, Nan; Gao, Nong; Starink, Marco J.

2016-11-01

Anodic titanium dioxide nanotube (TNT) arrays have wide applications in photocatalytic, catalysis, electronics, solar cells and biomedical implants. When TNT coatings are combined with severe plastic deformation (SPD), metal processing techniques which efficiently improve the strength of metals, a new generation of biomedical implant is made possible with both improved bulk and surface properties. This work investigated the effect of processing by high pressure torsion (HPT) and different mechanical preparations on the substrate and subsequently on the morphology of TNT layers. HPT processing was applied to refine the grain size of commercially pure titanium samples and substantially improved their strength and hardness. Subsequent anodization at 30 V in 0.25 wt.% NH4F for 2 h to form TNT layers on sample surfaces prepared with different mechanical preparation methods was carried out. It appeared that the local roughness of the titanium surface on a microscopic level affected the TNT morphology more than the macroscopic surface roughness. For HPT-processed sample, the substrate has to be pre-treated by a mechanical preparation finer than 4000 grit for HPT to have a significant influence on TNTs. During the formation of TNT layers the oxide dissolution rate was increased for the ultrafine-grained microstructure formed due to HPT processing.

Enhanced photovoltaic performance of dye sensitized solar cell using SnO2 nanoflowers

NASA Astrophysics Data System (ADS)

Arote, Sandeep A.; Tabhane, Vilas A.; Pathan, Habib M.

2018-01-01

The study highlighted enhanced performance of SnO2 based DSSC using photoanode with nanostructured morphology. The simple organic surfactant free hydrothermal synthesis method was used for preparation of SnO2 nanoflowers for dye sensitized solar cell (DSSC) application. The hydrothermal reaction time was varied to obtain different SnO2 nanostructures. The hydrothermal reaction time showed considerable effect on optical and structural properties of the prepared samples. The results indicated that the prepared samples were pure rutile SnO2. The band gap of prepared samples was greater than bulk SnO2 and varied from 3.64 to 3.81 eV with increase in hydrothermal reaction time. With increase in reaction time from 4 to 24 h, the microstructure of SnO2 changed from agglomerated nanoparticles to nanopetals and finally to self-assembled nanoflowers. Flower-like SnO2 nanostructures showed size around 300-700 nm, and composed of large numbers of 3 dimensional petals connected with each other forming 3D nanoflowers by self-assembly. Consequently, the DSSC with flower-like SnO2 nanostructures exhibited good photovoltaic performance with Voc, Jsc and η about 0.43 V, 4.36 mA/cm2 and 1.11%, respectively.

Sample preparation of metal alloys by electric discharge machining

NASA Technical Reports Server (NTRS)

Chapman, G. B., II; Gordon, W. A.

1976-01-01

Electric discharge machining was investigated as a noncontaminating method of comminuting alloys for subsequent chemical analysis. Particulate dispersions in water were produced from bulk alloys at a rate of about 5 mg/min by using a commercially available machining instrument. The utility of this approach was demonstrated by results obtained when acidified dispersions were substituted for true acid solutions in an established spectrochemical method. The analysis results were not significantly different for the two sample forms. Particle size measurements and preliminary results from other spectrochemical methods which require direct aspiration of liquid into flame or plasma sources are reported.

Molecular precursor routes to transition metal sulfides

NASA Astrophysics Data System (ADS)

Dinnage, Christopher Walker

This thesis is primarily concerned with the synthesis of homoleptic early transition meta thiolates and the subsequent preparation of bulk and thin-film metal disulfides from these compounds. Chapter 1 gives an introduction into the properties, preparation procedures and uses of bulk and thin-film transition metal disulfides as well as giving an overview of early transition metal thiolates synthesied so far in the literature (for titanium, zirconium, tantalum and niobium). Chapter 2 is concerned with the synthesis of a number of ionic and neutral transition metal thiolates. The main synthetic methodologies discussed in this chapter include substitution reactions of transition metal amides and alkyls with thiols, salt metathesis reactions of transition metal chlorides with alkali metal thiolates or with a base / thiol and the use of Grignard reagents. Chapter 3 discusses the preparation of bulk transition metal disulfides using the thiolates prepared in the previous chapter via a thio "sol-gel" route. The preparation of a range of bulk metal and mixed-metal disulfides using transition metal chlorides and hexamethyldisilathiane is also discussed in this chapter. Finally, chapter 4 is concerned with the attempted preparation of thin-films of some transition metal disulfides. Decomposition studies of some of the thiolates prepared in chapter 2 are discussed using thermal gravimetric analysis. Vapour-phase deposition studies are also explored in order to test the potential of the transition metal thiolates as precursors to the disulfides. Experiments using low-pressure chemical vapour deposition and aerosol-assisted chemical vapour deposition are also described.

Bismuth molybdate thick films as ethanol sensor

NASA Astrophysics Data System (ADS)

Jain, Kiran; Kumar, Vipin; Gupta, H. P.; Rastogi, A. C.

2003-10-01

Ethanol sensitivity of bismuth molybdate thick films and sintered pellets were investigated. Sintered pellets were prepared by traditional ceramic processing. Thick films were prepared by metallorganic decomposition process. Ethanol gas sensitivity was measured at various temperatures and concentrations. Thick films of alpha phase bismuth molybdate prepared by spray pyrolysis showed a very fast response to ethanol detection. The response time for the bulk samples is about 40 sec which decreased to about 6 sec for thick films at an operating temperature of 300°C. An extremely low level approximately 10 ppm detection and fast response makes this technique ideal for sensor element fabrication for detection and estimation of alcohol in breath-analyzer. Unlike SnO2, the resistance of these sensors is not affected by humidity at the operating temperature.

Preparation of bulk superhard B-C-N nanocomposite compact

DOEpatents

Zhao, Yusheng [Los Alamos, NM; He, Duanwei [Sichuan, CN

2011-05-10

Bulk, superhard, B--C--N nanocomposite compacts were prepared by ball milling a mixture of graphite and hexagonal boron nitride, encapsulating the ball-milled mixture at a pressure in a range of from about 15 GPa to about 25 GPa, and sintering the pressurized encapsulated ball-milled mixture at a temperature in a range of from about 1800-2500 K. The product bulk, superhard, nanocomposite compacts were well sintered compacts with nanocrystalline grains of at least one high-pressure phase of B--C--N surrounded by amorphous diamond-like carbon grain boundaries. The bulk compacts had a measured Vicker's hardness in a range of from about 41 GPa to about 68 GPa.

Attrition resistant bulk iron catalysts and processes for preparing and using same

DOEpatents

Jothimurugesan, Kandaswamy [Ponca City, OK; Goodwin, Jr., James G.; Gangwal, Santosh K [Cary, NC

2007-08-21

An attrition resistant precipitated bulk iron catalyst is prepared from iron oxide precursor and a binder by spray drying. The catalysts are preferably used in carbon monoxide hydrogenation processes such as Fischer-Tropsch synthesis. These catalysts are suitable for use in fluidized-bed reactors, transport reactors and, especially, slurry bubble column reactors.

Susceptibility of volcanic ash-influenced soil in northern Idaho to mechanical compaction

Treesearch

Deborah S. Page-Dumroese

1993-01-01

Timber harvesting and mechanical site preparation can reduce site productivity if they excessively disturb or compact the soil. Volcanic ash-influenced soils with low undisturbed bulk densities and rock content are particularly susceptible. This study evaluates the effects of harvesting and site preparation on changes in the bulk density of ash-influenced forest soils...

Large magnetoresistance and Hall effect in paramagnetic black phosphorus synthesized from red phosphorus

NASA Astrophysics Data System (ADS)

Jiang, X. H.; Xiong, F.; Zhang, X. W.; Hua, Z. H.; Wang, Z. H.; Yang, S. G.

2018-05-01

Black phosphorus (BP) is an important material, which can be used in the fabrication of phosphorene. In this manuscript, a systematic study was described on the high-pressure synthesis of BP from red phosphorus. For physical characterization, the bulk BP was synthesized under the high pressure of 1.6 GPa and high temperature of 700 °C for 2 h. X-ray diffraction and Raman studies illustrated the formation of high-quality pure phase pleomorphic BP. A nonlinear Hall effect was observed in the BP sample. Magnetoresistance (MR) in the bulk BP reached 90% at 40 K, and positive-to-negative crossover in MR was measured. A paramagnetic feature was found in the prepared bulk BP, and the MR results were attributed to the combination of the effect of classical resistor network and magnetic polaron. The conduction tensors were analyzed by a two-band model to determine the carrier concentration and mobility at several temperatures.

Effect of sintering temperature on the microstructure and properties of foamed glass-ceramics prepared from high-titanium blast furnace slag and waste glass

NASA Astrophysics Data System (ADS)

Chen, Chang-hong; Feng, Ke-qin; Zhou, Yu; Zhou, Hong-ling

2017-08-01

Foamed glass-ceramics were prepared via a single-step sintering method using high-titanium blast furnace slag and waste glass as the main raw materials The influence of sintering temperature (900-1060°C) on the microstructure and properties of foamed glass-ceramics was studied. The results show that the crystal shape changed from grainy to rod-shaped and finally turned to multiple shapes as the sintering temperature was increased from 900 to 1060°C. With increasing sintering temperature, the average pore size of the foamed glass-ceramics increased and subsequently decreased. By contrast, the compressive strength and the bulk density decreased and subsequently increased. An excessively high temperature, however, induced the coalescence of pores and decreased the compressive strength. The optimal properties, including the highest compressive strength (16.64 MPa) among the investigated samples and a relatively low bulk density (0.83 g/cm3), were attained in the case of the foamed glass-ceramics sintered at 1000°C.

Study of GaAs-oxide interface by transient capacitance spectroscopy - Discrete energy interface states

NASA Technical Reports Server (NTRS)

Kamieniecki, E.; Kazior, T. E.; Lagowski, J.; Gatos, H. C.

1980-01-01

Interface states and bulk GaAs energy levels were simultaneously investigated in GaAs MOS structures prepared by anodic oxidation. These two types of energy levels were successfully distinguished by carrying out a comparative analysis of deep level transient capacitance spectra of the MOS structures and MS structures prepared on the same samples of epitaxially grown GaAs. The identification and study of the interface states and bulk levels was also performed by investigating the transient capacitance spectra as a function of the filling pulse magnitude. It was found that in the GaAs-anodic oxide interface there are states present with a discrete energy rather than with a continuous energy distribution. The value of the capture cross section of the interface states was found to be 10 to the 14th to 10 to the 15th/sq cm, which is more accurate than the extremely large values of 10 to the -8th to 10 to the -9th/sq cm reported on the basis of conductance measurements.

Structure of water in mesoporous organosilica by calorimetry and inelastic neutron scattering

NASA Astrophysics Data System (ADS)

Levy, Esthy; Kolesnikov, Alexander I.; Li, Jichen; Mastai, Yitzhak

2009-01-01

In this paper, we describe the preparation of mesoporous organosilica samples with hydrophilic or hydrophobic organic functionality inside the silica channel. We synthesized mesoporous organosilica of identical pore sizes based on two different organic surface functionality namely hydrophobic (based on octyltriethoxysilane OTES) and hydrophilic (3-aminopropyltriethoxysilane ATES) and MCM-41 was used as a reference system. The structure of water/ice in those porous silica samples have been investigated over a range temperatures by differential scanning calorimetry (DSC) and inelastic neutron scattering (INS). INS study revealed that water confined in hydrophobic mesoporous organosilica shows vibrational behavior strongly different than bulk water. It consists of two states: water with strong and weak hydrogen bonds (with ratio 1:2.65, respectively), compared to ice-Ih. The corresponding O-O distances in these water states are 2.67 and 2.87 Ǻ, which strongly differ compared to ice-Ih (2.76 Ǻ). INS spectra for water in hydrophilic mesoporous organosilica ATES show behavior similar to bulk water, but with greater degree of disorder.

Ku-band electromagnetic wave absorbing properties of polysiloxane derived Si-O-C bulk ceramics

NASA Astrophysics Data System (ADS)

Ding, Donghai; Li, Zipei; Xiao, Guoqing; Yang, Shaoyu

2018-02-01

The bulk Si-O-C ceramics were prepared by polymer derived ceramics (PDCs) route using polysiloxane as precursor and their properties were investigated for electromagnetic wave absorbing in the frequency range of 12.4-18 GHz (Ku-band). It was found that the catalytic pyrolysis can enhance substantially the absorbing properties by in situ formation of turbostratic carbon network, ordered carbon, and multi-wall carbon nanotubes. The matching thickness of sample containing 1.5 wt% FeCl3 (FPSO-1.5) is 2.2 mm, and its reflection loss exceeds -10 dB in the whole Ku-band with an absorption peak of -35.48 dB at 14.16 GHz. For sample containing 1.5 wt% FeCl3, its absorption peak increases to -15.78 dB, but its matching thickness decreases significantly to 2.2 mm. The polymer derived Si-O-C ceramics could be used as excellent electromagnetic functional devices working in harsh environments.

Sample preparation for the determination of 241Am in sediments utilizing gamma-spectroscopy.

PubMed

Ristic, M; Degetto, S; Ast, T; Cantallupi, C

2002-01-01

This paper describes a procedure developed to separate americium-241 from the bulk of a sample by coprecipitation followed by high sensitivity gamma-counting of the concentrate in a well-type detector. It enables the measurement of 241Am at low concentrations, e.g. fallout levels in soils and sediments, or where large sample sizes are not available. The method is much faster and more reliable than those involving separation from other alpha-emitters, electroplating and alpha-spectrometry. A number of tracer experiments was performed in order to optimize the conditions for coprecipitation of 241Am from sediment leachates. The general outline of the determination of americium is also given.

Effects of High-Pressure High-Temperature Sintering on the Band Gap and Thermoelectric Properties of PbSe

NASA Astrophysics Data System (ADS)

Chen, Bo; Li, Yi; Sun, Zhen-Ya

2018-06-01

In this study, PbSe bulk samples were prepared by a high-pressure high-temperature (HPHT) sintering technique, and the phase compositions, band gaps and thermoelectric properties of the samples were systematically investigated. The sintering pressure exerts a significant influence on the preferential orientation, band gap and thermoelectric properties of PbSe. With increasing pressure, the preferential orientation decreases, mainly due to the decreased crystallinity, while the band gap first decreases and then increases. The electrical conductivity and power factor decrease gradually with increasing pressure, mainly attributed to the decreased carrier concentration and mobility. Consequently, the sample prepared by 2 GPa shows the highest thermoelectric figure-of-merit, ZT, of 0.55 at ˜ 475 K. The ZT of the HPHT-sintered PbSe could be further improved by properly doping or optimizing the HPHT parameters. This study further demonstrates that the sintering pressure could be another degree of freedom to manipulate the band structure and thermoelectric properties of materials.

Microwave surface resistance of bulk YBa2Cu3O6+x material

NASA Astrophysics Data System (ADS)

Fathy, A.; Kalokitis, D.; Belohoubek, E.; Sundar, H. G. K.; Safari, A.

1988-10-01

Superconducting Y-Ba-Cu-O samples were prepared by conventional solid-state reaction. The microwave surface resistance of 1:2:3 compound superconductor material was measured in a special disk resonator structure at 10 GHz. At liquid-nitrogen temperatures the microwave surface resistance is comparable to that of Au. At lower temperature (~10 K) the surface resistance is an order of magnitude lower than that of Au at the same temperature.

Preparation of Authigenic Pyrite from Methane-bearing Sediments for In Situ Sulfur Isotope Analysis Using SIMS.

PubMed

Lin, Zhiyong; Sun, Xiaoming; Peckmann, Jörn; Lu, Yang; Strauss, Harald; Xu, Li; Lu, Hongfeng; Teichert, Barbara M A

2017-08-31

Different sulfur isotope compositions of authigenic pyrite typically result from the sulfate-driven anaerobic oxidation of methane (SO4-AOM) and organiclastic sulfate reduction (OSR) in marine sediments. However, unravelling the complex pyritization sequence is a challenge because of the coexistence of different sequentially formed pyrite phases. This manuscript describes a sample preparation procedure that enables the use of secondary ion mass spectroscopy (SIMS) to obtain in situ δ 34 S values of various pyrite generations. This allows researchers to constrain how SO4-AOM affects pyritization in methane-bearing sediments. SIMS analysis revealed an extreme range in δ 34 S values, spanning from -41.6 to +114.8‰, which is much wider than the range of δ 34 S values obtained by the traditional bulk sulfur isotope analysis of the same samples. Pyrite in the shallow sediment mainly consists of 34 S-depleted framboids, suggesting early diagenetic formation by OSR. Deeper in the sediment, more pyrite occurs as overgrowths and euhedral crystals, which display much higher SIMS δ 34 S values than the framboids. Such 34 S-enriched pyrite is related to enhanced SO4-AOM at the sulfate-methane transition zone, postdating OSR. High-resolution in situ SIMS sulfur isotope analyses allow for the reconstruction of the pyritization processes, which cannot be resolved by bulk sulfur isotope analysis.

The effect of a simple annealing heat treatment on the mechanical properties of cold-sprayed aluminum

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hall, Aaron Christopher; Roemer, Timothy John; Hirschfeld, Deidre A.

2004-11-01

Cold spray, a new member of the thermal spray process family, can be used to prepare dense, thick metal coatings. It has tremendous potential as a spray-forming process. However, it is well known that significant cold work occurs during the cold spray deposition process. This cold work results in hard coatings but relatively brittle bulk deposits. This work investigates the mechanical properties of cold-sprayed aluminum and the effect of annealing on those properties. Cold spray coatings approximately 1 cm thick were prepared using three different feedstock powders: Valimet H-10; Valimet H-20; and Brodmann Flomaster. ASTM E8 tensile specimens were machinedmore » from these coatings and tested using standard tensile testing procedures. Each material was tested in two conditions: as-sprayed; and after a 300 C, 22 h air anneal. The as-sprayed material showed high ultimate strength and low ductility, with <1% elongation. The annealed samples showed a reduction in ultimate strength but a dramatic increase in ductility, with up to 10% elongation. The annealed samples exhibited mechanical properties that were similar to those of wrought 1100 H14 aluminum. Microstructural examination and fractography clearly showed a change in fracture mechanism between the as-sprayed and annealed materials. These results indicate good potential for cold spray as a bulk-forming process.« less

Polymerization stress evolution of a bulk-fill flowable composite under different compliances.

PubMed

Guo, Yongwen; Landis, Forrest A; Wang, Zhengzhi; Bai, Ding; Jiang, Li; Chiang, Martin Y M

2016-04-01

To use a compliance-variable instrument to simultaneously measure and compare the polymerization stress (PS) evolution, degree of conversion (DC), and exotherm of a bulk-fill flowable composite to a packable composite. A bulk-fill flowable composite (Filtek Bulk-fill, FBF) and a conventional packable composite (Filtek Z250, Z250) purchased from 3M ESPE were investigated. The composites were studied using a cantilever-beam based instrument equipped with an in situ near infrared (NIR) spectrometer and a microprobe thermocouple. The measurements were carried out under various instrumental compliances (ranging from 0.3327μm/N to 12.3215μm/N) that are comparable to the compliances of clinically prepared tooth cavities. Correlations between the PS and temperature change as well as the DC were interpreted. The maximum PS of both composites at 10min after irradiation decreased with the increase in the compliance of the cantilever beam. The FBF composite generated a lower final stress than the Z250 sample under instrumental compliances less than ca. 4μm/N; however, both materials generated statistically similar PS values at higher compliances. The reaction exotherm and the DC of both materials were found to be independent of compliance. The DC of the FBF sample was slightly higher than that of the packable Z250 composite while the peak exotherm of FBF was almost double that of the Z250 composite. For FBF, a characteristic drop in the PS was observed during the early stage of polymerization for all compliances studied which was not observed in the Z250 sample. This drop was shown to relate to the greater exotherm of the less-filled FBF sample relative to the Z250 composite. While the composites with lower filler content (low viscosity) are generally considered to have lower PS than the conventional packable composites, a bulk-fill flowable composite was shown to produce lower PS under a lower compliance of constraint as would be experienced if the composite was used as the base material in clinical procedures. Published by Elsevier Ltd.

Synthesis and magnetostrictive properties of Pr(Fe1.95B0.05)1.93 bulk nanocrystalline alloy

NASA Astrophysics Data System (ADS)

Shi, Y. G.; Hu, C. C.; Fan, J. Y.; Shi, D. N.; Lv, L. Y.; Tang, S. L.

2012-11-01

The structure, magnetic properties, and magnetostriction of Pr(Fe1.95B0.05)1.93 alloys prepared by annealing its precursor amorphous ribbons under high pressure were investigated. It was found that Pr(Fe1.95B0.05)1.93 single cubic Laves phase could be obtained only when the pressure is up to 3 GPa. The average grain size about 20 nm is found in the sample synthesized under 6 GPa. A large linear magnetostriction of 541 ppm at 3 kOe is observed in the Pr(Fe1.95B0.05)1.93 compound synthesized under 6 GPa, which is 25% larger than that under 3 GPa. The present work offers an effective method to obtain bulk nanocrystalline magnetostrictive compounds.

Wet-Chemical Synthesis of Enhanced-Thermopower Bi1 -xSbx Nanowire Composites for Solid-State Active Cooling of Electronics

NASA Astrophysics Data System (ADS)

Vandaele, K.; He, Bin; Van Der Voort, P.; De Buysser, K.; Heremans, J. P.

2018-02-01

This paper is a contribution to the Physical Review Applied collection in memory of Mildred S. Dresselhaus. In 1993, Hicks and Dresselhaus [Thermoelectric figure of merit of a one-dimensional conductor, Phys. Rev. B 47, 16631 (1993)., 10.1103/PhysRevB.47.16631] suggested that Bi nanowires could result in values of the thermoelectric figure of merit z T >1 . The Dresselhaus group also calculated a ternary phase diagram for Bi1 -xSbx nanowires as a function of x and wire diameter. This manuscript reports a wet-chemical method to synthesize Bi1 -xSbx -silica nanowire composites. Resistivity, Hall electron concentration, electron mobility, Seebeck and Nernst coefficients, and thermal conductivity of composites are measured and compared to bulk polycrystalline Bi1 -xSbx samples prepared either by ingot casting or by the same wet chemistry but without nanostructuring. A clear increase of the thermopower in 20-nm Bi94Sb6 -silica is reported when compared to bulk samples, and the values are among the highest found in the literature from 300 to 380 K, even though the electron concentration is higher than in the bulk. This suggests that consistent with theory, size quantization is responsible for the thermopower increase.

The contribution of grain boundary and defects to the resistivity in the ferromagnetic state of polycrystalline manganites

NASA Astrophysics Data System (ADS)

Sagdeo, P. R.; Anwar, Shahid; Lalla, N. P.; Patil, S. I.

2006-11-01

In the present study we report the precise resistivity measurements for the polycrystalline bulk sample as well as highly oriented thin-films of La 0.8Ca 0.2MnO 3. The poly crystalline sample was prepared by standard solid-state reaction route and the oriented thin film was prepared by pulsed laser deposition (PLD). The phase purity of these samples was confirmed by X-ray diffraction and the back-scattered electron imaging using scanning electron microscopy (SEM). The oxygen stoichiometry analysis was done by iodimetry titration. The resistivities of these samples were carried out with four-probe resistivity measurement setup. The observed temperature dependence of resistivity data for both the samples was fitted using the polaron model. We have found that polaronic model fits well with the experimental data of both polycrystalline and single crystal samples. A new phenomenological model is proposed and used to estimate contribution to the resistivity due to grain boundary in the ferromagnetic state of polycrystalline manganites and it has been shown that the scattering of electrons from the grain boundary (grain surface) is a function of temperature and controlled by the effective grain resistance at that temperature.

Results of a Saxitoxin Proficiency Test Including Characterization of Reference Material and Stability Studies

PubMed Central

Harju, Kirsi; Rapinoja, Marja-Leena; Avondet, Marc-André; Arnold, Werner; Schär, Martin; Luginbühl, Werner; Kremp, Anke; Suikkanen, Sanna; Kankaanpää, Harri; Burrell, Stephen; Söderström, Martin; Vanninen, Paula

2015-01-01

A saxitoxin (STX) proficiency test (PT) was organized as part of the Establishment of Quality Assurance for the Detection of Biological Toxins of Potential Bioterrorism Risk (EQuATox) project. The aim of this PT was to provide an evaluation of existing methods and the European laboratories’ capabilities for the analysis of STX and some of its analogues in real samples. Homogenized mussel material and algal cell materials containing paralytic shellfish poisoning (PSP) toxins were produced as reference sample matrices. The reference material was characterized using various analytical methods. Acidified algal extract samples at two concentration levels were prepared from a bulk culture of PSP toxins producing dinoflagellate Alexandrium ostenfeldii. The homogeneity and stability of the prepared PT samples were studied and found to be fit-for-purpose. Thereafter, eight STX PT samples were sent to ten participating laboratories from eight countries. The PT offered the participating laboratories the possibility to assess their performance regarding the qualitative and quantitative detection of PSP toxins. Various techniques such as official Association of Official Analytical Chemists (AOAC) methods, immunoassays, and liquid chromatography-mass spectrometry were used for sample analyses. PMID:26602927

Comparative study of the molecularly imprinted polymers prepared by reversible addition-fragmentation chain transfer "bulk" polymerization and traditional radical "bulk" polymerization.

PubMed

Ma, Yue; Pan, Guoqing; Zhang, Ying; Guo, Xianzhi; Zhang, Huiqi

2013-05-01

Bisphenol A (BPA) and propranolol-imprinted polymers have been prepared via both reversible addition-fragmentation chain transfer "bulk" polymerization (RAFTBP) and traditional radical "bulk" polymerization (TRBP) under similar reaction conditions, and their equilibrium binding properties were compared in detail for the first time. The chemical compositions, specific surface areas, equilibrium bindings, and selectivity of the obtained molecularly imprinted polymers (MIPs) were systematically characterized. The experimental results showed that the MIPs with molecular imprinting effects and quite fast binding kinetics could be readily prepared via RAFTBP, but they did not show improved template binding properties in comparison with those prepared via TRBP, which is in sharp contrast to many previous reports. This could be attributed to the heavily interrupted equilibrium between the dormant species and active radicals in the RAFT mechanism because of the occurrence of fast gelation during RAFTBP. The findings presented here strongly demonstrates that the application of controlled radical polymerizations (CRPs) in molecular imprinting does not always benefit the binding properties of the resultant MIPs, which is of significant importance for the rational use of CRPs in generating MIPs with improved properties. Copyright © 2013 John Wiley & Sons, Ltd.

Simple eco-friendly synthesis of the surfactant free SnS nanocrystal toward the photoelectrochemical cell application.

PubMed

Huang, Xiaoguang; Woo, Heechul; Wu, Peinian; Hong, Hyo Jin; Jung, Wan Gil; Kim, Bong-Joong; Vanel, Jean-Charles; Choi, Jin Woo

2017-11-28

A simple, low cost, non-toxic and eco-friendly pathway for synthesizing efficient sunlight-driven tin sulfide photocatalyst was studied. SnS nanocrystals were prepared by using mechanical method. The bulk SnS was obtained by evaporation of SnS nanocrystal solution. The synthesized samples were characterized by using XRD, SEM, TEM, UV-vis, and Raman analyses. Well crystallized SnS nanocrystals were verified and the electrochemical characterization was also performed under visible light irradiation. The SnS nanocrystals have shown remarkable photocurrent density of 7.6 mA cm -2 under 100 mW cm -2 which is about 10 times larger than that of the bulk SnS under notably stable operation conditions. Furthermore, the SnS nanocrystals presented higher stability than the bulk form. The IPCE(Incident photon to current conversion efficiency) of 9.3% at 420 nm was obtained for SnS nanocrystal photoanode which is strikingly higher than that of bulk SnS, 0.78%. This work suggests that the enhancement of reacting area by using SnS nanocrystal absorbers could give rise to the improvement of photoelectrochemical cell efficiency.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shipra, Fnu; Idrobo Tapia, Juan Carlos; Sefat, Athena Safa

This study provides an account of the bulk preparation of TlBa 2Ca 2Cu 3O 9-δ (Tl-1223) superconductor at ambient pressure, and the Tc features under thermal-annealing conditions. The ‘as-prepared’ Tl-1223 (Tc =106 K) presents a significantly higher T c = 125 K after annealing the polycrystalline material in either flowing Ar+4% H 2, or N 2 gases. In order to understand the fundamental reasons for a particular Tc, we refined the average bulk structures using powder X-ray diffraction data. Although Ar+4%H2 annealed Tl- 1223 shows an increased ‘c’ lattice parameter, it shrinks by 0.03% (approximately unchanged) upon N2 anneal. Duemore » to such indeterminate conclusions on the average structural changes, local structures were investigated at using aberration-corrected scanning-transmission electron microscopy technique. Similar compositional changes in the atomic arrangements of both annealed-samples of Tl-1223 were detected in which the plane containing Ca atomic layer gives a non-uniform contrast, due to substitution of some heavier Tl. In this report, extensive bulk properties are summarized through temperature-dependent resistivity, and shielding and Meissner fractions of magnetic susceptibility results; the bulk and local structures are investigated to correlate to properties.« less

Development of a Thermal Rectifier Usable at High Temperature

NASA Astrophysics Data System (ADS)

Takeuchi, Tsunehiro; Goto, Hiroki; Toyama, Yasuhiro; Itoh, Takashi; Mikami, Masashi

2011-05-01

By using Al-based metallic alloys characterized by a disordered structure and a narrow pseudogap of a few hundred meV in energy width persisting at the Fermi level, we succeeded in preparing materials possessing a large increase of thermal conductivity with increasing temperature. This unusual increase of thermal conductivity is caused by the electronic structure effect known as the bipolar diffusion effect (BDE) in the context of the two-band model. A thermal rectifier was constructed using materials exhibiting the BDE. By showing the thermal rectification of the bulk sample prepared in this study, we demonstrate that our newly proposed idea of a thermal rectifier using the BDE is applicable for practical use.

Effect of synthesis methods with different annealing temperatures on micro structure, cations distribution and magnetic properties of nano-nickel ferrite

NASA Astrophysics Data System (ADS)

El-Sayed, Karimat; Mohamed, Mohamed Bakr; Hamdy, Sh.; Ata-Allah, S. S.

2017-02-01

Nano-crystalline NiFe2O4 was synthesized by citrate and sol-gel methods at different annealing temperatures and the results were compared with a bulk sample prepared by ceramic method. The effect of methods of preparation and different annealing temperatures on the crystallize size, strain, bond lengths, bond angles, cations distribution and degree of inversions were investigated by X-ray powder diffraction, high resolution transmission electron microscope, Mössbauer effect spectrometer and vibrating sample magnetometer. The cations distributions were determined at both octahedral and tetrahedral sites using both Mössbauer effect spectroscopy and a modified Bertaut method using Rietveld method. The Mössbauer effect spectra showed a regular decrease in the hyperfine field with decreasing particle size. Saturation magnetization and coercivity are found to be affected by the particle size and the cations distribution.

Making the practically impossible "Merely difficult"--Cryogenic FIB lift-out for "Damage free" soft matter imaging.

PubMed

Parmenter, Christopher D J; Fay, Michael W; Hartfield, Cheryl; Eltaher, Hoda M

2016-04-01

The preparation of thinned lamellae from bulk samples for transmission electron microscopy (TEM) analysis has been possible in the focussed ion beam scanning electron microscope (FIB-SEM) for over 20 years via the in situ lift-out method. Lift-out offers a fast and site specific preparation method for TEM analysis, typically in the field of materials science. More recently it has been applied to a low-water content biological sample (Rubino 2012). This work presents the successful lift-out of high-water content lamellae, under cryogenic conditions (cryo-FIB lift-out) and using a nanomanipulator retaining its full range of motion, which are advances on the work previously done by Rubino (2012). Strategies are explored for maintaining cryogenic conditions, grid attachment using cryo-condensation of water and protection of the lamella when transferring to the TEM. © 2016 Wiley Periodicals, Inc.

Observation of amorphous to crystalline phase transformation in Te substituted Sn-Sb-Se thin films

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chander, Ravi, E-mail: rcohri@yahoo.com

2015-05-15

Thin films of Sn-Sb-Se-Te (8 ≤ x ≤ 14) chalcogenide system were prepared by thermal evaporation technique using melt quenched bulk samples. The as-prepared thin films were found amorphous as evidenced from X-ray diffraction studies. Resistivity measurement showed an exponential decrease with temperature upto critical temperature (transition temperature) beyond which a sharp decrease was observed and with further increase in temperature showed an exponential decrease in resistivity with different activation energy. The transition temperature showed a decreasing trend with tellurium content in the sample. The resistivity measurement during cooling run showed no abrupt change in resistivity. The resistivity measurements ofmore » annealed films did not show any abrupt change revealing the structural transformation occurring in the material. The transition width showed an increase with tellurium content in the sample. The resistivity ratio showed two order of magnitude improvements for sample with higher tellurium content. The observed transition temperature in this system was found quite less than already commercialized Ge-Sb-Te system for optical and electronic memories.« less

Synthesis and magnetic characterization of nickel ferrite nanoparticles prepared by co-precipitation route

NASA Astrophysics Data System (ADS)

Maaz, K.; Karim, S.; Mumtaz, A.; Hasanain, S. K.; Liu, J.; Duan, J. L.

2009-06-01

Magnetic nanoparticles of nickel ferrite (NiFe 2O 4) have been synthesized by co-precipitation route using stable ferric and nickel salts with sodium hydroxide as the precipitating agent and oleic acid as the surfactant. X-ray diffraction (XRD) and transmission electron microscope (TEM) analyses confirmed the formation of single-phase nickel ferrite nanoparticles in the range 8-28 nm depending upon the annealing temperature of the samples during the synthesis. The size of the particles ( d) was observed to be increasing linearly with annealing temperature of the sample while the coercivity with particle size goes through a maximum, peaking at ˜11 nm and then decreases for larger particles. Typical blocking effects were observed below ˜225 K for all the prepared samples. The superparamagnetic blocking temperature ( T B) was found to be increasing with increasing particle size that has been attributed to the increased effective anisotropy energy of the nanoparticles. The saturation moment of all the samples was found much below the bulk value of nickel ferrite that has been attributed to the disordered surface spins or dead/inert layer in these nanoparticles.

A validated spectrofluorimetric method for the determination of citalopram in bulk and pharmaceutical preparations based on the measurement of the silver nanoparticles-enhanced fluorescence of citalopram/terbium complexes.

PubMed

Khan, Muhammad Naeem; Shah, Jasmin; Jan, Muhammad Rasul; Lee, Sang Hak

2013-01-01

A simple, sensitive, and accurate spectrofluorimetric method was developed for the determination of citalopram in bulk and pharmaceutical preparations. The method is based on the enhancement of the weak fluorescence signal (FL) of the Tb (III)-citalopram system in the presence of silver nanoparticles. Fluorescence intensities were measured at 555 nm after excitation at 281 nm. Prepared silver nanoparticles (AgNPs) were characterized by UV-Visible spectra and transmission electron microscopy (TEM). Various factors affecting the formation of citalopram-Tb (III)-AgNPs complexes were studied and optimized. The fluorescence intensity versus concentration plot was linear over the range 0.02-14 μg mL(-1), with an excellent correlation coefficient of 0.9978. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 7.15 × 10(-6) μg mL(-1) and 2.38 × 10(-5) μg mL(-1) respectively. The proposed method was found to have good reproducibility with a relative standard deviation of 3.66% (n = 6). The interference effects of common excipients found in pharmaceutical preparations were studied. The developed method was validated statistically by performing recoveries studies and successfully applied for the assay of citalopram in bulk powder and pharmaceutical preparations. Percent recoveries were found to range from 98.98% to 100.97% for bulk powder and from 96.57% to 101.77% for pharmaceutical preparations.

Magnetic properties of Mn0.1Mg0.2TM0.7Fe2O4 (TM = Zn, Co, or Ni) prepared by hydrothermal processes: The effects of crystal size and chemical composition

NASA Astrophysics Data System (ADS)

Nhlapo, T. A.; Msomi, J. Z.; Moyo, T.

2018-02-01

Nano-crystalline Zn-, Co-, and Ni-substituted Mn-Mg ferrites were prepared by hydrothermal process and annealed at 1100 °C. Annealing conditions are critical on the crystalline phase. TEM and XRD data reveal particle sizes between 8 nm and 15 nm for the as-prepared fine powders, which increase to about 73 nm after sintering at 1100 °C. Mӧssbauer spectra show well resolved magnetic splitting in bulk samples. The as-prepared fine powders show weak hyperfine splitting and broad central doublets associated with fine particles. Magnetization data reveal a high coercive field at about 300 K of about 945 Oe in the Co-based nanosized oxide, which reduces to about 360 Oe after thermal annealing at 1100 °C. The magnetization curves of Zn- and Ni-based samples show much lower coercive fields indicative of superparamagnetic nanoparticles. The crystallite size and chemical composition have significant effects on the properties of Mn0.1Mg0.2(Zn,Co,Ni)0.7Fe2O4 investigated.

Influence of Ag, Cd or Pb Addition on Electrical and Dielectric Properties of Bulk Glassy Se-Ge

NASA Astrophysics Data System (ADS)

El-Metwally, E. G.; Shakra, A. M.

2018-05-01

Bulk glassy samples of Se0.7Ge0.3 and Se0.7Ge0.25 X 0.05 (X = Ag, Cd or Pb) chalcogenide glass have been prepared by melt-quenching method. The studied compositions were examined in powder form by x-ray diffraction analysis. The direct-current (dc) conductivity σ_{{dc}} was measured for bulk samples in the temperature range from 303 K to 433 K, revealing enhancement with temperature for all samples. The results indicate two values of activation energy ( Δ E_{{σ1 }} and Δ E_{{σ2 }} ) due to two conduction mechanisms. Measurements of the alternating-current (ac) conductivity σ_{{ac}} ( ω ) and dielectric properties for bulk samples were carried out in the temperature range from 303 K to 433 K and frequency range from 1 kHz to 1 MHz. The ac conductivity σ_{{ac}} ( ω ) was temperature dependent and proportional to ωS , where S is the frequency exponent, which reduced with rising temperature, and ω is the angular frequency. These results are discussed based on a correlated barrier hopping model. The calculated values of the maximum height of the barrier W_{{M}} for each composition are consistent with carrier hopping over a potential barrier. The density of localized states N( {E_{{F}} } ) at the Fermi level lay in the range from 1019 eV-1 cm-3 to 1020 eV-1 cm-3, and increased with temperature. The dielectric constant ɛ1 ( ω ) and loss ɛ2 ( ω ) increased with temperature but decreased with frequency. The values of σ_{{dc}} , σ_{{ac}} ( ω ) , ɛ1 ( ω ) , and ɛ2 ( ω ) increased with temperature and with addition of Ag, Cd or Pb. The observed increase was greater for Se0.7Ge0.25Pb0.05 than for Se0.7Ge0.25Cd0.05, which was greater than for Se0.7Ge0.25Ag0.05.

Structural and AC loss study for pure and doped MgB{sub 2} superconductor

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hansdah, J. S.; Sarun, P. M., E-mail: sarun.res@gmail.com

2015-06-24

Superconducting polycrystalline bulk MgB{sub 2} samples doped with n-C, n-Y{sub 2}O{sub 3} and n-Ho{sub 2}O{sub 3} were prepared by powder-in-sealed (PIST) method. XRD measurement shows the influence of dopants on phase and lattice parameters of samples. The ac susceptibility measurement reveals ac loss and activation energy of the samples. Nano-C doped sample shows less ac loss in all frequency (208 Hz – 999 Hz) among the doped samples; whereas n-Ho{sub 2}O{sub 3} doped sample shows highest ac loss. The activation energy is high for rare earth (n-Y{sub 2}O{sub 3} and n-Ho{sub 2}O{sub 3}) doped samples as compare to n-C doped samples whichmore » reveals the enhancement in flux-pinning properties of these materials.« less

Laboratory Evaluation of Remediation Alternatives for U.S. Coast Guard Small Arms Firing Ranges

DTIC Science & Technology

1999-11-01

S) is an immobilization process that involves the mixing of a contaminated soil with a binder material to enhance the physical and chemical...samples were shipped to WES for laboratory analysis. Phase III: Homogenization of the Bulk Samples. Each of the bulk samples was separately mixed to...produce uniform samples for testing. These mixed bulk soil samples were analyzed for metal content. Phase IV: Characterization of the Bulk Soils

Incidence of Listeria spp. in Dairy Cows Feed and Raw Milk in Latvia

PubMed Central

Konosonoka, I. H.; Jemeljanovs, A.; Osmane, B.; Ikauniece, D.; Gulbe, G.

2012-01-01

Feed is a risk factor for poisoning the farm environment thus also fresh milk with pathogenic microorganisms of Listeria genus species. Listeria ivanovii, Listeria innocua, and Listeria seeligeri were isolated from 9.2%, but Listeria monocytogenes from 20.0% of feed samples. Most often different fodders (9.3%) and silage (4.7%) were contaminated with Listeria monocytogenes. Listeria genus species were isolated more often from feed prepared and used in organic dairy farm than from that used in conventional dairy farm, correspondingly 44.4% and 18.3%. No Listeria monocytogenes was found in bulk milk samples of organic dairy farm. PMID:23738125

Correlative transmission electron microscopy and electrical properties study of switchable phase-change random access memory line cells

DOE Office of Scientific and Technical Information (OSTI.GOV)

Oosthoek, J. L. M.; Kooi, B. J., E-mail: B.J.Kooi@rug.nl; Voogt, F. C.

2015-02-14

Phase-change memory line cells, where the active material has a thickness of 15 nm, were prepared for transmission electron microscopy (TEM) observation such that they still could be switched and characterized electrically after the preparation. The result of these observations in comparison with detailed electrical characterization showed (i) normal behavior for relatively long amorphous marks, resulting in a hyperbolic dependence between SET resistance and SET current, indicating a switching mechanism based on initially long and thin nanoscale crystalline filaments which thicken gradually, and (ii) anomalous behavior, which holds for relatively short amorphous marks, where initially directly a massive crystalline filament ismore » formed that consumes most of the width of the amorphous mark only leaving minor residual amorphous regions at its edges. The present results demonstrate that even in (purposely) thick TEM samples, the TEM sample preparation hampers the probability to observe normal behavior and it can be debated whether it is possible to produce electrically switchable TEM specimen in which the memory cells behave the same as in their original bulk embedded state.« less

Correlative transmission electron microscopy and electrical properties study of switchable phase-change random access memory line cells

NASA Astrophysics Data System (ADS)

Oosthoek, J. L. M.; Voogt, F. C.; Attenborough, K.; Verheijen, M. A.; Hurkx, G. A. M.; Gravesteijn, D. J.; Kooi, B. J.

2015-02-01

Phase-change memory line cells, where the active material has a thickness of 15 nm, were prepared for transmission electron microscopy (TEM) observation such that they still could be switched and characterized electrically after the preparation. The result of these observations in comparison with detailed electrical characterization showed (i) normal behavior for relatively long amorphous marks, resulting in a hyperbolic dependence between SET resistance and SET current, indicating a switching mechanism based on initially long and thin nanoscale crystalline filaments which thicken gradually, and (ii) anomalous behavior, which holds for relatively short amorphous marks, where initially directly a massive crystalline filament is formed that consumes most of the width of the amorphous mark only leaving minor residual amorphous regions at its edges. The present results demonstrate that even in (purposely) thick TEM samples, the TEM sample preparation hampers the probability to observe normal behavior and it can be debated whether it is possible to produce electrically switchable TEM specimen in which the memory cells behave the same as in their original bulk embedded state.

[Comparison of wear resistance and flexural strength of three kinds of bulk-fill composite resins].

PubMed

Zhang, Huan; Zhang, Meng-Long; Qiu, Li-Hong; Yu, Jing-Tao; Zhan, Fu-Liang

2016-06-01

To compare the abrasion resistance and flexure strength of three bulk-fill resin composites with an universal nano-hybrid composite resins. The specimens were prepared with three kinds of bulk fill composites (SDR , sonicfill, Tetric N-Ceram Bulk Fill) and an universal nano-hybrid composite resins(Herculite Precis). 10 mm in diameter × 2mm in height specimens were prepared for abrasion resistance, while 2 mm in width × 2 mm in depth×25 mm in length specimens were prepared for flexure strength. The specimens were mounted in a bal1-on-disc wear testing machine and abraded with the media artificial saliva(50 N loads, 10000 cycles).Flexural test was performed with an Universal Testing Machine at a cross-head speed of 1mm/min. One-way variance analysis was used to determine the statistical differences of volume loss and flexural strength among groups with SPSS 13.0 software package(P<0.05). The volume loss was as follows: SDR (1.2433±0.11) mm30.05). With regard to wear resistance and flexural strength, Tetric N-Ceram Bulk Fill is recommended as an alternative for posterior restorations.

Size effect on the structural, magnetic, and magnetotransport properties of electron doped manganite La0.15Ca0.85MnO3

NASA Astrophysics Data System (ADS)

Thomas, Rini; Das, Gangadhar; Mondal, Rajib; Pradheesh, R.; Mahato, R. N.; Geetha Kumary, T.; Nirmala, R.; Morozkin, A. V.; Lamsal, J.; Yelon, W. B.; Nigam, A. K.; Malik, S. K.

2012-04-01

Nanocrystalline La0.15Ca0.85MnO3 samples of various grain sizes ranging from ˜17 to 42 nm have been prepared by sol-gel technique. Phase purity and composition were verified by room temperature x-ray diffraction and SEM-EDAX analysis. The bulk La0.15Ca0.85MnO3 is known to order antiferromagnetically around 170 K and to undergo a simultaneous crystal structural transition. DC magnetization measurements on 17 nm size La0.15Ca0.85MnO3 show a peak at ˜130 K (TN) in zero-field-cooled (ZFC) state. Field-cooled magnetization bifurcates from ZFC data around 200 K hinting a weak ferromagnetic component near room temperature due to surface moments of the nanoparticle sample. Low temperature powder neutron diffraction experiments reveal that the incomplete structural transition from room temperature orthorhombic to low temperature orthorhombic-monoclinic state also occurs in the nanoparticle sample as in the bulk. Magnetization in the ordered state decreases as particle size increases, thus indicating the reduction of the competing ferromagnetic surface moments.

Green and Fast Laser Fusion Technique for Bulk Silicate Rock Analysis by Laser Ablation-Inductively Coupled Plasma Mass Spectrometry.

PubMed

Zhang, Chenxi; Hu, Zhaochu; Zhang, Wen; Liu, Yongsheng; Zong, Keqing; Li, Ming; Chen, Haihong; Hu, Shenghong

2016-10-18

Sample preparation of whole-rock powders is the major limitation for their accurate and precise elemental analysis by laser ablation inductively-coupled plasma mass spectrometry (ICPMS). In this study, a green, efficient, and simplified fusion technique using a high energy infrared laser was developed for major and trace elemental analysis. Fusion takes only tens of milliseconds for each sample. Compared to the pressed pellet sample preparation, the analytical precision of the developed laser fusion technique is higher by an order of magnitude for most elements in granodiorite GSP-2. Analytical results obtained for five USGS reference materials (ranging from mafic to intermediate to felsic) using the laser fusion technique generally agree with recommended values with discrepancies of less than 10% for most elements. However, high losses (20-70%) of highly volatile elements (Zn and Pb) and the transition metal Cu are observed. The achieved precision is within 5% for major elements and within 15% for most trace elements. Direct laser fusion of rock powders is a green and notably simple method to obtain homogeneous samples, which will significantly accelerate the application of laser ablation ICPMS for whole-rock sample analysis.

Effect of CNT as a Nucleating Agent on Cell Morphology and Thermal Insulation Property of the Rigid Polyurethane Foams.

PubMed

Ahn, WonSool; Lee, Joon-Man

2015-11-01

The effects of MWCNT on the cell sizes, cell uniformities, thermal conductivities, bulk densities, foaming kinetics, and compressive mechanical properties of the rigid PUFs were investigated. To obtain the better uniform dispersed state of MWCNT, grease-type master batch of MWCNT/surfactant was prepared by three-roll mill. Average cell size of the PUF samples decreased from 185.1 for the neat PUF to 162.9 μm for the sample of 0.01 phr of MWCNT concentration. Cell uniformity was also enhanced showing the standard cell-size deviation of 61.7 and 35.2, respectively. While the thermal conductivity of the neat PUF was 0.0222 W/m(o)K, that of the sample with 0.01 phr of MWCNT showed 0.0204 W/m(o)K, resulting 8.2% reduction of the thermal conductivity. Bulk density of the PUF samples was observed as nearly the same values as 30.0 ± 1.0 g/cm3 regardless of MWCNT. Temperature profiles during foaming process showed that an indirect indication of the nucleation effect of MWCNT for the PUF foaming system, showing faster and higher temperature rising with time. The compressive yield stress is nearly the same as 0.030 x 10(5) Pa regardless of MWCNT.

Fluorescence-excitation and emission spectra from LH2 antenna complexes of Rhodopseudomonas acidophila as a function of the sample preparation conditions.

PubMed

Kunz, Ralf; Timpmann, Kõu; Southall, June; Cogdell, Richard J; Köhler, Jürgen; Freiberg, Arvi

2013-10-10

The high sensitivity of optical spectra of pigment-protein complexes to temperature and pressure is well known. In the present study, we have demonstrated the significant influence of the environments commonly used in bulk and single-molecule spectroscopic studies at low temperatures on the LH2 photosynthetic antenna complex from Rhodopseudomonas acidophila. A transfer of this LH2 complex from a bulk-buffer solution into a spin-coated polymer film results in a 189 cm(-1) blue shift of the B850 excitonic absorption band at 5 K. Within the molecular exciton model, the origin of this shift could be disentangled into three parts, namely to an increase of the local site energies, a contraction of the exciton band, and a decrease of the displacement energy.

7 CFR 201.40 - Bulk.

Code of Federal Regulations, 2011 CFR

2011-01-01

... Sampling in the Administration of the Act § 201.40 Bulk. Bulk seeds or screenings shall be sampled by inserting a long probe or thrusting the hand into the bulk as circumstances require in at least seven... 7 Agriculture 3 2011-01-01 2011-01-01 false Bulk. 201.40 Section 201.40 Agriculture Regulations of...

7 CFR 201.40 - Bulk.

Code of Federal Regulations, 2010 CFR

2010-01-01

... Sampling in the Administration of the Act § 201.40 Bulk. Bulk seeds or screenings shall be sampled by inserting a long probe or thrusting the hand into the bulk as circumstances require in at least seven... 7 Agriculture 3 2010-01-01 2010-01-01 false Bulk. 201.40 Section 201.40 Agriculture Regulations of...

Extrinsic contributions to the dielectric response in sintered BaTiO3 nanostructures in paraelectric and ferroelectric regimes

NASA Astrophysics Data System (ADS)

Jaffari, G. Hassnain; Rehman, Atiq ur; Iqbal, Asad M.; Awan, M. S.; Saleemi, Mohsin

2017-11-01

Post sintering studies of BaTiO3 (BTO) nanoparticles are presented in detail. Bulk nanostructures were prepared via three different compaction processes, namely, uniaxial cold pressing (UCP), Cold Isostatic Pressing (CIP) and Spark Plasma Sintering (SPS). Effect of compaction technique on microstructures have been investigated and correlated with electrical response for each sample. In addition to the transport properties, temperature and frequency dependent dielectric response of variously sintered samples and bulk counterpart was recorded. Several aspects have been identified that are essential to be taken into account in order to completely understand physical processes. Drastically distinct features were observed in paraelectric (PE) regime well above ferroelectric (FE)-PE transition temperature. These features include intra grain conduction with a reduction in the magnitude of PE to FE peak dielectric constant magnitude. Role of strain, grain boundary conduction associated with observation of Maxwell Wagner relaxation and hopping conduction in dielectric and ferroelectric response have been observed and discussed. Densification with presence of oxygen vacancies, significantly enhances conductivity associated with the hopping of the carriers, in turn deteriorated ferroelectric response.

Development and validation of a high performance liquid chromatographic method for the separation of exo and endo isomers of granatamine (9-methyl-9-azabicyclo[3.3.1]nonan-3-amine); a key intermediate of granisetron.

PubMed

Krishna, S Radha; Babu, P Suresh; Rao, B M; Rao, N Someswara

2009-12-01

A simple and accurate high-performance liquid chromatographic method was developed for the determination of exo-9-methyl-9-azabicyclo[3.3.1]nonan-3-amine in endo-9-methyl-9-azabicyclo[3.3.1]nonan-3-amine, commercially known as grantamine and used as a key intermediate in the preparation of granisetron bulk drug. Chromatographic separation of the exo and endo isomers of 9-methyl-9-azabicyclo[3.3.1]nonan-3-amine was achieved on an Inertsil C8 column using a mobile phase containing 0.3% trifluoroacetic acid. The resolution between the two isomers was found to be more than 4. The limit of detection (LOD) and limit of quantification (LOQ) of exo isomer were 0.8 and 2.5 microg x mL(-1) respectively, for a 10 microL injection volume. The percentage recovery of exo-isomer ranged from 99 to 102% w/w in the endo-9-methyl-9-azabicyclo[3.3.1]nonan-3-amine sample. The test solution and mobile phase were observed to be stable up to 48 h after preparation. The validated method yielded good results for precision, linearity, accuracy, robustness and ruggedness. The proposed method was found to be suitable and accurate for the quantitative determination of exo-isomer in bulk samples of endo-9-methyl-9-azabicyclo[3.3.1]nonan-3-amine.

Structural elucidation and magnetic behavior evaluation of Cu-Cr doped BaCo-X hexagonal ferrites

NASA Astrophysics Data System (ADS)

Azhar Khan, Muhammad; Hussain, Farhat; Rashid, Muhammad; Mahmood, Asif; Ramay, Shahid M.; Majeed, Abdul

2018-04-01

Ba2-xCuxCo2CryFe28-yO46 (x = 0.0, 0.1, 0.2, 0.3, 0.4, y = 0.0, 0.2, 0.4, 0.6, 0.8) X-type hexagonal ferrites were synthesized via micro-emulsion route. The techniques which were applied to characterize the prepared samples are as follows: X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Dielectric measurements and vibrating sample magnetometer (VSM). The structural parameters i.e. lattice constant (a, c), cell volume (V), X-ray density, bulk density and crystallite size of all the prepared samples were obtained using XRD analysis. The lattice parameters 'a' and 'c' increase from 5.875 Å to 5.934 Å and 83.367 Å to 83.990 Å respectively. The crystallite size of investigated samples lies in the range of 28-32 nm. The magnetic properties of all samples have been calculated by vibrating sample magnetometer (VSM) analysis. The increase in coercivity (Hc) was observed with the increase of doping contents. It was observed that the coercivity (Hc) of all prepared samples is inversely related to the crystalline size which reflects that all materials are super-paramagnetic. The dielectric parameters i.e. dielectric constant, dielectric loss, tangent loss etc were obtained in the frequency range of 1 MHz-3 GHz and followed the Maxwell-Wagner's model. The significant variation the dielectric parameters are observed with increasing frequency. The maximum Q value is obtained at ∼2 GHz due to which these materials are used for high frequency multilayer chip inductors.

Characterization of mono-ethylene-glycol based industrial polyurethanes samples by fast-neutron radiography and neutron tomography

NASA Astrophysics Data System (ADS)

Rogante, Massimo; Söllradl, Stefan

2016-09-01

A complicated structural organization of polyurethanes may have a strong influence on the materials functional properties. Under particular conditions such as mechanical and thermal loading and aging, it leads to the material degradation, even in fresh-prepared bulk polymers and especially if defects are present in the material. Unwanted bubbles can be observed, which form during the expansion of the mixture during its chemical reaction and remain present in the final product. These macro-, micro- and nano-bubbles influence the material's performance. In this work, neutron radiography and tomography have been adopted to characterize at a macro-scale level the bulk of commercially available polyurethane samples, obtained from dissimilar- mixture ratios with different densities and branching levels as well as from different zones of the production mould. The characterisation allowed an estimation of the different dense materials - as they are used, e.g., in soles of shoes - as well as the invisible defects like pores and cracks, responsible for the materials fracture by mechanical loading. The obtained information are expected to be useful for various industrial sectors such as automotive and footwear industry. It will be completed by applying SANS, which has already proved to characterize the microstructure of the bulk-polymer with respect to nano-pores, micro-cracks and their arrangement in the polymer matrix.

[Effect of techniques of composite resin insertion and polymerization on microleakage and microhardness].

PubMed

Amaral, Cristiane Mariote; Castro, Ana Karina Barbieri Bedran de; Pimenta, Luiz André Freire; Ambrosano, Glaucia Maria Boni

2002-01-01

The aim of this study was to evaluate the influence of techniques of composite resin polymerization and insertion on microleakage and microhardness. One hundred and eighty class II cavities were prepared in bovine teeth and assigned to six groups: G1 - bulk filling + conventional polymerization; G2 - bucco-lingual increments + conventional polymerization; G3 - bulk filling + soft-start polymerization; G4 - bucco-lingual increments + soft-start polymerization; G5 - bulk filling + progressive polymerization; G6 - bucco-lingual increments + progressive polymerization. All cavities were restored with the Z100/Single Bond system (3M). After thermocycling, the samples were immersed in 2% methylene blue dye solution for 4 hours. Half of the samples were embedded in polystyrene resin, and Knoop microhardness was measured. The Kruskal-Wallis test did not reveal statistical differences (p > 0.05) between the polymerization and insertion techniques as to microleakage. Regarding microhardness, the two-way ANOVA and the Tukey test did not reveal statistical differences between the restorative techniques (p > 0.05), but progressive polymerization (G5 and G6) was associated with smaller Knoop microhardness values (p < 0.05): G = 144.11; G2 = 143.89; G3 = 141.14; G4 = 142.79; G5 = 132.15; G6 = 131.67. It was concluded that the evaluated polymerization and insertion techniques did not affect marginal microleakage, but a decrease in microhardness occurred when progressive polymerization was carried out.

46 CFR 154.1831 - Persons in charge of transferring liquid cargo in bulk or preparing cargo tanks.

Code of Federal Regulations, 2011 CFR

2011-10-01

... in bulk or a cool-down, warm-up, gas-free, or air-out of each cargo tank; (2) Each transfer of liquid cargo in bulk, and each cool-down, warm-up, gas-free, or air-out of a cargo tank, is supervised by a... in bulk or a cool-down, warm-up, gas-free, or air-out of a cargo tank possesses the qualifications...

46 CFR 154.1831 - Persons in charge of transferring liquid cargo in bulk or preparing cargo tanks.

Code of Federal Regulations, 2014 CFR

2014-10-01

... in bulk or a cool-down, warm-up, gas-free, or air-out of each cargo tank; (2) Each transfer of liquid cargo in bulk, and each cool-down, warm-up, gas-free, or air-out of a cargo tank, is supervised by a... in bulk or a cool-down, warm-up, gas-free, or air-out of a cargo tank possesses the qualifications...

46 CFR 154.1831 - Persons in charge of transferring liquid cargo in bulk or preparing cargo tanks.

Code of Federal Regulations, 2012 CFR

2012-10-01

... in bulk or a cool-down, warm-up, gas-free, or air-out of each cargo tank; (2) Each transfer of liquid cargo in bulk, and each cool-down, warm-up, gas-free, or air-out of a cargo tank, is supervised by a... in bulk or a cool-down, warm-up, gas-free, or air-out of a cargo tank possesses the qualifications...

46 CFR 154.1831 - Persons in charge of transferring liquid cargo in bulk or preparing cargo tanks.

Code of Federal Regulations, 2013 CFR

2013-10-01

... in bulk or a cool-down, warm-up, gas-free, or air-out of each cargo tank; (2) Each transfer of liquid cargo in bulk, and each cool-down, warm-up, gas-free, or air-out of a cargo tank, is supervised by a... in bulk or a cool-down, warm-up, gas-free, or air-out of a cargo tank possesses the qualifications...

Sources of polycyclic hydrocarbons and pesticides in soluble fraction of deposition samples in Kocaeli, Turkey.

PubMed

Binici, Burcu; Yenisoy-Karakaş, Serpil; Bilsel, Mine; Durmaz-Hilmioğlu, Nilüfer

2014-02-01

A wet-dry deposition sampler was located at The Scientific and Technological Research Council of Turkey-National Metrology Institute (TUBITAK-UME) station, and a bulk deposition sampler was placed at the Kadıllı village to determine the atmospheric deposition flux of polycyclic aromatic hydrocarbons (PAHs) and pesticides (organochlorine and organophosphorus) in soluble fraction of samples in Kocaeli, Turkey. The 28 samples for each wet, dry, and total deposition were collected weekly from March 2006 to March 2007. Gas chromatography-tandem mass spectrometry was used to analyze the samples which were prepared by using solid-phase extraction (SPE) method. The sum of volume weighted mean of deposition fluxes was obtained as 7.43 μg m(-2) day(-1) for wet deposition, 0.28 μg m(-2) day(-1) for dry deposition and 0.54 μg m(-2) day(-1) for bulk deposition samples for PAHs and 9.88 μg m(-2) day(-1) for wet deposition, 4.49 μg m(-2) day(-1) for dry deposition, and 3.29 μg m(-2) day(-1) for bulk deposition samples for pesticides. While benzo(a)anthracene had the highest fluxes among PAH compounds for all types of depositions, guthion and phosphamidon had the highest deposition flux compared with the other pesticides. Benzo(ghi)perylene, dibenz(a,h)anthracene, indeno(1,2,3-c,d)pyrene, benzo(a)pyrene, and acenaphthene were not detected in any of the samples. Beta-HCH, gamma-HCH, and endrin aldehyde were the only compounds among 18 organochlorine pesticides to be detected in all deposition samples. The main sources of pesticides were the high number of greenhouses around the sampling stations. However, all of the organophosphorus pesticides were detected in all deposition samples. The pollution sources were identified as coal and natural gas combustion, petrogenic sources, and traffic for TUBITAK-UME station whereas coal and natural gas combustion and traffic were the main sources for Kadıllı station by considering the results of factor analysis, ratios, and wind sector analysis.

Influence of substitution, nonstoichiometry and annealing-conditions on superconductivity and normal conductivity of Fe1+δ (Te1‑x Xx ) (X=Se, S)

NASA Astrophysics Data System (ADS)

Lima, M. S. L.; ElMassalami, M.; Deguchi, K.; Takeya, H.; Takano, Y.

2018-03-01

Thermal evolution of resistivity, ρ(T, x), of as-prepared samples of Fe1+δ Te1‑x S x (δ ≈ 0, x ≤ 0.2 = solubility limit) demonstrate a granular log-in-T character within Ts < T <300K, a Kondo-like resistive contribution within Tc < T < Ts and granular superconductivity at low temperature (Ts = structural transition point of Fe1+δ Te, Tc =superconducting transition point). We attribute the log-in-T character as well as the nonbulk superconducting features of as-prepared samples to their granular superconductor nature. Annealing in oxygen removes Kondo-like contribution, annihilates pair-breaking centres and establishes bulk superconductivity but, in contrast, the high-temperature granular log-in-T character is hardly influenced. This analysis was successfully extended to the isomorphous Fe1+δ Te1‑x Se x as well as to other types of post-synthesis sample-treatment (e.g. annealing in different gas ambient or soaking in particular liquids).

CuO nanoparticles encapsulated inside Al-MCM-41 mesoporous materials via direct synthetic route

PubMed Central

Huo, Chengli; Ouyang, Jing; Yang, Huaming

2014-01-01

Highly ordered aluminum-containing mesoporous silica (Al-MCM-41) was prepared using attapulgite clay mineral as a Si and Al source. Mesoporous complexes embedded with CuO nanoparticles were subsequently prepared using various copper sources and different copper loadings in a direct synthetic route. The resulting CuO/Al-MCM-41 composite possessed p6mm hexagonally symmetry, well-developed mesoporosity, and relatively high BET surface area. In comparison to pure silica, these mesoporous materials embedded with CuO nanoparticles exhibited smaller pore diameter, thicker pore wall, and enhanced thermal stability. Long-range order in the aforementioned samples was observed for copper weight percentages as high as 30%. Furthermore, a significant blue shift of the absorption edge for the samples was observed when compared with that of bulk CuO. H2-TPR measurements showed that the direct-synthesized CuO/Al-MCM-41 exhibited remarkable redox properties compared to the post-synthesized samples, and most of the CuO nanoparticles were encapsulated within the mesoporous structures. The possible interaction between CuO and Al-MCM-41 was also investigated. PMID:24419589

40 CFR 761.265 - Sampling bulk PCB remediation waste and porous surfaces.

Code of Federal Regulations, 2010 CFR

2010-07-01

... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Sampling bulk PCB remediation waste..., DISTRIBUTION IN COMMERCE, AND USE PROHIBITIONS Cleanup Site Characterization Sampling for PCB Remediation Waste in Accordance with § 761.61(a)(2) § 761.265 Sampling bulk PCB remediation waste and porous surfaces...

A new RE + 011 TSIG method for the fabrication of high quality and large size single domain YBCO bulk superconductors

NASA Astrophysics Data System (ADS)

Yang, W. M.; Chen, L. P.; Wang, X. J.

2016-02-01

High quality single domain YBCO bulk superconductors, 20 mm in diameter, have been fabricated using a new top seeded infiltration and growth method (called the RE + 011 TSIG method), with a new solid phase (Y2O3 + xBaCuO2) instead of the conventional Y2BaCuO5 solid phase, x = 0, 0.5, 1.0, 1.2, 1.5, 1.8, 2.0, 2.5, 3.0. The effects of different BaCuO2 contents x on the growth morphology, microstructure, and levitation force have been investigated. The results show that the levitation force of the YBCO bulks first increases and then decreases with increasing x, and reaches maximum levitation forces of about 49.2 N (77 K, 0.5 T, with the traditional liquid phase of YBa2Cu3O y + 3 BaCuO2 + 2 CuO) and 47 N (77.3 K, 0.5 T, with the new liquid phase of Y2O3 + 10 BaCuO2 + 6 CuO) when x = 1.2, which is much higher than that of the samples fabricated with the conventional solid phases (23 N). The average Y2BaCuO5 particle size is about 1 μm, which is much smaller than the 3.4 μm in the samples prepared with the conventional Y2BaCuO5 solid phase; this means that the flux pinning force of the sample can be improved by using the new solid phase. Based on this method, single domain YBCO bulks 40 mm, 59 mm, and 93 mm in diameter have also been fabricated using the TSIG process with the new solid phases (Y2O3 + 1.2BaCuO2). These results indicate that the new TSIG process developed by our lab is a very important and practical method for the fabrication of low cost, large size, and high quality single domain REBCO bulk superconductors.

Three-dimensional microstructural characterization of bulk plutonium and uranium metals using focused ion beam technique

NASA Astrophysics Data System (ADS)

Chung, Brandon W.; Erler, Robert G.; Teslich, Nick E.

2016-05-01

Nuclear forensics requires accurate quantification of discriminating microstructural characteristics of the bulk nuclear material to identify its process history and provenance. Conventional metallographic preparation techniques for bulk plutonium (Pu) and uranium (U) metals are limited to providing information in two-dimension (2D) and do not allow for obtaining depth profile of the material. In this contribution, use of dual-beam focused ion-beam/scanning electron microscopy (FIB-SEM) to investigate the internal microstructure of bulk Pu and U metals is demonstrated. Our results demonstrate that the dual-beam methodology optimally elucidate microstructural features without preparation artifacts, and the three-dimensional (3D) characterization of inner microstructures can reveal salient microstructural features that cannot be observed from conventional metallographic techniques. Examples are shown to demonstrate the benefit of FIB-SEM in improving microstructural characterization of microscopic inclusions, particularly with respect to nuclear forensics.

Three-dimensional microstructural characterization of bulk plutonium and uranium metals using focused ion beam technique

DOE PAGES

Chung, Brandon W.; Erler, Robert G.; Teslich, Nick E.

2016-03-03

Nuclear forensics requires accurate quantification of discriminating microstructural characteristics of the bulk nuclear material to identify its process history and provenance. Conventional metallographic preparation techniques for bulk plutonium (Pu) and uranium (U) metals are limited to providing information in two-dimension (2D) and do not allow for obtaining depth profile of the material. In this contribution, use of dual-beam focused ion-beam/scanning electron microscopy (FIB-SEM) to investigate the internal microstructure of bulk Pu and U metals is demonstrated. Our results demonstrate that the dual-beam methodology optimally elucidate microstructural features without preparation artifacts, and the three-dimensional (3D) characterization of inner microstructures can revealmore » salient microstructural features that cannot be observed from conventional metallographic techniques. As a result, examples are shown to demonstrate the benefit of FIB-SEM in improving microstructural characterization of microscopic inclusions, particularly with respect to nuclear forensics.« less

Lithium niobate bulk crystallization promoted by CO2 laser radiation

NASA Astrophysics Data System (ADS)

Ferreira, N. M.; Costa, F. M.; Nogueira, R. N.; Graça, M. P. F.

2012-09-01

The crystallization induced by laser radiation is a very promising technique to promote glass/ceramic transformation, being already used to produce crystalline patterns on glass surfaces. In this work, a SiO2-Li2O-Nb2O5 glass, prepared by the sol-gel route, was submitted to CO2 laser radiation and conventional heat-treatments in order to induce the LiNbO3 crystallization. The structure and morphology of the samples prepared by both routes was analyzed as a function of exposure time, radiation power and heat-treatment temperatures by XRD, Raman spectroscopy and SEM. The results reveal a correlation between the crystallization degree of LiNbO3 particles and glass matrix with the heat treatment type and experimental parameters. An heat-treatment at 650 °C/4 h was necessary to induce crystallization in heat treatments samples while 4 W/500 s was enough for laser radiation ones, corresponding a reduction time processing of ˜14 000 s.

Evaluation of dredged material proposed for ocean disposal from Shark River Project area

DOE Office of Scientific and Technical Information (OSTI.GOV)

Antrim, L.D.; Gardiner, W.W.; Barrows, E.S.

1996-09-01

The objective of the Shark River Project was to evaluate proposed dredged material to determine its suitability for unconfined ocean disposal at the Mud Dump Site. Tests and analyses were conducted on the Shark River sediments. The evaluation of proposed dredged material consisted of bulk sediment chemical and physical analysis, chemical analyses of dredging site water and elutriate, water-column and benthic acute toxicity tests, and bioaccumulation tests. Individual sediment core samples collected from the Shark River were analyzed for grain size, moisture content, and total organic carbon (TOC). One sediment composite was analyzed for bulk density, specific gravity, metals, chlorinatedmore » pesticides, polychlorinated biphenyl (PCB) congeners, polynuclear aromatic hydrocarbons (PAHs), and 1,4- dichlorobenzene. Dredging site water and elutriate, prepared from suspended-particulate phase (SPP) of the Shark River sediment composite, were analyzed for metals, pesticides, and PCBs. Benthic acute toxicity tests and bioaccumulation tests were performed.« less

Effects of grain size on the properties of bulk nanocrystalline Co-Ni alloys

NASA Astrophysics Data System (ADS)

Qiao, Gui-Ying; Xiao, Fu-Ren

2017-08-01

Bulk nanocrystalline Co78Ni22 alloys with grain size ranging from 5 nm to 35 nm were prepared by high-speed jet electrodeposition (HSJED) and annealing. Microhardness and magnetic properties of these alloys were investigated by microhardness tester and vibrating sample magnetometer. Effects of grain size on these characteristics were also discussed. Results show that the microhardness of nanocrystalline Co78Ni22 alloys increases following a d -1/2-power law with decreasing grain size d. This phenomenon fits the Hall-Petch law when the grain size ranges from 5 nm to 35 nm. However, coercivity H c increases following a 1/d-power law with increasing grain size when the grain size ranges from 5 nm to 15.9 nm. Coercivity H c decreases again for grain sizes above 16.6 nm according to the d 6-power law.

Inelastic neutron scattering study of phonon density of states in nanostructured Si1 xGex thermoelectrics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dhital, Chetan; Abernathy, Douglas L; Zhu, Gaohua

2012-01-01

Inelastic neutron scattering measurements are utilized to explore relative changes in the generalized phonon density of states of nanocrystalline Si1 xGex thermoelectric materials prepared via ball-milling and hot-pressing techniques. Dynamic signatures of Ge clustering can be inferred from the data by referencing the resulting spectra to a density functional theoretical model assuming homogeneous alloying via the virtual-crystal approximation. Comparisons are also presented between as-milled Si nanopowder and bulk, polycrystalline Si where a preferential low-energy enhancement and lifetime broadening of the phonon density of states appear in the nanopowder. Negligible differences are however observed between the phonon spectra of bulk Simore » andhot-pressed, nanostructured Si samples suggesting that changes to the single-phonon dynamics above 4 meV play only a secondary role in the modified heat conduction of this compound.« less

Preparation and Characterization of Ato Nanoparticles by Coprecipitation with Modified Drying Method

NASA Astrophysics Data System (ADS)

Liu, Shimin; Liang, Dongdong; Liu, Jindong; Jiang, Weiwei; Liu, Chaoqian; Ding, Wanyu; Wang, Hualin; Wang, Nan

Antimony-doped tin oxide (ATO) nanoparticles were prepared by coprecipitation by packing drying and traditional direct drying (for comparison) methods. The as-prepared ATO nanoparticles were characterized by TG, XRD, EDS, TEM, HRTEM, BET, bulk density and electrical resistivity measurements. Results indicated that the ATO nanoparticles obtained by coprecipitation with direct drying method featured hard-agglomerated morphology, high bulk density, low surface area and low electrical resistivity, probably due to the direct liquid evaporation during drying, the fast shrinkage of the precipitate, the poor removal efficiency of liquid molecules and the hard agglomerate formation after calcination. Very differently, the ATO product obtained by the packing and drying method featured free-agglomerated morphology, low bulk density, high surface area and high electrical resistivity ascribed probably to the formed vapor cyclone environment and liquid evaporation-resistance, avoiding fast liquid removal and improving the removal efficiency of liquid molecules. The intrinsic formation mechanism of ATO nanoparticles from different drying methods was illustrated based on the dehydration process of ATO precipitates. Additionally, the packing and drying time played key roles in determining the bulk density, morphology and electrical conductivity of ATO nanoparticles.

Full in-vitro analyses of new-generation bulk fill dental composites cured by halogen light.

PubMed

Tekin, Tuçe Hazal; Kantürk Figen, Aysel; Yılmaz Atalı, Pınar; Coşkuner Filiz, Bilge; Pişkin, Mehmet Burçin

2017-08-01

The objective of this study was to investigate the full in-vitro analyses of new-generation bulk-fill dental composites cured by halogen light (HLG). Two types' four composites were studied: Surefill SDR (SDR) and Xtra Base (XB) as bulk-fill flowable materials; QuixFill (QF) and XtraFill (XF) as packable bulk-fill materials. Samples were prepared for each analysis and test by applying the same procedure, but with different diameters and thicknesses appropriate to the analysis and test requirements. Thermal properties were determined by thermogravimetric analysis (TG/DTG) and differential scanning calorimetry (DSC) analysis; the Vickers microhardness (VHN) was measured after 1, 7, 15 and 30days of storage in water. The degree of conversion values for the materials (DC, %) were immediately measured using near-infrared spectroscopy (FT-IR). The surface morphology of the composites was investigated by scanning electron microscopes (SEM) and atomic-force microscopy (AFM) analyses. The sorption and solubility measurements were also performed after 1, 7, 15 and 30days of storage in water. In addition to his, the data were statistically analyzed using one-way analysis of variance, and both the Newman Keuls and Tukey multiple comparison tests. The statistical significance level was established at p<0.05. According to the ISO 4049 standards, all the tested materials showed acceptable water sorption and solubility, and a halogen light source was an option to polymerize bulk-fill, resin-based dental composites. Copyright © 2017 Elsevier B.V. All rights reserved.

A New Commercializable Route for the Preparation of Single-Source Precursors for Bulk, Thin-Film, and Nanocrystallite I-III-IV Semiconductors

NASA Technical Reports Server (NTRS)

Banger, Kulbinder K.; Jin, Michael H. C.; Harris, Jerry D.; Fanwick, Philip E.; Hepp, Aloysius F.

2004-01-01

We report a new simplified synthetic procedure for commercial manufacture of ternary single source precursors (SSP). This new synthetic process has been successfully implemented to fabricate known SSPs on bulk scale and the first liquid SSPs to the semiconductors CuInSe2 and AgIn(x)S(y). Single crystal X-ray determination reveals the first unsolvated ternary AgInS SSP. SSPs prepared via this new route have successfully been used in a spray assisted chemical vapor deposition (CVD) process to deposit polycrystalline thin films, and for preparing ternary nanocrystallites.

Thermal conductivity of bulk and thin film β-Ga2O3 measured by the 3ω technique

NASA Astrophysics Data System (ADS)

Blumenschein, N.; Slomski, M.; Paskov, P. P.; Kaess, F.; Breckenridge, M. H.; Muth, J. F.; Paskova, T.

2018-02-01

Thermal conductivity of undoped and Sn-doped β-Ga2O3 bulk and single-crystalline thin films have been measured by the 3ω technique. The bulk samples were grown by edge-defined film-field growth (EFG) method, while the thin films were grown on c-plane sapphire by pulsed-laser deposition (PLD). All samples were with (-201) surface orientation. Thermal conductivity of bulk samples was calculated along the in-plane and cross-plane crystallographic directions, yielding a maximum value of 29 W/m-K in the [010] direction at room temperature. A slight thermal conductivity decrease was observed in the Sn-doped bulk samples, which was attributed to enhanced phonon-impurity scattering. The differential 3ω method was used for β-Ga2O3 thin film samples due to the small film thickness. Results show that both undoped and Sndoped films have a much lower thermal conductivity than that of the bulk samples, which is consistent with previous reports in the literature showing a linear relationship between thermal conductivity and film thickness. Similarly to bulk samples, Sn-doped thin films have exhibited a thermal conductivity decrease. However, this decrease was found to be much greater in thin film samples, and increased with Sn doping concentration. A correlation between thermal conductivity and defect/dislocation density was made for the undoped thin films.

Defect ordering in YBa 2Cu 3O 6.5 and YBa 2Cu 3O 6.6: Synthesis and characterization by neutron and electron diffraction

NASA Astrophysics Data System (ADS)

Lin, Y. P.; Greedan, J. E.; O'Reilly, A. H.; Reimers, J. N.; Stager, C. V.; Post, M. L.

1990-02-01

Polycrystalline samples of YBa 2Cu 3O 6.5 and YBa 2Cu 3O 6.6 were prepared by oxygen titration of YBa 2 Cu 3O 6.0 at 450°C followed by slow cooling to room temperature. Both samples showed evidence for the a' = 2a supercell in individual grains by electron diffraction as reported previously. In addition the superlattice was observed in neutron powder diffraction indicating that the bulk material is also well ordered. In this study the YBa 2Cu 3O 6.6 phase showed longer correlation lengths for ordering along both a* and b* than YBa 2Cu 3O 6.5. For the former compound the powder-averaged, sample-averaged a* correlation distance is 26A˚from neutron diffraction. Analysis of electron diffraction profiles on selected single crystals give correlation lengths along a*, b*, and c* of 100, 200, and 50A˚, respectively. Dark field imaging discloses the presence of striped, ordered domains elongated along b* with a distribution of sizes. Both neutron diffraction and dark field imaging indicate that the volume fraction of the ordered domains is about 50%. A correlation is noted between the Meissner Effect and the extent of defect ordering in the bulk samples of the two phases.

Piezoelectric and dielectric characterization of corona and contact poled PZT-epoxy-MWCNT bulk composites

NASA Astrophysics Data System (ADS)

Banerjee, S.; Cook-Chennault, K. A.; Du, W.; Sundar, U.; Halim, H.; Tang, A.

2016-11-01

Three-phase lead zirconate titanate (PZT, PbZr0.52Ti0.48O3)-epoxy-multi-walled carbon nanotube (MWCNT) bulk composites were prepared, where the volume fraction of PZT was held constant at 30%, while the volume fraction of the MWCNTs was varied from 1.0%-10%. The samples were poled using either a parallel plate contact or contactless (corona) poling technique. The piezoelectric strain coefficient (d33), dielectric constant (ɛ), and dielectric loss tangent (tan δ) of the samples were measured at 110 Hz, and compared as a function of poling technique and volume fraction of MWCNTs. The highest values for dielectric constant and piezoelectric strain coefficients were 465.82 and 18.87 pC/N for MWCNT volume fractions of 10% and 6%, respectively. These values were obtained for samples that were poled using the corona contactless method. The impedance and dielectric spectra of the composites were recorded over a frequency range of 100 Hz-20 MHz. The impedance values observed for parallel-plate contact poled samples are higher than that of corona poled composites. The fractured surface morphology and distribution of the PZT particles and MWCNTs were observed with the aid of electron dispersion spectroscopy and a scanning electron microscope. The surface morphology of the MWCNTs was observed with the aid of a field emission transmission electron microscope.

Absence of morphotropic phase boundary effects in BiFeO3-PbTiO3 thin films grown via a chemical multilayer deposition method

NASA Astrophysics Data System (ADS)

Gupta, Shashaank; Bhattacharjee, Shuvrajyoti; Pandey, Dhananjai; Bansal, Vipul; Bhargava, Suresh K.; Peng, Ju Lin; Garg, Ashish

2011-07-01

We report an unusual behavior observed in (BiFeO3)1- x -(PbTiO3) x (BF- xPT) thin films prepared using a multilayer chemical solution deposition method. Films of different compositions were grown by depositing several bilayers of BF and PT precursors of varying BF and PT layer thicknesses followed by heat treatment in air. X-ray diffraction showed that samples of all compositions show mixing of two compounds resulting in a single-phase mixture, also confirmed by transmission electron microscopy. In contrast to bulk compositions, samples show a monoclinic (MA-type) structure suggesting disappearance of the morphotropic phase boundary (MPB) at x=0.30 as observed in the bulk. This is accompanied by the lack of any enhancement of the remanent polarization at the MPB, as shown by the ferroelectric measurements. Magnetic measurements showed an increase in the magnetization of the samples with increasing BF content. Significant magnetization in the samples indicates melting of spin spirals in the BF- xPT films, arising from a random distribution of iron atoms. Absence of Fe2+ ions was corroborated by X-ray photoelectron spectroscopy measurements. The results illustrate that thin film processing methodology significantly changes the structural evolution, in contrast to predictions from the equilibrium phase diagram, besides modifying the functional characteristics of the BP- xPT system dramatically.

Advances in understanding the surface chemistry of lignocellulosic biomass via time-of-flight secondary ion mass spectrometry

DOE PAGES

Tolbert, Allison K.; Ragauskas, Arthur J.

2016-12-12

Overcoming the natural recalcitrance of lignocellulosic biomass is necessary in order to efficiently convert biomass into biofuels or biomaterials and many times this requires some type of chemical pretreatment and/or biological treatment. While bulk chemical analysis is the traditional method of determining the impact a treatment has on biomass, the chemistry on the surface of the sample can differ from the bulk chemistry. Specifically, enzymes and microorganisms bind to the surface of the biomass and their efficiency could be greatly impacted by the chemistry of the surface. Therefore, it is important to study and understand the chemistry of the biomassmore » at the surface. Time-of- flight secondary ion mass spectrometry (ToF-SIMS) is a powerful tool that can spectrally and spatially analyze the surface chemistry of a sample. This review discusses the advances in understanding lignocellulosic biomass surface chemistry using the ToF-SIMS by addressing the instrument parameters, biomass sample preparation, and characteristic lignocellulosic ion fragmentation peaks along with their typical location in the plant cell wall. Furthermore, the use of the ToF-SIMS in detecting chemical changes due to chemical pretreatments, microbial treatments, and physical or genetic modifications is discussed along with possible future applications of the instrument in lignocellulosic biomass studies.« less

Advances in understanding the surface chemistry of lignocellulosic biomass via time-of-flight secondary ion mass spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tolbert, Allison K.; Ragauskas, Arthur J.

Overcoming the natural recalcitrance of lignocellulosic biomass is necessary in order to efficiently convert biomass into biofuels or biomaterials and many times this requires some type of chemical pretreatment and/or biological treatment. While bulk chemical analysis is the traditional method of determining the impact a treatment has on biomass, the chemistry on the surface of the sample can differ from the bulk chemistry. Specifically, enzymes and microorganisms bind to the surface of the biomass and their efficiency could be greatly impacted by the chemistry of the surface. Therefore, it is important to study and understand the chemistry of the biomassmore » at the surface. Time-of- flight secondary ion mass spectrometry (ToF-SIMS) is a powerful tool that can spectrally and spatially analyze the surface chemistry of a sample. This review discusses the advances in understanding lignocellulosic biomass surface chemistry using the ToF-SIMS by addressing the instrument parameters, biomass sample preparation, and characteristic lignocellulosic ion fragmentation peaks along with their typical location in the plant cell wall. Furthermore, the use of the ToF-SIMS in detecting chemical changes due to chemical pretreatments, microbial treatments, and physical or genetic modifications is discussed along with possible future applications of the instrument in lignocellulosic biomass studies.« less

Cuspal Deflection of Premolars Restored with Bulk-Fill Composite Resins.

PubMed

Behery, Haytham; El-Mowafy, Omar; El-Badrawy, Wafa; Saleh, Belal; Nabih, Sameh

2016-01-01

This in vitro study compared cuspal deflection of premolars restored with three bulk-fill composite resins to that of incrementally-restored ones with a low-shrinkage silorane-based restorative material. Forty freshly-extracted intact human upper premolars were used. Reference points at buccal and palatal cusp tips were acid-etched and composite rods were horizontally bonded to them (TPH-Spectra-HV, Dentsply). Two acrylic resin guiding paths were made for each premolar to guide beaks of a digital micrometer used for cuspal deflection measurements. Standardized MOD cavities, 3 mm wide bucco-lingually and 3.5 mm deep, were prepared on each premolar. Prepared teeth were then equally divided into four groups (n = 10) and each group was assigned to one of four composite resin (QuiXX, Dentsply; X-tra fil, Voco; Tetric EvoCeram Bulk Fill, Ivoclar Vivadent; low-shrinkage Filtek LS, 3M/ESPE). Adper Single Bond-Plus, 3M/ESPE was used with all bulk-fill restoratives. LS-System Adhesive, 3M/ESPE was used with Filtek LS. For each prepared premolar, cuspal deflection was measured in microns as the difference between two readings between reference points before and after restoration completion. Means and SDs were calculated and data statistically-analyzed using One-way ANOVA and Tukey's test. Filtek LS showed the lowest mean cuspal deflection value 6.4(0.84)μm followed by Tetric EvoCeram Bulk Fill 10.1(1.2) μm and X-tra fil 12.4(1.35)μm, while QuiXX showed the highest mean 13(1.05)μm. ANOVA indicated significant difference among mean values of groups (p < 0.001). Tukey's test indicated no significant difference in mean values between QuiXX and X-tra fil (p = 0.637). Tetric EvoCeram Bulk Fill had significantly lower mean cuspal deflection compared with the two other bulk-fill composite resins tested. Filtek LS had the lowest significant mean cuspal deflection in comparison to all tested bulk-fill restoratives. The use of Tetric EvoCeram Bulk fill composite resin restorative for class II MOD cavities resulted in reduced cuspal deflection in comparison to the two other bulk-fill composite resins tested. The silorane-based Filtek LS restorative resulted in the least cuspal deflection in comparison to all tested bulk-fill composite restoratives. © 2016 Wiley Periodicals, Inc.

Synthesis of lithium superionic conductor by growth of a nanoglass within mesoporous silica SBA-15 template

NASA Astrophysics Data System (ADS)

Chatterjee, Soumi; Miah, Milon; Saha, Shyamal Kumar; Chakravorty, Dipankar

2018-04-01

Nanodimensional silica based glasses containing alkali ions have recently been grown using suitable templates. These have shown electrical properties drastically different from those of their bulk counterpart. We have synthesized silicophosphate glasses having lithium ions with concentrations of 15-35 mole% Li2O within mesoporous silica SBA-15 (Santa Barbara amorphous-15) comprising of pores of diameter ~5 nm. The nanoglasses are characterized by electrical conductivities 5-6 orders of magnitude higher than those of the corresponding bulk glasses. These properties are attributed to the presence of a larger free volume in the nanoglasses as compared to their bulk states. The nanocomposites with 35 mole% Li2O exhibit an electrical conductivity of ~3 × 10-4 S · cm-1 at around room temperature. The activation energy for Li+ ion migration has been estimated from the conductivity-temperature variation to be 0.078 eV. These nanocomposites are believed to be ideally suited for the fabrication of solid state lithium ion batteries. We have also explored the efficiency of silicophosphate glass powders as possible electrode materials. Glass of composition 70SiO2/30P2O5 was prepared by using Pluronic P-123 tri-block copolymer along with suitable precursor sols. Cyclic voltammetric and galvanostatic charge/discharge measurements were carried out on the samples prepared in combination with suitable conductive fillers using a two-electrode system. These exhibited a high specific capacitance of 356 F g-1 making them ideally suitable as electrode materials for making a lithium ion solid state battery system.

Hexaferrite multiferroics: from bulk to thick films

NASA Astrophysics Data System (ADS)

Koutzarova, T.; Ghelev, Ch; Peneva, P.; Georgieva, B.; Kolev, S.; Vertruyen, B.; Closset, R.

2018-03-01

We report studies of the structural and microstructural properties of Sr3Co2Fe24O41 in bulk form and as thick films. The precursor powders for the bulk form were prepared following the sol-gel auto-combustion method. The prepared pellets were synthesized at 1200 °C to produce Sr3Co2Fe24O41. The XRD spectra of the bulks showed the characteristic peaks corresponding to the Z-type hexaferrite structure as a main phase and second phases of CoFe2O4 and Sr3Fe2O7-x. The microstructure analysis of the cross-section of the bulk pellets revealed a hexagonal sheet structure. Large areas were observed of packages of hexagonal sheets where the separate hexagonal particles were ordered along the c axis. Sr3Co2Fe24O41 thick films were deposited from a suspension containing the Sr3Co2Fe24O41 powder. The microstructural analysis of the thick films showed that the particles had the perfect hexagonal shape typical for hexaferrites.

ASBESTOS CONTAINING MATERIALS IN SCHOOL BUILDINGS: BULK SAMPLE ANALYSIS QUALITY ASSURANCE PROGRAM. BULK SAMPLE ROUNDS 12, 13 AND BLIND ROUND III

EPA Science Inventory

The report presents the results of laboratories participating in the twelveth, thirteenth and third (III) blind round of the bulk sample analysis quality assurance program sponsored by the U.S. Environmental Protection Agency. Three hundred twenty-three, 386 and 51 laboratories w...

46 CFR 154.1831 - Persons in charge of transferring liquid cargo in bulk or preparing cargo tanks.

Code of Federal Regulations, 2010 CFR

2010-10-01

... SECURITY (CONTINUED) CERTAIN BULK DANGEROUS CARGOES SAFETY STANDARDS FOR SELF-PROPELLED VESSELS CARRYING... vessel, and his or her agent, and each of them, shall provide documentary evidence that the person in...

Microtensile bond strength of bulk-fill restorative composites to dentin.

PubMed

Mandava, Jyothi; Vegesna, Divya-Prasanna; Ravi, Ravichandra; Boddeda, Mohan-Rao; Uppalapati, Lakshman-Varma; Ghazanfaruddin, M D

2017-08-01

To facilitate the easier placement of direct resin composite in deeper cavities, bulk fill composites have been introduced. The Mechanical stability of fillings in stress bearing areas restored with bulk-fill resin composites is still open to question, since long term clinical studies are not available so far. Thus, the objective of the study was to evaluate and compare the microtensile bond strength of three bulk-fill restorative composites with a nanohybrid composite. Class I cavities were prepared on sixty extracted mandibular molars. Teeth were divided into 4 groups (n= 15 each) and in group I, the prepared cavities were restored with nanohybrid (Filtek Z250 XT) restorative composite in an incremental manner. In group II, III and IV, the bulk-fill composites (Filtek, Tetric EvoCeram, X-tra fil bulk-fill restoratives) were placed as a 4 mm single increment and light cured. The restored teeth were subjected to thermocycling and bond strength testing was done using instron testing machine. The mode of failure was assessed by scanning electron microscope (SEM). The bond strength values obtained in megapascals (MPa) were subjected to statistical analysis, using SPSS/PC version 20 software.One-way ANOVA was used for groupwise comparison of the bond strength. Tukey's Post Hoc test was used for pairwise comparisons among the groups. The highest mean bond strength was achieved with Filtek bulk-fill restorative showing statistically significant difference with Tetric EvoCeram bulk-fill ( p < 0.003) and X-tra fil bulk-fill ( p <0.001) composites. Adhesive failures are mostly observed with X-tra fil bulk fill composites, whereas mixed failures are more common with other bulk fill composites. Bulk-fill composites exhibited adequate bond strength to dentin and can be considered as restorative material of choice in posterior stress bearing areas. Key words: Bond strength, Bulk-fill restoratives, Configuration factor, Polymerization shrinkage.

Fracture resistance of endodontically treated teeth restored with Zirconia filler containing composite core material and fiber posts.

PubMed

Jeaidi, Zaid Al

2016-01-01

To assess the fracture resistance of endodontically treated teeth with a novel Zirconia (Zr) nano-particle filler containing bulk fill resin composite. Forty-five freshly extracted maxillary central incisors were endodontically treated using conventional step back preparation and warm lateral condensation filling. Post space preparation was performed using drills compatible for fiber posts (Rely X Fiber Post) on all teeth (n=45), and posts were cemented using self etch resin cement (Rely X Unicem). Samples were equally divided into three groups (n=15) based on the type of core materials, ZirconCore (ZC) MulticCore Flow (MC) and Luxacore Dual (LC). All specimens were mounted in acrylic resin and loads were applied (Universal testing machine) at 130° to the long axis of teeth, at a crosshead speed of 0.5 mm/min until failure. The loads and the site at which the failures occurred were recorded. Data obtained was tabulated and analyzed using a statistical program. The means and standard deviations were compared using ANOVA and Multiple comparisons test. The lowest and highest failure loads were shown by groups LC (18.741±3.02) and MC (25.16±3.30) respectively. Group LC (18.741±3.02) showed significantly lower failure loads compared to groups ZC (23.02±4.21) and MC (25.16±3.30) (p<0.01). However groups ZC (23.02±4.21) and MC (25.16±3.30) showed comparable failure loads (p=0.23). Fracture resistance of endodontically treated teeth restored with Zr filler containing bulk fill composite cores was comparable to teeth restored with conventional Zr free bulk fill composites. Zr filled bulk fill composites are recommended for restoration of endodontically treated teeth as they show comparable fracture resistance to conventional composite materials with less catastrophic failures.

Methods for producing silicon carbide architectural preforms

NASA Technical Reports Server (NTRS)

DiCarlo, James A. (Inventor); Yun, Hee (Inventor)

2010-01-01

Methods are disclosed for producing architectural preforms and high-temperature composite structures containing high-strength ceramic fibers with reduced preforming stresses within each fiber, with an in-situ grown coating on each fiber surface, with reduced boron within the bulk of each fiber, and with improved tensile creep and rupture resistance properties for each fiber. The methods include the steps of preparing an original sample of a preform formed from a pre-selected high-strength silicon carbide ceramic fiber type, placing the original sample in a processing furnace under a pre-selected preforming stress state and thermally treating the sample in the processing furnace at a pre-selected processing temperature and hold time in a processing gas having a pre-selected composition, pressure, and flow rate. For the high-temperature composite structures, the method includes additional steps of depositing a thin interphase coating on the surface of each fiber and forming a ceramic or carbon-based matrix within the sample.

Advances in imaging secondary ion mass spectrometry for biological samples

DOE PAGES

Boxer, Steven G.; Kraft, Mary L.; Weber, Peter K.

2008-12-16

Imaging mass spectrometry combines the power of mass spectrometry to identify complex molecules based on mass with sample imaging. Recent advances in secondary ion mass spectrometry have improved sensitivity and spatial resolution, so that these methods have the potential to bridge between high-resolution structures obtained by X-ray crystallography and cyro-electron microscopy and ultrastructure visualized by conventional light microscopy. Following background information on the method and instrumentation, we address the key issue of sample preparation. Because mass spectrometry is performed in high vacuum, it is essential to preserve the lateral organization of the sample while removing bulk water, and this hasmore » been a major barrier for applications to biological systems. Furthermore, recent applications of imaging mass spectrometry to cell biology, microbial communities, and biosynthetic pathways are summarized briefly, and studies of biological membrane organization are described in greater depth.« less

ASBESTOS-CONTAINING MATERIALS IN SCHOOL BUILDINGS: BULK SAMPLE ANALYSIS QUALITY ASSURANCE PROGRAM-BULK SAMPLE ROUNDS 9, 10, 11 AND BLIND ROUND 2

EPA Science Inventory

The report presents the results of laboratories participating in the nineth, tenth, eleventh and second blind round(s) of the bulk sample analysis quality assurance program sponsored by the U.S. Environmental Protection Agency. Two hundred fifty-four, 320, 318, and 50 laboratorie...

Wastewater Biosolid Composting Optimization Based on UV-VNIR Spectroscopy Monitoring

PubMed Central

Temporal-Lara, Beatriz; Melendez-Pastor, Ignacio; Gómez, Ignacio; Navarro-Pedreño, Jose

2016-01-01

Conventional wastewater treatment generates large amounts of organic matter–rich sludge that requires adequate treatment to avoid public health and environmental problems. The mixture of wastewater sludge and some bulking agents produces a biosolid to be composted at adequate composting facilities. The composting process is chemically and microbiologically complex and requires an adequate aeration of the biosolid (e.g., with a turner machine) for proper maturation of the compost. Adequate (near) real-time monitoring of the compost maturity process is highly difficult and the operation of composting facilities is not as automatized as other industrial processes. Spectroscopic analysis of compost samples has been successfully employed for compost maturity assessment but the preparation of the solid compost samples is difficult and time-consuming. This manuscript presents a methodology based on a combination of a less time-consuming compost sample preparation and ultraviolet, visible and short-wave near-infrared spectroscopy. Spectroscopic measurements were performed with liquid compost extract instead of solid compost samples. Partial least square (PLS) models were developed to quantify chemical fractions commonly employed for compost maturity assessment. Effective regression models were obtained for total organic matter (residual predictive deviation—RPD = 2.68), humification ratio (RPD = 2.23), total exchangeable carbon (RPD = 2.07) and total organic carbon (RPD = 1.66) with a modular and cost-effective visible and near infrared (VNIR) spectroradiometer. This combination of a less time-consuming compost sample preparation with a versatile sensor system provides an easy-to-implement, efficient and cost-effective protocol for compost maturity assessment and near-real-time monitoring. PMID:27854280

Wastewater Biosolid Composting Optimization Based on UV-VNIR Spectroscopy Monitoring.

PubMed

Temporal-Lara, Beatriz; Melendez-Pastor, Ignacio; Gómez, Ignacio; Navarro-Pedreño, Jose

2016-11-15

Conventional wastewater treatment generates large amounts of organic matter-rich sludge that requires adequate treatment to avoid public health and environmental problems. The mixture of wastewater sludge and some bulking agents produces a biosolid to be composted at adequate composting facilities. The composting process is chemically and microbiologically complex and requires an adequate aeration of the biosolid (e.g., with a turner machine) for proper maturation of the compost. Adequate (near) real-time monitoring of the compost maturity process is highly difficult and the operation of composting facilities is not as automatized as other industrial processes. Spectroscopic analysis of compost samples has been successfully employed for compost maturity assessment but the preparation of the solid compost samples is difficult and time-consuming. This manuscript presents a methodology based on a combination of a less time-consuming compost sample preparation and ultraviolet, visible and short-wave near-infrared spectroscopy. Spectroscopic measurements were performed with liquid compost extract instead of solid compost samples. Partial least square (PLS) models were developed to quantify chemical fractions commonly employed for compost maturity assessment. Effective regression models were obtained for total organic matter (residual predictive deviation-RPD = 2.68), humification ratio (RPD = 2.23), total exchangeable carbon (RPD = 2.07) and total organic carbon (RPD = 1.66) with a modular and cost-effective visible and near infrared (VNIR) spectroradiometer. This combination of a less time-consuming compost sample preparation with a versatile sensor system provides an easy-to-implement, efficient and cost-effective protocol for compost maturity assessment and near-real-time monitoring.

46 CFR 153.975 - Preparation for cargo transfer.

Code of Federal Regulations, 2013 CFR

2013-10-01

... Shipping COAST GUARD, DEPARTMENT OF HOMELAND SECURITY (CONTINUED) CERTAIN BULK DANGEROUS CARGOES SHIPS CARRYING BULK LIQUID, LIQUEFIED GAS, OR COMPRESSED GAS HAZARDOUS MATERIALS Operations Cargo Transfer... facility is made before the cargo transfer piping is joined. (c) Any supplemental inert gas supply...

46 CFR 153.975 - Preparation for cargo transfer.

Code of Federal Regulations, 2011 CFR

2011-10-01

... Shipping COAST GUARD, DEPARTMENT OF HOMELAND SECURITY (CONTINUED) CERTAIN BULK DANGEROUS CARGOES SHIPS CARRYING BULK LIQUID, LIQUEFIED GAS, OR COMPRESSED GAS HAZARDOUS MATERIALS Operations Cargo Transfer... facility is made before the cargo transfer piping is joined. (c) Any supplemental inert gas supply...

46 CFR 153.975 - Preparation for cargo transfer.

Code of Federal Regulations, 2012 CFR

2012-10-01

... Shipping COAST GUARD, DEPARTMENT OF HOMELAND SECURITY (CONTINUED) CERTAIN BULK DANGEROUS CARGOES SHIPS CARRYING BULK LIQUID, LIQUEFIED GAS, OR COMPRESSED GAS HAZARDOUS MATERIALS Operations Cargo Transfer... facility is made before the cargo transfer piping is joined. (c) Any supplemental inert gas supply...

46 CFR 153.975 - Preparation for cargo transfer.

Code of Federal Regulations, 2014 CFR

2014-10-01

... Shipping COAST GUARD, DEPARTMENT OF HOMELAND SECURITY (CONTINUED) CERTAIN BULK DANGEROUS CARGOES SHIPS CARRYING BULK LIQUID, LIQUEFIED GAS, OR COMPRESSED GAS HAZARDOUS MATERIALS Operations Cargo Transfer... facility is made before the cargo transfer piping is joined. (c) Any supplemental inert gas supply...

Preparation and magnetic properties of nickel nanowires by reduction in ethylene glycol medium under the influence of magnetic field

NASA Astrophysics Data System (ADS)

Sun, Wanshuo; Cheng, Junsheng; Li, Lankai; Chen, Shunzhong; Chang, Kun

2017-01-01

Nickel nanowires have successfully been fabricated through a simple liquid reduction in ethylene glycol medium with a 0.3T magnetic field applied. The effect of uniform magnetic field and solvent on the morphology and the crystal structure of magnetic nickel were studied. Scanning electron microscope images and transmission electron scope images s how that the effect of the external magnetic field on the morphology of nickel nanowires. X-ray diffraction shows the crystal structure of as-prepared products. And a energy disperse spectroscopy and a vibrating sample magnetometer are used to analyze the composition and static magnetic properties. The results show that the straight wires with an average diameter of about 100 nm and a length of several microns were obtained and mainly composed by fcc structure in the solvent of ethylene glycol. Magnetic measurements show that the saturation magnetization of the as-obtained products in a 0.3 T external magnetic field is 36 emu/g, less than that of bulk nickel crystal, and the coercivity of them is 186 emu/g, larger than that of bulk crystal with the mole ratio of sodium borohydride to nickel sulfate is 1:1000. This kind of nanowires array has potential applications with the special one-dimensional structures.

Improved thermoelectric properties of Bi2Te3-xSex alloys by melt spinning and resistance pressing sintering

NASA Astrophysics Data System (ADS)

Cai, Xinzhi; Fan, Xi'an; Rong, Zhenzhou; Yang, Fan; Gan, Zhanghua; Li, Guangqiang

2014-03-01

Starting from bismuth, tellurium and selenium chunks, n-type Bi2Te3-xSex (x ⩽ 0.3) alloys were obtained by melt spinning (MS) combined with a resistance pressing sintering (RPS) process. The phases, microstructures and compositions of the samples were evaluated by x-ray diffraction, field emission scanning electron microscopy, and energy dispersive x-ray spectroscopy during each step in the preparation process, respectively. The influences of Se doping, MS and RPS processes on the thermoelectric (TE) properties of Bi2Te3-xSex alloys were investigated in detail. The Bi2Te3-xSex powders could be well compacted by the RPS process and the relative densities of the bulks prepared by RPS were all higher than 96%. The partially oriented lamellar structure could be observed at some regions of the samples prepared by RPS, and the monolayer thickness of the lamellar structure in the MS-RPS samples was smaller than that in the smelting-RPS sample. The MS process was confirmed as an excellent method to obtain fine microstructures and low lattice thermal conductivity for the TE materials. All evidence about electrical and thermal transport properties suggested that suitably increasing the Se content could effectively improve the ZT value. The maximum ZT value of 0.84 was obtained for the Bi2Te2.7Se0.3 prepared by MS-RPS at 423 K. As opposed to the conventional hot pressing and spark plasma sintering, the RPS method introduced here is more suitable for practical industrial application due to its cost saving and high efficiency.

A review on preparation of silver nano-particles

NASA Astrophysics Data System (ADS)

Haider, Adawiya J.; Haider, Mohammad J.; Mehde, Mohammad S.

2018-05-01

The term "nano particle" (NP) refers to particle diameter in nanometers in size. Nanoparticles contain a small number of constituent atoms or molecules that differ from the properties inherent in their bulk counterparts, found in various forms such as spherical, triangular, cubic, pentagonal, rod-shaped, shells, elliptical and so on. In this chapter, it has been presented the theoretical concepts of the preparation of AgNPS as powders and collide nanoparticles, techniques of preparation with their characterization (morphology, sign charge and potential value, particle distribution ….etc.). Also, included unique properties of AgNPS that are different from those of their bulk materials like: High surface area to volume ratio effects Quantization of electronic and vibration properties.

New insights on the synthesis and electronic transport in bulk polycrystalline Pr-doped SrTiO3-δ

NASA Astrophysics Data System (ADS)

Dehkordi, Arash Mehdizadeh; Bhattacharya, Sriparna; Darroudi, Taghi; Alshareef, Husam N.; Tritt, Terry M.

2015-02-01

Recently, we have reported a significant enhancement in the electronic and thermoelectric properties of bulk polycrystalline SrTiO3 ceramics via praseodymium doping. This improvement was originated from the simultaneous enhancement in the thermoelectric power factor and reduction in thermal conductivity, which was contributed to the non-uniform distribution of Pr dopants. In order to further understand the underlying mechanism, we herein investigate the role of praseodymium doping source (Pr2O3 versus Pr6O11) on the synthesis and electronic transport in Pr-doped SrTiO3 ceramics. It was observed that the high-temperature electronic transport properties are independent of the choice of praseodymium doping source for samples prepared following our synthesis strategy. Theoretical calculations were also performed in order to estimate the maximum achievable power factor and the corresponding optimal carrier concentration. The result suggests the possibility of further improvement of the power factor. This study should shed some light on the superior electronic transport in bulk polycrystalline Pr-doped SrTiO3 ceramics and provide new insight on further improvement of the thermoelectric power factor.

Impact of Pb content on the physical parameters of Se-Te-Pb system

DOE Office of Scientific and Technical Information (OSTI.GOV)

Anjali,; Sharma, Raman; Thakur, Nagesh

2015-05-15

In the present study, we have investigated the impact of Pb content on the physical parameters in Se-Te-Pb system via average coordination number, constraints, the fraction of floppy modes, cross-linking density, lone pairs electrons, heat of atomization, mean bond energy, cohesive energy and electronegativity. The bulk samples have been prepared by using melt quenching technique. X-ray diffraction pattern of various samples indicates the amorphous nature of investigated glassy alloys. It is observed that average coordination number, average number of constraints and cross-linking density increase with Pb content. However, lone-pair electrons, floppy modes, average heat of atomization, cohesive energy and meanmore » bond energy are found to decrease with Pb atomic percentage.« less

Study of the superconducting properties of the Bi-Ca-Sr-Cu-O system

NASA Technical Reports Server (NTRS)

Khan, Musheer H.; Naqvi, S. M. M. R.; Zia-Ul-haq, S. M.

1991-01-01

High Temperature Superconductivity in the Bi-Ca-Sr-Cu-O System has been observed and has attracted considerable attention in 1988. The 80 K superconductivity phase has been identified to have a composition of Bi2CaSr2Cu2Ox, while the 110 K phase as reported in the literature has a possible composition of Bi2Ca2Sr2Cu3O(x). Researchers present here a study of the electrical properties of bulk samples of the slowly cooled and rapidly quenched 2:1:2:2 system. The samples used in this study were prepared from appropriate amounts of Bi2O3, CuO, SrCO3, CaCO3.

Flower-like nanostructure MNb{sub 2}O{sub 6} (M = Mn, Zn) with high surface area: Hydrothermal synthesis and enhanced photocatalytic performance

DOE Office of Scientific and Technical Information (OSTI.GOV)

Huang, Xue; Jing, Yan; Yang, Jia

Graphical abstract: - Highlights: • MNb{sub 2}O{sub 6} was prepared by a mild two-step hydrothermal method. • Their flower-like nanostructure morphology was studied by SEM and TEM. • High BET surface areas for MnNb{sub 2}O{sub 6} (∼50 m{sup 2}/g) and ZnNb{sub 2}O{sub 6} (∼100 m{sup 2}/g). • Band gap energies were estimated by UV–vis diffuse reflectance spectra. • Photocatalytic activities were evaluated under UV-light irradiation. - Abstract: Nano-scaled MNb{sub 2}O{sub 6} (M = Mn, Zn) was successfully synthesized via a two-step hydrothermal method. It is important to control the exact pH of the reaction solution in order to obtain puremore » products. The as-prepared samples both crystallize in the columbite structure. Interestingly, the products possess a flower-like morphology in a pseudo-six-fold symmetry, which is in fact arrayed by two-dimensional nanosheets. Their surface areas (51 m{sup 2}/g for MnNb{sub 2}O{sub 6} and 103 m{sup 2}/g for ZnNb{sub 2}O{sub 6}) are about 25–50 times of those prepared by solid state reaction. UV–vis diffuse reflectance spectra show the nano-scaled sample has a stronger absorption and a narrower band gap than its bulk form. The estimated band gap energies are 2.70 eV (MnNb{sub 2}O{sub 6}) and 3.77 eV (ZnNb{sub 2}O{sub 6}), respectively. The nano-scaled ZnNb{sub 2}O{sub 6} exhibits a double enhancement of photocatalytic activity in the decolorization of methylene blue than bulk ZnNb{sub 2}O{sub 6}.« less

Effect of resin infiltration on the thermal and mechanical properties of nano-sized silica-based thermal insulation.

PubMed

Lee, Jae Chun; Kim, Yun-Il; Lee, Dong-Hun; Kim, Won-Jun; Park, Sung; Lee, Dong Bok

2011-08-01

Several kinds of nano-sized silica-based thermal insulation were prepared by dry processing of mixtures consisting of fumed silica, ceramic fiber, and a SiC opacifier. Infiltration of phenolic resin solution into the insulation, followed by hot-pressing, was attempted to improve the mechanical strength of the insulation. More than 22% resin content was necessary to increase the strength of the insulation by a factor of two or more. The structural integrity of the resin-infiltrated samples could be maintained, even after resin burn-out, presumably due to reinforcement from ceramic fibers. For all temperature ranges and similar sample bulk density values, the thermal conductivities of the samples after resin burn-out were consistently higher than those of the samples obtained from the dry process. Mercury intrusion curves indicated that the median size of the nanopores formed by primary silica aggregates in the samples after resin burn-out is consistently larger than that of the sample without resin infiltration.

Bulk Thermoelectric Materials Reinforced with SiC Whiskers

NASA Astrophysics Data System (ADS)

Akao, Takahiro; Fujiwara, Yuya; Tarui, Yuki; Onda, Tetsuhiko; Chen, Zhong-Chun

2014-06-01

SiC whiskers have been incorporated into Zn4Sb3 compound as reinforcements to overcome its extremely brittle nature. The bulk samples were prepared by either hot-extrusion or hot-pressing techniques. The obtained products containing 1 vol.% to 5 vol.% SiC whiskers were confirmed to exhibit sound appearance, high density, and fine-grained microstructure. Mechanical properties such as the hardness and fracture resistance were improved by the addition of SiC whiskers, as a result of dispersion strengthening and microstructural refinement induced by a pinning effect. Furthermore, crack deflection and/or bridging/pullout mechanisms are invoked by the whiskers. Regarding the thermoelectric properties, the Seebeck coefficient and electrical resistivity values comparable to those of the pure compound are retained over the entire range of added whisker amount. However, the thermal conductivity becomes large with increasing amount of SiC whiskers because of the much higher conductivity of SiC relative to the Zn4Sb3 matrix. This results in a remarkable degradation of the dimensionless figure of merit in the samples with addition of SiC whiskers. Therefore, the optimum amount of SiC whiskers in the Zn4Sb3 matrix should be determined by balancing the mechanical properties and thermoelectric performance.

Sample sizes to control error estimates in determining soil bulk density in California forest soils

Treesearch

Youzhi Han; Jianwei Zhang; Kim G. Mattson; Weidong Zhang; Thomas A. Weber

2016-01-01

Characterizing forest soil properties with high variability is challenging, sometimes requiring large numbers of soil samples. Soil bulk density is a standard variable needed along with element concentrations to calculate nutrient pools. This study aimed to determine the optimal sample size, the number of observation (n), for predicting the soil bulk density with a...

Effects of inoculum type and bulk dissolved oxygen concentration on achieving partial nitrification by entrapped-cell-based reactors.

PubMed

Rongsayamanont, Chaiwat; Limpiyakorn, Tawan; Khan, Eakalak

2014-07-01

An entrapment of nitrifiers into gel matrix is employed as a tool to fulfill partial nitrification under non-limiting dissolved oxygen (DO) concentrations in bulk solutions. This study aims to clarify which of these two attributes, inoculum type and DO concentration in bulk solutions, is the decisive factor for partial nitrification in an entrapped-cell based system. Four polyvinyl alcohol entrapped inocula were prepared to have different proportions of nitrite-oxidizing bacteria (NOB) and nitrite-oxidizing activity. At a DO concentration of 3 mg l(-1), the number of active NOB cells in an inoculum was the decisive factor for partial nitrification enhancement. However, when the DO concentration was reduced to 2 mg l(-1), all entrapped cell inocula showed similar degrees of partial nitrification. The results suggested that with the lower bulk DO concentration, the preparation of entrapped cell inocula is not useful as the DO level becomes the decisive factor for achieving partial nitrification. Copyright © 2014 Elsevier Ltd. All rights reserved.

Preparation of Y-Ba-Cu oxide superconductor thin films using pulsed laser evaporation from high T/sub c/ bulk material

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dijkkamp, D.; Venkatesan, T.; Wu, X.D.

We report the first successful preparation of thin films of Y-Ba-Cu-O superconductors using pulsed excimer laser evaporation of a single bulk material target in vacuum. Rutherford backscattering spectrometry showed the composition of these films to be close to that of the bulk material. Growth rates were typically 0.1 nm per laser shot. After an annealing treatment in oxygen the films exhibited superconductivity with an onset at 95 K and zero resistance at 85 and 75 K on SrTiO/sub 3/ and Al/sub 2/O/sub 3/ substrates, respectively. This new deposition method is relatively simple, very versatile, and does not require the usemore » of ultrahigh vacuum techniques.« less

The miniaturized Raman system and detection of traces of life in halite from the Atacama Desert: some considerations for the search for life signatures on Mars.

PubMed

Vítek, Petr; Jehlička, Jan; Edwards, Howell G M; Hutchinson, Ian; Ascaso, Carmen; Wierzchos, Jacek

2012-12-01

Raman spectroscopy is being adopted as a nondestructive instrumentation for the robotic exploration of Mars to search for traces of life in the geological record. Here, miniaturized Raman spectrometers of two different types equipped with 532 and 785 nm lasers for excitation, respectively, were compared for the detection of microbial biomarkers in natural halite from the hyperarid region of the Atacama Desert. Measurements were performed directly on the rock as well as on the homogenized, powdered samples prepared from this material-the effects of this sample preparation and the excitation wavelength employed in the analysis are compared and discussed. From these results, 532 nm excitation was found to be superior for the analysis of powdered specimens due to its high sensitivity toward carotenoids and hence a higher capability for their detection at relatively low concentration in bulk powdered specimens. For the same reason, this wavelength was a better choice for the detection of carotenoids in direct measurements made on the rock samples. The 785 nm excitation wavelength, in contrast, proved to be more sensitive toward the detection of scytonemin.

Influence of CeO2 addition on the preparation of foamed glass-ceramics from high-titanium blast furnace slag

NASA Astrophysics Data System (ADS)

Zhou, Hong-ling; Feng, Ke-qin; Chen, Chang-hong; Yan, Zi-di

2018-06-01

Foamed glass-ceramics doped with cerium oxide (CeO2) were successfully prepared from high-titanium blast furnace slag by one-step sintering. The influence of CeO2 addition (1.5wt%-3.5wt%) on the crystalline phases, microstructure, and properties of foamed glass-ceramics was studied. Results show that CeO2 improves the stability of the glass phase and changes the two-dimensional crystallization mechanism into three-dimensional one. XRD analysis indicates the presence of Ca(Mg, Fe)Si2O6 and Ca(Ti, Mg, Al)(Si, Al)2O6 in all sintered samples. Added with CeO2, TiCeO4 precipitates, and crystallinity increases, leading to increased thickness of pore walls and uniform pores. The comprehensive properties of foamed glass-ceramics are better than that of samples without CeO2. In particular, the sample added with a suitable amount of CeO2 (2.5wt%) exhibits bulk density that is similar to and compressive strength (14.9 MPa) that is more than twice of foamed glass-ceramics without CeO2.

Shear wave EMAT thickness measurements of low carbon steel at 450 °C without cooling

NASA Astrophysics Data System (ADS)

Lunn, Natasha; Potter, Mark; Dixon, Steve

2017-02-01

Performing high temperature online inspection without plant shutdown is highly desirable, yet, development of portable or permanently installed high temperature ultrasonic sensors, without the need for sample surface preparation, remains a key challenge. Low carbon steel pipelines operating at elevated temperatures often develop a magnetostrictive oxide coating (magnetite), which improves electromagnetic acoustic transducer (EMAT) efficiency below the Curie temperature of magnetite (575 °C), via a magnetostrictive mechanism. Coupling the inherent non-contacting nature of EMATs with the enhanced efficiency from a magnetite coating, we are able to continuously operate an uncoded EMAT at elevated temperatures without permanent installation or surface preparation. In this work, a high temperature shear wave EMAT utilizing a high field, high Curie point, permanent magnet has been developed to generate ultrasonic bulk thickness measurements on magnetite coated steel at temperatures of up to 450 °C, without cooling. Relatively high signal-to-noise ratios, in the region of 30 dB for single shot data, have been measured at 450 °C using this technique. The EMAT design and results from high temperature trials, including the performance with change in temperature, sample thickness and EMAT-sample lift-off, are presented here.

Examining the Magnetic Properties of LaCoO3 Thin Films Using Magnetic Force Microscopy

NASA Astrophysics Data System (ADS)

Berg, Morgann; Posadas, Agham; de Lozanne, Alex; Demkov, Alexander

2011-03-01

In contrast to the non-magnetic ground state of bulk LaCo O3 (LCO) at low temperatures, ferromagnetism has been observed in elastically strained thin film specimens. The origins of ferromagnetism in strained LCO thin films have been obscured by conflicting experimental results. Pulsed laser deposition (PLD) is the current standard of preparation techniques used to grow thin films of LCO, but results from thin film LCO samples prepared by PLD have been questioned on the basis of chemical inhomogeneity and film defects. Using magnetic force microscopy, we investigate the microscale magnetic properties of strained thin films of LCO prepared by molecular beam epitaxy and deposited on lanthanum aluminate and strontium titanate substrates. We observe these properties across a temperature range surrounding the Curie temperature (Tc ~ 80 K) and compare our results to global magnetic characteristics of these films as measured by a SQUID magnetometer. Supported by NSF-DMR and NSF-IGERT.

A Surface Plasmon Resonance-Based Optical Fiber Probe Fabricated with Electropolymerized Molecular Imprinting Film for Melamine Detection

PubMed Central

Zheng, Yongping; Zhang, Tingwei; Wu, Songjie; Zhang, Jue; Fang, Jing

2018-01-01

Molecularly imprinted polymer (MIP) films prepared by bulk polymerization suffer from numerous deficiencies, including poor mass transfer ability and difficulty in controlling reaction rate and film thickness, which usually result in poor repeatability. However, polymer film synthesized by electropolymerization methods benefit from high reproducibility, simplicity and rapidity of preparation. In the present study, an Au film served as the refractive index-sensitive metal film to couple with the light leaked out from optical fiber core and the electrode for electropolymerizing MIP film simultaneously. The manufactured probe exhibited satisfactory sensitivity and specificity. Furthermore, the surface morphology and functional groups of the synthesized MIP film were characterized by Atomic Force Microscopy (AFM) and Fourier transform infrared microspectroscopy (FTIR) for further insights into the adsorption and desorption processes. Given the low cost, label-free test, simple preparation process and fast response, this method has a potential application to monitor substances in complicated real samples for out-of-lab test in the future. PMID:29522472

Very high frequency (beyond 100 MHz) PZT kerfless linear arrays.

PubMed

Wu, Da-Wei; Zhou, Qifa; Geng, Xuecang; Liu, Chang-Geng; Djuth, Frank; Shung, K Kirk

2009-10-01

This paper presents the design, fabrication, and measurements of very high frequency kerfless linear arrays prepared from PZT film and PZT bulk material. A 12-microm PZT thick film fabricated from PZT-5H powder/solution composite and a piece of 15-microm PZT-5H sheet were used to fabricate 32-element kerfless high-frequency linear arrays with photolithography. The PZT thick film was prepared by spin-coating of PZT sol-gel composite solution. The thin PZT-5H sheet sample was prepared by lapping a PZT-5H ceramic with a precision lapping machine. The measured results of the 2 arrays were compared. The PZT film array had a center frequency of 120 MHz, a bandwidth of 60% with a parylene matching layer, and an insertion loss of 41 dB. The PZT ceramic sheet array was found to have a center frequency of 128 MHz with a poorer bandwidth (40% with a parylene matching layer) but a better sensitivity (28 dB insertion loss).

Very High Frequency (Beyond 100 MHz) PZT Kerfless Linear Arrays

PubMed Central

Wu, Da-Wei; Zhou, Qifa; Geng, Xuecang; Liu, Chang-Geng; Djuth, Frank; Shung, K. Kirk

2010-01-01

This paper presents the design, fabrication, and measurements of very high frequency kerfless linear arrays prepared from PZT film and PZT bulk material. A 12-µm PZT thick film fabricated from PZT-5H powder/solution composite and a piece of 15-µm PZT-5H sheet were used to fabricate 32-element kerfless high-frequency linear arrays with photolithography. The PZT thick film was prepared by spin-coating of PZT sol-gel composite solution. The thin PZT-5H sheet sample was prepared by lapping a PZT-5H ceramic with a precision lapping machine. The measured results of the 2 arrays were compared. The PZT film array had a center frequency of 120 MHz, a bandwidth of 60% with a parylene matching layer, and an insertion loss of 41 dB. The PZT ceramic sheet array was found to have a center frequency of 128 MHz with a poorer bandwidth (40% with a parylene matching layer) but a better sensitivity (28 dB insertion loss). PMID:19942516

Momentum microscopy of ? single crystals with detailed surface characterisation

NASA Astrophysics Data System (ADS)

Ellguth, M.; Tusche, C.; Iga, F.; Suga, S.

2016-11-01

We report the in situ preparation of surfaces of the proposed topological Kondo insulator SmB? by controlled cycles of Ar ion sputtering and annealing. The procedure provides a reproducible way for the preparation of Sm- or B-rich surface terminations by low (?1080 ?C) or high (?1200 ?C) temperature annealing. The surface quality and termination were checked by low energy electron diffraction and Auger electron spectroscopy. Photoemission studies were carried out using momentum microscopy and two laboratory light sources providing polarised radiation with an energy of 6 eV (fourth harmonic of a pulsed Ti:Sapphire laser) and unpolarised radiation with an energy of 21.2 eV (He-I line of a gas discharge lamp). Full dispersions of electronic states in a wide two-dimensional momentum space were obtained by momentum microscopy from the in situ prepared Sm-terminated surface. The shape of the Fermi surface is discussed based on the sections through the bulk Brillouin zone sampled by the different photon energies.

Sample Curation in Support of the OSIRIS-REx Asteroid Sample Return Mission

NASA Technical Reports Server (NTRS)

Righter, Kevin; Nakamura-Messenger, Keiko

2017-01-01

The OSIRIS-REx asteroid sample return mission launched to asteroid Bennu Sept. 8, 2016. The spacecraft will arrive at Bennu in late 2019, orbit and map the asteroid, and perform a touch and go (TAG) sampling maneuver in July 2020. After sample is stowed and confirmed the spacecraft will return to Earth, and the sample return capsule (SRC) will land in Utah in September 2023. Samples will be recovered from Utah [2] and then transported and stored in a new sample cleanroom at NASA Johnson Space Center in Houston [3]. The materials curated for the mission are described here. a) Materials Archive and Witness Plate Collection: The SRC and TAGSAM were built between March 2014 and Summer of 2015, and instruments (OTES,OVIRS, OLA, OCAMS, REXIS) were integrated from Summer 2015 until May 2016. A total of 395 items were received for the materials archive at NASA-JSC, with archiving finishing 30 days after launch (with the final archived items being related to launch operations)[4]. The materials fall into several general categories including metals (stainless steel, aluminum, titanium alloys, brass and BeCu alloy), epoxies, paints, polymers, lubricants, non-volatile-residue samples (NVR), sapphire, and various miscellaneous materials. All through the ATLO process (from March 2015 until late August 2016) contamination knowledge witness plates (Si wafer and Al foil) were deployed in the various cleanrooms in Denver and KSC to provide an additional record of particle counts and volatiles that is archived for current and future scientific studies. These plates were deployed in roughly monthly increments with each unit containing 4 Si wafers and 4 Al foils. We archived 128 individual witness plates (64 Si wafers and 64 Al foils); one of each witness plate (Si and Al) was analyzed immediately by the science team after archiving, while the remaining 3 of each are archived indefinitely. Information about each material archived is stored in an extensive database at NASA-JSC, and key summary information for each will be presented in an online catalog. b) Bulk Asteroid sample: The Touch and Go Sampling Mechanism (TAGSAM) head will contain up to 1.5 kg of asteroid material. Upon return to Earth, the TAGSAM head with the sample canister will be subjected to a nitrogen purge and then opened in a nitrogen cabinet in Houston. Once the TAGSAM head is removed from the canister, it will be dis-assembled slowly and carefully under nitrogen until the sample can be removed for processing in a dedicated nitrogen glovebox. Bennu surface samples are expected to be sub-cm sized, based on thermal infrared and radar polarization ratio measurements [1]. The upper limit on material collected by the TAGSAM head is 2 cm. Therefore, we will be prepared to handle, subdivide, and characterize materials of a wide grain size (from 10 ?m to 2 cm), and for both organic (UV fluorescence) and inorganic (SEM, FTIR, optical) properties. Representative portions of the bulk sample will be prepared for JAXA (0.5 %; see also [5]) and Canadian Space Agency (4%), with the remaining divided between the science team (<25%) and archived for future studies (NASA) (>75%). c) Contact Pad samples: The base of the TAGSAM head contains 24 contact pads that are designed to trap the upper surface layer of material and thus offer an opportunity to study asteroid samples that have resided at the very top surface of the regolith. Asteroid material is trapped on the pads in spring steel Velcro hooks, and material will have to be removed from these pads by curation specialists in the lab. d) Hardware: Some canister and SRC hardware items will contain information that will be important to understanding the collected samples, including the canister gas filter, temperature strips, flight witness plates, and the TAGSAM and canister parts that might have adhering dust grains. Some challenges remaining for both bulk sample and contact pad samples include: i) working with intermediate size range (200 to 500 micron) samples - a size range NASA has not previously worked in such detail; ii) techniques for removal of contact pad material from the spring steel hooks, iii) static electrical effects of dust sized particles during sample handling and curation is likely to be significant, and iv) the TAGSAM head and associated canister hardware will undoubtedly be coated with fine adhering dust grains from Bennu. In the case of collection of a large bulk sample mass, the adhering dust grains may be of lower priority. If a small sample mass is returned, the adhering dust may attain a higher priority, so recovery of adhering dust grains is an additional challenge to consider. In the year leading up to sample return we plan a variety of sample handling rehearsals that will enables the curation team to be prepared for many new aspects posed by this sample suite.

Enhanced magnetization in morphologically and magnetically distinct BiFeO3 and La0.7Sr0.3MnO3 composites

NASA Astrophysics Data System (ADS)

Pillai, Shreeja; Reshi, Hilal Ahmad; Bagwaiya, Toshi; Banerjee, Alok; Shelke, Vilas

2017-09-01

Nanomaterials exhibit properties different from those of their bulk counterparts. The modified magnetic characteristics of manganite nanoparticles were exploited to improve magnetization in multiferroic BiFeO3 compound. We studied the composite of two morphologically and magnetically distinct compounds BiFeO3 (BFO) and La0.7Sr0.3MnO3 (LSMO). The microcrystalline BiFeO3 sample was prepared by solid state reaction method and the nanocrystalline La0.7Sr0.3MnO3 by sol-gel method. Composites with nominal compositions (1-x)BiFeO3-(x)La0.7Sr0.3MnO3 were prepared by modified solid state reaction method. The phase purity and crystal structures were checked by using X-ray diffraction. The formation of composites with phase separated BFO and LSMO was confirmed using Raman and Fourier Transform Infrared spectroscopy studies. The composite samples showed relatively high value of magnetization with finite coercivity. This improvement in magnetic behavior is ascribed to the coexistence of multiple magnetic orderings in composite samples. We scrutinized the possibility of oxygen vacancy or Fe mixed valency formation in the samples using X-ray photoelectron spectroscopy technique.

Recent developments in melt processed Gd-123 and MgB2 materials at RTRI

NASA Astrophysics Data System (ADS)

Muralidhar, M.; Fukumoto, Y.; Ishihara, A.; Suzuki, K.; Tomita, M.; Koblischka, M. R.; Yamamoto, A.; Kishio, K.

2014-01-01

In this contribution we will report on the current status, recent developments in GdBa2Cu3Oy "Gd-123" and MgB2 material processing, characterization, and applications at the Railway Technical Research Institute (RTRI). Batch-processing of Gd-123 bulk material grown in air was performed using novel thin film Nd-123 seeds grown on MgO crystals. In this way, we are able to fabricate materials with good quality, and uniform performance. We examined the technology of the uniform performance of the large 45 mm diameter, single grain Gd-123 bulks for use in application of NMR. For this purpose, four 5 mm thick pieces are cut vertically from a single grain Gd-123 material and the magnetic field distribution is measured using a scanning hall sensor. We found that all four pieces are single domain and exhibit a quite uniform field distribution. Furthermore, the batch-processed bulk materials are used for the construction of a chilled Maglev vehicle. On the other hand, to optimize the trapped field performance of bulk MgB2 material, several samples were prepared by solid state reaction at different temperatures ranging from 750 to 950 °C in pure argon atmosphere. X-ray diffraction results indicated that single phase and homogenous MgB2 bulks are produced when sintering them around 775 °C. Further, atomic force microscopy (AFM) and scanning electron microscopy (SEM) indicated that an uniform grain size results by controlling the processing temperature. So, higher trapped fields can be achieved in sintered MgB2 material.

Effect of annealing and In content on the properties of electron beam evaporated ZnO films

NASA Astrophysics Data System (ADS)

Mohamed, S. H.; Ali, H. M.; Mohamed, H. A.; Salem, A. M.

2005-08-01

The effect of both annealing and In content on the properties of ZnO films prepared by electron beam evaporation were investigated. The evaporation was carried out at room temperature from bulk samples prepared by sintering technique. X-ray diffraction showed that the structure of ZnO-In{2}O{3} films depends on both the In content and annealing temperature. Amorphous, highly transparent and relatively low resistive films which can be suitable for the usage as transparent electrode of organic light-emitting diode were obtained upon annealing at 300 circC. Partially crystalline, highly transparent and highly resistive films which can be used in piezoelectric applications were obtained upon annealing at 500 circC. For each composition the refractive index has no monotonic variation upon increasing annealing temperature.

Non-noble catalysts and catalyst supports for phosphoric acid fuel cells

NASA Technical Reports Server (NTRS)

Mcalister, A. J.

1981-01-01

Four different samples of the cubic alloys W sub x-1 Ti sub x C sub 1-y were prepared and found to be active and CO tolerant. When the activities of these cubic alloys were weighted by the reciprocal of the square of the W exchange, they displayed magnitudes and dependence on bulk C deficiency comparable to those of highly active forms of WC. It is concluded that they may offer important insight into the nature of the active sites on, and means for improving the performance of, W-C anode catalysts for use in phosphoric acid fuel cells.

Electronic and magnetic properties of epitaxial SrRh O 3 films

DOE PAGES

Nichols, John A.; Yuk, Simuck F.; Sohn, Changhee; ...

2017-06-16

The strong interplay of fundamental order parameters in complex oxides is known to give rise to exotic physical phenomena. The 4$d$ transition-metal oxide SrRh O 3 has generated much interest, but advances have been hindered by difficulties in preparing single-crystalline phases. Here we epitaxially stabilize high-quality single-crystalline SrRh O 3 films and investigate their structural, electronic, and magnetic properties. Lastly, we determine that their properties significantly differ from the paramagnetic metallic ground state that governs bulk samples and are strongly related to rotations of Rh O 6 octahedra.

Photocatalytic Degradation of Isopropanol Over PbSnO3Nanostructures Under Visible Light Irradiation

PubMed Central

2009-01-01

Nanostructured PbSnO3photocatalysts with particulate and tubular morphologies have been synthesized from a simple hydrothermal process. As-prepared samples were characterized by X-ray diffraction, Brunauer–Emmet–Teller surface area, transmission electron microscopy, and diffraction spectroscopy. The photoactivities of the PbSnO3nanostructures for isopropanol (IPA) degradation under visible light irradiation were investigated systematically, and the results revealed that these nanostructures show much higher photocatalytic properties than bulk PbSnO3material. The possible growth mechanism of tubular PbSnO3catalyst was also investigated briefly. PMID:20596379

Technical issues of a high-Tc superconducting bulk magnet

NASA Astrophysics Data System (ADS)

Fujimoto, Hiroyuki

2000-06-01

Superconducting magnets made of high-Tc superconductors are promising for industrial applications. It is well known that REBa2Cu3O7-x superconductors prepared by melt processes have a high critical current density, Jc, at 77 K and high magnetic fields. The materials are very promising for high magnetic field applications as a superconducting permanent/bulk magnet with liquid-nitrogen refrigeration. Light rare-earth (LRE) BaCuO bulks, compared with REBaCuO bulks, exhibit a larger Jc in high magnetic fields and a much improved irreversibility field, Hirr, at 77 K. In this study, we discuss technical issues of a high-Tc superconducting bulk magnet, namely the aspects of the melt processing for bulk superconductors, their characteristic superconducting properties and mechanical properties, and trapped field properties of a superconducting bulk magnet. One of the possible applications is a superconducting bulk magnet for the magnetically levitated (Maglev) train in the future.

Spectroscopic and Mechanical Properties of a New Generation of Bulk Fill Composites

PubMed Central

Monterubbianesi, Riccardo; Orsini, Giovanna; Tosi, Giorgio; Conti, Carla; Librando, Vito; Procaccini, Maurizio; Putignano, Angelo

2016-01-01

Objectives: The aims of this study were to in vitro evaluate the degree of conversion and the microhardness properties of five bulk fill resin composites; in addition, the performance of two curing lamps, used for composites polymerization, was also analyzed. Materials and Methods: The following five resin-based bulk fill composites were tested: SureFil SDR®, Fill Up!™, Filtek™, SonicFill™, and SonicFill2™. Samples of 4 mm in thickness were prepared using Teflon molds filled in one increment and light-polymerized using two LED power units. Ten samples for each composite were cured using Elipar S10 and 10 using Demi Ultra. Additional samples of SonicFill2, (3 and 5 mm-thick) were also tested. The degree of conversion (DC) was determined by Raman spectroscopy, while the Vickers microhardness (VMH) was evaluated using a microhardness tester. The experimental evaluation was carried out on top and bottom sides, immediately after curing (t0), and, on bottom, after 24 h (t24). Two-ways analysis of variance was applied to evaluate DC and VMH-values. In all analyses, the level of significance was set at p < 0.05. Results: All bulk fill resin composites recorded satisfactory DCs on top and bottom sides. At t0, the top of SDR and SonicFill2 showed the highest DCs-values (85.56 ± 9.52 and 85.47 ± 1.90, respectively), when cured using Elipar S10; using Demi Ultra, SonicFill2 showed the highest DCs-values (90.53 ± 2.18). At t0, the highest DCs-values of bottom sides were recorded by SDR (84.64 ± 11.68), when cured using Elipar S10, and Filtek (81.52 ± 4.14), using Demi Ultra. On top sides, Demi Ultra lamp showed significant higher DCs compared to the Elipar S10 (p < 0.05). SonicFill2 reached suitable DCs also on bottom of 5 mm-thick samples. At t0, VMH-values ranged between 24.4 and 69.18 for Elipar S10, and between 26.5 and 67.3 for Demi Ultra. Using both lamps, the lowest VMH-values were shown by SDR, while the highest values by SonicFill2. At t24, all DC and VMH values significantly increased. Conclusions: Differences in DC and VMH among materials are suggested to be material and curing lamp dependent. Even at t0, the three high viscosity bulk composites showed higher VMH than the flowable or dual curing composites. PMID:28082918

Spectroscopic and Mechanical Properties of a New Generation of Bulk Fill Composites.

PubMed

Monterubbianesi, Riccardo; Orsini, Giovanna; Tosi, Giorgio; Conti, Carla; Librando, Vito; Procaccini, Maurizio; Putignano, Angelo

2016-01-01

Objectives: The aims of this study were to in vitro evaluate the degree of conversion and the microhardness properties of five bulk fill resin composites; in addition, the performance of two curing lamps, used for composites polymerization, was also analyzed. Materials and Methods: The following five resin-based bulk fill composites were tested: SureFil SDR®, Fill Up!™, Filtek™, SonicFill™, and SonicFill2™. Samples of 4 mm in thickness were prepared using Teflon molds filled in one increment and light-polymerized using two LED power units. Ten samples for each composite were cured using Elipar S10 and 10 using Demi Ultra. Additional samples of SonicFill2, (3 and 5 mm-thick) were also tested. The degree of conversion (DC) was determined by Raman spectroscopy, while the Vickers microhardness (VMH) was evaluated using a microhardness tester. The experimental evaluation was carried out on top and bottom sides, immediately after curing (t0), and, on bottom, after 24 h (t24). Two-ways analysis of variance was applied to evaluate DC and VMH-values. In all analyses, the level of significance was set at p < 0.05. Results: All bulk fill resin composites recorded satisfactory DCs on top and bottom sides. At t0, the top of SDR and SonicFill2 showed the highest DCs-values (85.56 ± 9.52 and 85.47 ± 1.90, respectively), when cured using Elipar S10; using Demi Ultra, SonicFill2 showed the highest DCs-values (90.53 ± 2.18). At t0, the highest DCs-values of bottom sides were recorded by SDR (84.64 ± 11.68), when cured using Elipar S10, and Filtek (81.52 ± 4.14), using Demi Ultra. On top sides, Demi Ultra lamp showed significant higher DCs compared to the Elipar S10 ( p < 0.05). SonicFill2 reached suitable DCs also on bottom of 5 mm-thick samples. At t0, VMH-values ranged between 24.4 and 69.18 for Elipar S10, and between 26.5 and 67.3 for Demi Ultra. Using both lamps, the lowest VMH-values were shown by SDR, while the highest values by SonicFill2. At t24, all DC and VMH values significantly increased. Conclusions: Differences in DC and VMH among materials are suggested to be material and curing lamp dependent. Even at t0, the three high viscosity bulk composites showed higher VMH than the flowable or dual curing composites.

Enhancement in magnetocaloric properties of ErCrO3 via A-site Gd substitution

NASA Astrophysics Data System (ADS)

Shi, Jianhang; Yin, Shiqi; Seehra, Mohindar S.; Jain, Menka

2018-05-01

Rare earth chromites (RCrO3) continue to be of considerable interest due to their intriguing physical properties such as spin-reorientation, multiferroicity, and magnetocaloric effect. In this paper, we compare the structural, magnetic, and magnetocaloric properties of bulk ErCrO3 with those of bulk Er0.33Gd0.67CrO3, the latter obtained by Gd substitution at the A-site (Er-site) and report substantial enhancement in the magnetocaloric response by Gd substitution. The samples prepared by the citrate route were structurally characterized at room temperature using x-ray diffraction (XRD), Raman spectroscopy, and scanning electron microscopy. The XRD measurements refined by Rietveld analysis indicate that both samples crystallized in the orthorhombically distorted perovskite structure with Pbnm space group. Magnetic measurements on both samples were carried out between 5 K and 300 K in magnetic fields up to 7 T and show that TNC r (where Cr3+ orders) for Er0.33Gd0.67CrO3 is enhanced to 155 K vs. 133 K for ErCrO3 with analogous changes in the other magnetic parameters. Isothermal magnetization M vs. H data at different temperatures were used to determine changes in the magnetic entropy ( -ΔS ) and relative cooling power (RCP) for the two samples showing considerable improvement with Gd substitution in bulk ErCrO3. The maximum value of -ΔS for Er0.33Gd0.67CrO3 is 27.6 J kg-1 K-1 at 5 K and 7 T with a RCP of 531.1 J kg-1, in comparison to maximum -ΔS = 10.7 J kg-1 K-1 at 15 K with an RCP of 416.4 J kg-1 for ErCrO3 at 7 T.

Effect of Surface Preparation and Gas Flow on Nitrogen Atom Surface Recombination

NASA Technical Reports Server (NTRS)

Prok, George M.

1961-01-01

The effects of surface preparation and gas flow on the recombination of nitrogen atoms at copper and platinum surfaces were determined. Atoms were generated by an electrodeless 2450-megacycle-per-second discharge, and their concentration was measured by gas-phase titration with nitric oxide. Test surfaces were either vacuum-evaporated films or spheres machined from bulk metal and cemented around small glass-bead thermistors. Heat released by recombination was measured as the difference in electrical energy required to maintain a given thermistor temperature with and without a catalytic surface exposed. Recombination coefficients measured at flow velocities of 1120, 1790, 2250, and 3460 centimeters per second and at pressures of 0.42 and 0.59 millimeter of mercury showed that flow conditions had no effect. The results were also independent of atom concentration. A rough indication of the temperature dependence was obtained; it was greater for copper than for platinum. Platinum films deposited on platinum or on glass had the same activity - about 3 percent of the atoms impinging recombined. With copper, however, the glass substrate greatly reduced the percent of atoms recombining over that of a bulk copper substrate where 4 percent of the impinging atoms recombined. This effect could be overcome by depositing a second film on top of the first. Bulk metal samples were subjected to various surface treatments including polishing, degreasing with a chlorinated hydrocarbon, washing with nitric acid, and rinsing with water. Polished, degreased platinum had low activity compared to an evaporated film, but nitric acid treatment made it equivalent. Polished, degreased copper was only slightly less active than a copper film; nitric acid etching decreased the activity still further, probably by preferentially exposing facets of low catalytic efficiency.

Transport properties of kA class QMG current limiting elements

NASA Astrophysics Data System (ADS)

Morita, M.; Miura, O.; Ito, D.

2001-09-01

In order to estimate the feasibility of a resistive type fault current limiter made of QMG, transport properties of QMG current limiting elements which can transport about 1 kA continuously in a superconducting state were studied. QMG is a rare earth based bulk superconductor that has high Jc properties and relatively high electrical resistivity in a normal state. Because of these properties, QMG is a promising bulk material for superconducting fault current limiter applications. A bar-shaped sample in which the cross-section and the effective length were 2.2×0.8 mm2 and 30 mm, respectively, was prepared. Bypass resistance of 7 mΩ was connected in parallel with the sample. A field assist mechanism that can apply a magnetic field of about 0.9 T to the sample was installed. A half cycle of AC current up to about 3 kA was applied to the samples at 77 K. In the case when applied current ( I) was less than 1000 A in a self-field, flux flow voltage was less than 0.5 mV. The n-value was about 6. In the applied field of 0.9 T, a rapid increase of voltage (quench) was observed around I=1820 A. The quench phenomena reproduced without degradation in the case of I>1820 A. From these results, it was found that QMG fault current elements can endure the thermal shock of the quench by the optimization of bypass resistance and the applied field.

Pulsed Laser Deposition of BaCe(sub 0.85)Y(sub 0.15)0(sub 3) FILMS

NASA Technical Reports Server (NTRS)

Dynys, F. W.; Sayir, A.

2006-01-01

Pulsed laser deposition has been used to grow nanostructured BaCe(sub 0.85)Y(sub 0.15)0(sub 3) films. The objective is to enhance protonic conduction by reduction of membrane thickness. Sintered samples and laser targets were prepared by sintering BaCe(sub 0.85)Y(sub 0.15)O(sub 3) powders derived by solid state synthesis. Films 2 to 6 m thick were deposited by KrF excimer laser on Si and porous Al2O3 substrates. Nanocrystalline films were fabricated at deposition temperatures of 600-800 C deg at O2 pressure of 30 mTorr and laser fluence of 1.2 J/cm square. Films were characterized by x-ray diffraction, scanning electron microscopy and electrical impedance spectroscopy. Dense single phase BaCe(sub 0.85)Y((sub 0.15) 0(sub 3) films with a columnar growth morphology is observed, preferred crystal growth was found to be dependent upon deposition temperature and substrate type. Electrical conductivity of bulk samples produced by solid state sintering and thin film samples were measured over a temperature range of 100 C deg to 900 C deg in moist argon. Electrical conduction of the fabricated films was 1 to 4 orders of magnitude lower than the sintered bulk samples. With respect to the film growth direction, activation energy for electrical conduction is 3 times higher in the perpendicular direction than the parallel direction.

The relationship between vickers microhardness and compressive strength of functional surface geopolymers

NASA Astrophysics Data System (ADS)

Subaer, Ekaputri, Januari Jaya; Fansuri, Hamzah; Abdullah, Mustafa Al Bakri

2017-09-01

An experimental study to investigate the relationship between Vickers microhardness and compressive strength of geopolymers made from metakaolin has been conducted. Samples were prepared by using metakaolin activated with a sodium silicate solution at a different ratio of Si to Al and Na to Al and cured at 70oC for one hour. The resulting geopolymers were stored in an open air for 28 days before conducting any measurement. Bulk density and apparent porosity of the samples were measured by using Archimedes's method. Vickers microhardness measurements were performed on a polished surface of geopolymers with a load ranging from 0.3 - 1.0 kg. The topographic of indented samples were examined by using scanning electron microscopy (SEM). Compressive strength of the resulting geopolymers was measured on the cylindrical samples with a ratio of height to the diameter was 2:1. The results showed that the molar ratios of geopolymers compositions play important roles in the magnitude of bulk density, porosity, Vickers's microhardness as well as the compressive strength. The porosity reduced exponentially the magnitude of the strength of geopolymers. It was found that the relationship between Vickers microhardness and compressive strength was linear. At the request of all authors and with the approval of the proceedings editor, article 020188 titled, "The relationship between vickers microhardness and compressive strength of functional surface geopolymers," is being retracted from the public record due to the fact that it is a duplication of article 020170 published in the same volume.

Application of GeO2 nanoparticle as electrically erasable memory and its photo catalytic behaviour

NASA Astrophysics Data System (ADS)

Seal, M.; Bose, N.; Mukherjee, S.

2018-06-01

Germanium oxide nanoparticle is synthesized from bulk GeO2 powder through hydrothermal technique. The structural characterization of the prepared sample is performed with x-ray Diffraction and Transmission Electron Microscope. From the PL emission spectra and x-ray photoelectron spectra, the existence of oxygen defects inside the sample is confirmed. Thermogravimetric (TG) analysis of the sample shows that there is no weight loss with increase in temperature instead of a very little weight gain. An estimation of Oxygen vacancy concentration is made from the amount of weight gain as measured during TG analysis. The sample is also characterized with PE loop tracer, which indicates that GeO2 nanoparticle is able to show hysteresis loop regarding variation of Polarization with electric field. Such phenomenon implies that the sample can be used as electrically erasable memory device. Further, GeO2 nanoparticle is also exploited as photo catalyst to degrade Methylene Blue (MB) solution in the presence of ultraviolet ray. This phenomenon is also explained with oxygen vacancy.

A comparative study of neutron activation analysis and proton-induced X-ray emission analysis for the determination of heavy metals in estuarine sediments

NASA Astrophysics Data System (ADS)

Randle, K.; Al-Jundi, J.; Mamas, C. J. V.; Sokhi, R. S.; Earwaker, L. G.

1993-06-01

Our work on heavy metals in the estuarine environment has involved the use of two multielement techniques: neutron activation analysis (NAA) and proton-induced X-ray emission (PIXE) analysis. As PIXE is essentially a surface analytical technique problems may arise due to sample inhomogeneity and surface roughness. In order to assess the contribution of these effects we have compared the results from PIXE analysis with those from a technique which analyzes a larger bulk sample rather than just the surface. An obvious method was NAA. A series of sediment samples containing particles of variable diameter were compared. Pellets containing a few mg of sediment were prepared from each sample and analyzed by the PIXE technique using both an absolute and a comparitive method. For INAA the rest of the sample was then irradiated with thermal neutrons and element concentrations determined from analyses of the subsequent gamma-ray spectrum. Results from the two methods are discussed.

Multiscale microstructures and improved thermoelectric performance of Mg2(Si0.4Sn0.6)Sbx solid solutions

NASA Astrophysics Data System (ADS)

Zhang, Xin; Liu, Hongliang; Li, Songhao; Zhang, Feipeng; Lu, Qingmei; Li, Jingfeng

2014-03-01

A series of Sb-doped Mg2(Si0.4Sn0.6)Sbx (0 ≤ x ≤ 0.025) solid solutions were prepared by an induction melting, Melt Spinning (MS) and Spark Plasma Sintering (SPS) method, namely the non-equilibrium technique MS-SPS, using bulks of Magnesium, Silicon, Tin, and Antimony as raw materials. The non-equilibrium technique generates the unique multiscale microstructures of samples containing micronscale grains and nanoscale precipitates, the multiscale microstructures remarkably make the lattice thermal conductivities decreased, particularly for samples with the nanoscale precipitates having the size of 10-20 nm. Meanwhile, Sb-doping greatly increased the electrical performance of samples. Consequently, the Sb-doping combined with the multiscale microstructures strategy remarkably improves the overall thermoelectric (TE) performance of Sb doped samples, and a high dimensionless figure of merit (ZT) value of up to 1.25 at 723 K is obtained with Mg2(Si0.4Sn0.6)Sb0.02 sample in a relatively wide temperature range.

Fabrication and Thermoelectric Properties of n-Type CoSb2.85Te0.15 Using Selective Laser Melting.

PubMed

Yan, Yonggao; Ke, Hongquan; Yang, Jihui; Uher, Ctirad; Tang, Xinfeng

2018-04-25

We report a nonequilibrium fabrication method of n-type CoSb 2.85 Te 0.15 skutterudites using selective laser melting (SLM) technology. A powder of CoSb 2.85 Te 0.15 was prepared by self-propagating high-temperature synthesis (SHS) and served as the raw material for the SLM process. The effect of SLM processing parameters such as the laser power and scanning speed on the quality of the forming CoSb 2.85 Te 0.15 thin layers was systematically analyzed, and the optimal processing window for SLM was determined. A brief postannealing at 450 °C for 4 h, following the SLM process, has resulted in a phase-pure CoSb 2.85 Te 0.15 bulk material deposited on a Ti substrate. The Seebeck coefficient of the annealed SLM prepared bulk material is close to that of the sample prepared by the traditional sintering method, and its maximum ZT value reached 0.56 at 823 K. Moreover, a Ti-Co-Sb ternary compound transition layer of about 70 μm in thickness was found at a dense interface between CoSb 2.85 Te 0.15 and the Ti substrate. The contact resistivity was measured as 37.1 μΩcm 2 . The results demonstrate that SLM, coupled with postannealing, can be used for fabrication of incongruently melting skutterudite compounds on heterogeneous substrates. This lays an important foundation for the follow-up research utilizing energy efficient SHS and SLM processes in rapid printing of thermoelectric modules.

49 CFR 178.1070 - Tear test.

Code of Federal Regulations, 2013 CFR

2013-10-01

... 49 Transportation 3 2013-10-01 2013-10-01 false Tear test. 178.1070 Section 178.1070... Containers § 178.1070 Tear test. (a) General. The tear test must be conducted for the qualification of all of Flexible Bulk Containers design types. (b) Special preparation for the tear test. Flexible Bulk Container...

49 CFR 173.24b - Additional general requirements for bulk packagings.

Code of Federal Regulations, 2010 CFR

2010-10-01

... packagings. 173.24b Section 173.24b Transportation Other Regulations Relating to Transportation PIPELINE AND... SHIPPERS-GENERAL REQUIREMENTS FOR SHIPMENTS AND PACKAGINGS Preparation of Hazardous Materials for Transportation § 173.24b Additional general requirements for bulk packagings. (a) Outage and filling limits. (1...

Single column comprehensive analysis of pharmaceutical preparations using dual-injection mixed-mode (ion-exchange and reversed-phase) and hydrophilic interaction liquid chromatography.

PubMed

Kazarian, Artaches A; Taylor, Mark R; Haddad, Paul R; Nesterenko, Pavel N; Paull, Brett

2013-12-01

The comprehensive separation and detection of hydrophobic and hydrophilic active pharmaceutical ingredients (APIs), their counter-ions (organic, inorganic) and excipients, using a single mixed-mode chromatographic column, and a dual injection approach is presented. Using a mixed-mode Thermo Fisher Acclaim Trinity P1 column, APIs, their counter-ions and possible degradants were first separated using a combination of anion-exchange, cation-exchange and hydrophobic interactions, using a mobile phase consisting of a dual organic modifier/salt concentration gradient. A complementary method was also developed using the same column for the separation of hydrophilic bulk excipients, using hydrophilic interaction liquid chromatography (HILIC) under high organic solvent mobile phase conditions. These two methods were then combined within a single gradient run using dual sample injection, with the first injection at the start of the applied gradient (mixed-mode retention of solutes), followed by a second sample injection at the end of the gradient (HILIC retention of solutes). Detection using both ultraviolet absorbance and refractive index enabled the sensitive detection of APIs and UV-absorbing counter-ions, together with quantitative determination of bulk excipients. The developed approach was applied successfully to the analysis of a dry powder inhalers (Flixotide(®), Spiriva(®)), enabling comprehensive quantification of all APIs and excipients in the sample. Copyright © 2013 Elsevier B.V. All rights reserved.

Magnetic studies of nickel ferrite nanoparticles prepared by sol-gel technique

DOE Office of Scientific and Technical Information (OSTI.GOV)

Anumol, C. N.; Chithra, M.; Sahoo, Subasa C., E-mail: subasa@cukerala.ac.in

2016-05-06

Ni-ferrite nanoparticles were synthesized by sol–gel technique by varying the solvent concentration. X-ray diffraction studies confirmed the phase purity in the samples. The lattice constant and grain size were found to be in the range of 0.833-0.834 nm and 14-26 nm respectively. There was no systematic variation in magnetization value with the solvent concentration and grain size. The highest magnetization, remanence and coercivity values of 60 emu/g, 12 emu/g and 180 Oe respectively were observed at 300K in the present study for the sample prepared in 75ml of solvent. The observed magnetization value is 20% higher than the bulk value of 50more » emu/g. The magnetization, coercivity and remanence values were enhanced at 60K compared to those at 300K. The observed high magnetization value in the nanoparticles can be explained on the basis of modified cation distribution in the lattice sites. The enhanced magnetic properties at 60K may be understood due to the reduced thermal fluctuation and increased anisotropy at low temperature.« less

Effects of densification of precursor pellets on microstructures and critical current properties of YBCO melt-textured bulks

NASA Astrophysics Data System (ADS)

Setoyama, Yui; Shimoyama, Jun-ichi; Motoki, Takanori; Kishio, Kohji; Awaji, Satoshi; Kon, Koichi; Ichikawa, Naoki; Inamori, Satoshi; Naito, Kyogo

2016-12-01

Effects of densification of precursor disks on the density of residual voids and critical current properties for YBCO melt-textured bulk superconductors were systematically investigated. Six YBCO bulks were prepared from precursor pellets with different initial particle sizes of YBa2Cu3Oy (Y123) powder and applied pressures for pelletization. It was revealed that use of finer Y123 powder and consolidation using cold-isostatic-pressing (CIP) with higher pressures result in reduction of residual voids at inner regions of bulks and enhance Jc especially under low fields below the second peak.

A study of preparation techniques and properties of bulk nanocomposites based on aqueous albumin dispersion

NASA Astrophysics Data System (ADS)

Gerasimenko, A. Yu.; Dedkova, A. A.; Ichkitidze, L. P.; Podgaetskii, V. M.; Selishchev, S. V.

2013-08-01

Bulk nanocomposites prepared from an aqueous albumin dispersion with carbon nanotubes by removing the liquid component from the dispersion have been investigated. The composites were obtained by thermostating and exposure to LED and IR diode laser radiation. The nanocomposites obtained under laser irradiation retain their shape and properties for several years, in contrast to the composites fabricated in different ways (which decompose into small fragments immediately after preparation). The low density of the composites under study (˜1200 kg/m3), which is close to the density of water, is due to their high porosity. The hardness of stable nanocomposites (˜300 MPa) was found to be at the same level as the hardness of polymethylmethacrylate, aluminum, and iron and close to the hardness of human bone tissue. The cluster quasiordering of the inner structure of nanocomposites revealed by atomic force microscopy indicates the possibility of forming a bulk nanotube framework in them, which can be caused by the effect of the electric field of laser radiation and ensure their stability and hardness. The presence of a framework in nanocomposites provides conditions for self-assembly of biological tissues and makes it possible to apply laser-prepared nanocomposites as a component of surgical implants.

Converting Y(OH){sub 3} nanofiber bundles to YVO{sub 4} polyhedrons for photodegradation of dye contaminants

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Li; School of Chemical Engineering and Materials Engineering, Huainan Normal University, Huainan 232038; Zou, Lei

2015-08-15

Highlights: • YVO{sub 4} polyhedrons were prepared from Y(OH){sub 3} nanofiber bundles through a hydrothermal conversion process. • In contrast to the bulk oxide, the photocatalytic performance of the polyhedrons was much improved. • The main active species involved in photocatalytic oxidative reaction were also investigated. - Abstract: This paper reports a hydrothermal conversion process of rare earth microstructures, Y(OH){sub 3} nanofiber bundles, into YVO{sub 4} polyhedrons, together with the investigation on the related photocatalytic properties. The as-synthesized samples were characterized by a variety of techniques, including XRD, SEM, TEM and UV–vis diffuse reflectance spectroscopy. The photocatalytic activities of YVO{submore » 4} polyhedrons were comparatively evaluated by the photodegradation of Rhodamine B and methylene blue. In contrast to the bulk oxide, the photocatalytic performance of the polyhedrons was much improved. The mechanism and the main active species involved in photocatalytic oxidative reaction were also investigated through the carriers trapping experiments.« less

Scanning electron microscopy imaging of dislocations in bulk materials, using electron channeling contrast.

PubMed

Crimp, Martin A

2006-05-01

The imaging and characterization of dislocations is commonly carried out by thin foil transmission electron microscopy (TEM) using diffraction contrast imaging. However, the thin foil approach is limited by difficult sample preparation, thin foil artifacts, relatively small viewable areas, and constraints on carrying out in situ studies. Electron channeling imaging of electron channeling contrast imaging (ECCI) offers an alternative approach for imaging crystalline defects, including dislocations. Because ECCI is carried out with field emission gun scanning electron microscope (FEG-SEM) using bulk specimens, many of the limitations of TEM thin foil analysis are overcome. This paper outlines the development of electron channeling patterns and channeling imaging to the current state of the art. The experimental parameters and set up necessary to carry out routine channeling imaging are reviewed. A number of examples that illustrate some of the advantages of ECCI over thin foil TEM are presented along with a discussion of some of the limitations on carrying out channeling contrast analysis of defect structures. Copyright (c) 2006 Wiley-Liss, Inc.

Hierarchical assembly of AgCl@Sn-TiO2 microspheres with enhanced visible light photocatalytic performance

NASA Astrophysics Data System (ADS)

Ganeshraja, Ayyakannu Sundaram; Zhu, Kaixin; Nomura, Kiyoshi; Wang, Junhu

2018-05-01

The hierarchical silver chloride loaded tin-doped titania (AgCl@Sn-TiO2) microspheres were first time prepared by a hydrothermal method and annealing at different temperatures. The catalyst showed the enhanced visible light photocatalytic activity as compared to the plasmonic photocatalysts of AgCl and Ag/AgCl, and commercial Degussa P25 (TiO2). The improved efficiency is considered to local surface plasmonic resonance (AgCl could reduce to Ag0 during photocatalytic reaction) in enhanced broad band visible light absorption in addition to the characteristics of heterojunction between Sn-TiO2 and AgCl NPs. Moreover, the surface and bulk properties of as-synthesized samples were analyzed by 119Sn Mössbauer spectroscopy. The magnetic property of the bulk was studied as a function of magnetic field with different temperatures. These results signify the clear details of the magnetic and visible light photocatalytic activities of hierarchical AgCl@Sn-TiO2 microspheres.

Correlation between structural, electrical and magnetic properties of GdMnO3 bulk ceramics

NASA Astrophysics Data System (ADS)

Samantaray, S.; Mishra, D. K.; Pradhan, S. K.; Mishra, P.; Sekhar, B. R.; Behera, Debdhyan; Rout, P. P.; Das, S. K.; Sahu, D. R.; Roul, B. K.

2013-08-01

This paper reports the effect of sintering temperature on ferroelectric properties of GdMnO3 (GMO) bulk ceramics at room temperature prepared by the conventional solid state reaction route following slow step sintering schedule. Ferroelectric hysteresis loop as well as sharp dielectric anomaly in pure (99.999%) GMO sintered ceramics has been clearly observed. Samples sintered at 1350 °C become orthorhombic with Pbnm space group and showed frequency independent sharp dielectric anomalies at 373 K and a square type of novel ferroelectric hysteresis loop was observed at room temperature. Interestingly, dielectric anomalies and ferroelectric behavior were observed to be dependent upon sintering temperature of GdMnO3. Room temperature dielectric constant (ɛr) value at different frequencies is observed to be abnormally high. The magnetic field and temperature dependent magnetization show antiferromagnetic behavior at 40 K for both 1350 °C and 1700 °C sintered GMO. Present findings showed the possibility of application of GdMnO3 at room temperature as multifunctional materials.

An investigation into the stability and sterility of citric acid solutions used for cough reflex testing.

PubMed

Falconer, James R; Wu, Zimei; Lau, Hugo; Suen, Joanna; Wang, Lucy; Pottinger, Sarah; Lee, Elaine; Alazawi, Nawar; Kallesen, Molly; Gargiulo, Derryn A; Swift, Simon; Svirskis, Darren

2014-10-01

Citric acid is used in cough reflex testing in clinical and research settings to assess reflexive cough in patients at risk of swallowing disorders. To address a lack of knowledge in this area, this study investigated the stability and sterility of citric acid solutions. Triplicate solutions of citric acid (0.8 M) in isotonic saline were stored at 4 ± 2 °C for up to 28 days and analysed by high-performance liquid chromatography. Microbiological sterility of freshly prepared samples and bulk samples previously used for 2 weeks within the hospital was determined using a pour plate technique. Microbial survival in citric acid was determined by inoculating Staphylococcus aureus, Escherichia coli, or Candida albicans into citric acid solution and monitoring the number of colony-forming units/mL over 40 min. Citric acid solutions remained stable at 4 °C for 28 days (98.4 ± 1.8 % remained). The freshly prepared and clinical samples tested were sterile. However, viability studies revealed that citric acid solution allows for the survival of C. albicans but not for S. aureus or E. coli. The microbial survival study showed that citric acid kills S. aureus and E. coli but has no marked effect on C. albicans after 40 min. Citric acid samples at 0.8 M remained stable over the 4-week testing period, with viable microbial cells absent from samples tested. However, C. albicans has the ability to survive in citric acid solution if inadvertently introduced in practice. For this reason, in clinical and research practice it is suggested to use single-use aliquots prepared aseptically which can be stored for up to 28 days at 4 °C.

Valence-band and core-level photoemission study of single-crystal Bi2CaSr2Cu2O8 superconductors

NASA Astrophysics Data System (ADS)

Shen, Z.-X.; Lindberg, P. A. P.; Wells, B. O.; Mitzi, D. B.; Lindau, I.; Spicer, W. E.; Kapitulnik, A.

1988-12-01

High-quality single crystals of Bi2CaSr2Cu2O8 superconductors have been prepared and cleaved in ultrahigh vacuum. Low-energy electron diffraction measurements show that the surface structure is consistent with the bulk crystal structure. Ultraviolet photoemission and x-ray photoemission experiments were performed on these well-characterized sample surfaces. The valence-band and the core-level spectra obtained from the single-crystal surfaces are in agreement with spectra recorded from polycrystalline samples, justifying earlier results from polycrystalline samples. Cu satellites are observed both in the valence band and Cu 2p core level, signaling the strong correlation among the Cu 3d electrons. The O 1s core-level data exhibit a sharp, single peak at 529-eV binding energy without any clear satellite structures.

Comparison of wet-only and bulk deposition at Chiang Mai (Thailand) based on rainwater chemical composition

NASA Astrophysics Data System (ADS)

Chantara, Somporn; Chunsuk, Nawarut

The chemical composition of 122 rainwater samples collected daily from bulk and wet-only collectors in a sub-urban area of Chiang Mai (Thailand) during August 2005-July 2006 has been analyzed and compared to assess usability of a cheaper and less complex bulk collector over a sophisticated wet-only collector. Statistical analysis was performed on log-transformed daily rain amount and depositions of major ions for each collector type. The analysis of variance (ANOVA) test revealed that the amount of rainfall collected from a rain gauge, bulk collector and wet-only collector showed no significant difference ( ∝=0.05). The volume weight mean electro-conductivity (EC) values of bulk and wet-only samples were 0.69 and 0.65 mS/m, respectively. The average pH of the samples from both types of collectors was 5.5. Scatter plots between log-transformed depositions of specific ions obtained from bulk and wet-only samples showed high correlation ( r>0.91). Means of log-transformed bulk deposition were 14% (Na + and K +), 13% (Mg 2+), 7% (Ca 2+), 4% (NO 3-), 3% (SO 42- and Cl -) and 2% (NH 4+) higher than that of wet-only deposition. However, multivariate analysis of variance (MANOVA) revealed that ion depositions obtained from bulk and wet-only collectors were not significantly different ( ∝=0.05). Therefore, it was concluded that a bulk collector can be used instead of a wet-only collector in a sub-urban area.

Single clay sheets inside electrospun polymer nanofibers

NASA Astrophysics Data System (ADS)

Sun, Zhaohui

2005-03-01

Nanofibers were prepared from polymer solution with clay sheets by electrospinning. Plasma etching, as a well controlled process, was used to supply electrically excited gas molecules from a glow discharge. To reveal the structure and arrangement of clay layers in the polymer matrix, plasma etching was used to remove the polymer by controlled gasification to expose the clay sheets due to the difference in reactivity. The shape, flexibility, and orientation of clay sheets were studied by transmission and scanning electron microscopy. Additional quantitative information on size distribution and degree of exfoliation of clay sheets were obtained by analyzing electron micrograph of sample after plasma etching. Samples in various forms including fiber, film and bulk, were thinned by plasma etching. Morphology and dispersion of inorganic fillers were studied by electron microscopy.

Room temperature magnetocaloric effect and refrigerant capacitance in La{sub 0.7}Sr{sub 0.3}MnO{sub 3} nanotube arrays

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumaresavanji, M., E-mail: vanji.hplt@gmail.com; Sousa, C. T.; Pires, A.

2014-08-25

High aspect ratio La{sub 0.7}Sr{sub 0.3}MnO{sub 3} nanotube (NT) arrays have been synthesized using nitrates based sol-gel precursor by nanoporous anodized aluminum oxide template assisted method. Their phase purity and microstructures were analyzed by X-ray diffraction, scanning electron microscopy, and energy-dispersive x-ray spectroscopy. Magnetocaloric effect (MCE) of as prepared NTs was investigated by means of field dependence magnetization measurements. Significant magnetic entropy change, −△S{sub M} = 1.6 J/kg K, and the refrigerant capacitance, RC = 69 J/kg, were achieved near the transition temperature at 315 K for 5 T. For comparison, a bulk sample was also prepared using the same precursor solution which gives a value of −△S{submore » M} = 4.2 J/kg K and a RC = 165 J/kg. Though the bulk sample exhibits higher △S{sub M} value, the NTs present an expanded temperature dependence of −△S{sub M} curves that spread over a broad temperature range and assured to be appropriate for active magnetic refrigeration. The diminutive MCE observed in manganite NTs is explained by the increased influence of surface sites of nanograins which affect the structural phase transition occurred by external magnetic field due to the coupling between magnetism and the lattice in manganese perovskites. Our report paves the way for further investigation in 1D manganite nanostructured materials towards applications in such magnetic refrigeration technology or even on hyperthermia/drug delivery.« less

Spray-dried chitosan as a direct compression tableting excipient.

PubMed

Chinta, Dakshinamurthy Devanga; Graves, Richard A; Pamujula, Sarala; Praetorius, Natalie; Bostanian, Levon A; Mandal, Tarun K

2009-01-01

The objective of this study was to prepare and evaluate a novel spray-dried tableting excipient using a mixture of chitosan and lactose. Three different grades of chitosan (low-, medium-, and high-molecular-weight) were used for this study. Propranolol hydrochloride was used as a model drug. A specific amount of chitosan (1, 1.9, and 2.5 g, respectively) was dissolved in 50 mL of an aqueous solution of citric acid (1%) and later mixed with 50 mL of an aqueous solution containing lactose (20, 19.1, and 18.5 g, respectively) and propanolol (2.2 g). The resultant solution was sprayed through a laboratory spray drier at 1.4 mL/min. The granules were evaluated for bulk density, tap density, Carr index, particle size distribution, surface morphology, thermal properties, and tableting properties. Bulk density of the granules decreased from 0.16 to 0.13 g/mL when the granules were prepared using medium- or high-molecular-weight chitosan compared with the low-molecular-weight chitosan. The relative proportion of chitosan also showed a significant effect on the bulk density. The granules prepared with 1 g of low-molecular-weight chitosan showed the minimum Carr index (11.1%) indicating the best flow properties among all five formulations. All three granules prepared with 1 g chitosan, irrespective of their molecular weight, showed excellent flow properties. Floating tablets prepared by direct compression of these granules with sodium bicarbonate showed 50% drug release between 30 and 35 min. In conclusion, the spray-dried granules prepared with chitosan and lactose showed excellent flow properties and were suitable for tableting.

Teaching Advanced SQL Skills: Text Bulk Loading

ERIC Educational Resources Information Center

Olsen, David; Hauser, Karina

2007-01-01

Studies show that advanced database skills are important for students to be prepared for today's highly competitive job market. A common task for database administrators is to insert a large amount of data into a database. This paper illustrates how an up-to-date, advanced database topic, namely bulk insert, can be incorporated into a database…

40 CFR 761.289 - Compositing samples.

Code of Federal Regulations, 2011 CFR

2011-07-01

... Remediation Waste and Porous Surfaces in Accordance With § 761.61(a)(6) § 761.289 Compositing samples. Compositing is a method of combining several samples of a specific type of bulk PCB remediation waste or... compositing bulk PCB remediation waste samples. These procedures are based on the method for selecting...

40 CFR 761.289 - Compositing samples.

Code of Federal Regulations, 2010 CFR

2010-07-01

... Remediation Waste and Porous Surfaces in Accordance With § 761.61(a)(6) § 761.289 Compositing samples. Compositing is a method of combining several samples of a specific type of bulk PCB remediation waste or... compositing bulk PCB remediation waste samples. These procedures are based on the method for selecting...

Ferroelectric relaxor behaviour and impedance spectroscopy of Bi2O3-doped barium zirconium titanate ceramics

NASA Astrophysics Data System (ADS)

Mahajan, Sandeep; Thakur, O P; Bhattacharya, D K; Sreenivas, K

2009-03-01

Bi2O3-doped barium zirconate titanate ceramics, Ba1-xBix(Zr0.05Ti0.95)O3, have been prepared by the conventional solid-state reaction method. The ferroelectric relaxor behaviour and dielectric properties have been investigated in detail. By XRD analysis, it is suggested that up to x = 0.04, Bi3+ substitutes A-site ion, and thereafter with higher Bi3+ content, it enters the B-site sub lattice. Substitution of Bi3+ ions induces ferroelectric relaxor behaviour and the degree of relaxation behaviour increases with bismuth concentration. The remanent polarization and strain behaviour show a slight increase with the substitution level. The degree of hysteresis (strain versus electric field) also reduces from 21.4% to 4.6% with bismuth substitution. Impedance measurements were made on the prepared sample over a wide range of temperatures (300-723 K) and frequencies (40 Hz-1 MHz), which show the presence of both bulk and grain boundary effects in the material. The bulk and grain boundary conductivities determined from impedance study indicate the Arrhenius-type thermally activated process. Impedance spectroscopy is shown to be an efficient method capable of detecting the contributions of the resistances of grains and grain boundaries to the complex impedance of a ceramic system, accurately estimating its electrical conductivity as well as its corresponding activation energies and drawing conclusions on its structural properties.

Etching of Cr tips for scanning tunneling microscopy of cleavable oxides

DOE Office of Scientific and Technical Information (OSTI.GOV)

Huang, Dennis; Liu, Stephen; Zeljkovic, Ilija

Here, we report a detailed three-step roadmap for the fabrication and characterization of bulk Cr tips for spin-polarized scanning tunneling microscopy. Our strategy uniquely circumvents the need for ultra-high vacuum preparation of clean surfaces or films. First, we demonstrate the role of ex situ electrochemical etch parameters on Cr tip apex geometry, using scanning electron micrographs of over 70 etched tips. Second, we describe the suitability of the in situ cleaved surface of the layered antiferromagnet La 1.4Sr 1.6Mn 2O 7 to evaluate the spin characteristics of the Cr tip, replacing the ultra-high vacuum-prepared test samples that have been usedmore » in prior studies. Third, we outline a statistical algorithm that can effectively delineate closely spaced or irregular cleaved step edges, to maximize the accuracy of step height and spin-polarization measurements.« less

Rare-gas-rich separates from carbonaceous chondrites

NASA Technical Reports Server (NTRS)

Reynolds, J. H.; Frick, U.; Neil, J. M.; Phinney, D. L.

1978-01-01

This paper describes an analysis of carbon-rich separates prepared by demineralization of colloidal fractions after disaggregation of bulk samples of the type C2 meteorites Murray, Murchison, and Cold Bokkeveld, as well as a methanol colloid extracted from acid-resistant residues of the Allende meteorite (type C3V) obtained by dissolution of most of the minerals in HCl and HF acids. The carbonaceous separates, or lAlates (a coined word designating colloids prepared sometimes before and sometimes after acid treatment), are characterized incompletely and with difficulty. A stepwise heating experiment on a Murray lAlate is discussed which revealed bimodal release of all noble gases, with similar patterns for Ar, Kr, and Xe. Chemical reactions are suggested as the likely mechanism for gas release. The results are shown to support the concept of a carbonaceous gas carrier uniformly present in meteorites of various types.

Etching of Cr tips for scanning tunneling microscopy of cleavable oxides

DOE PAGES

Huang, Dennis; Liu, Stephen; Zeljkovic, Ilija; ...

2017-02-21

Here, we report a detailed three-step roadmap for the fabrication and characterization of bulk Cr tips for spin-polarized scanning tunneling microscopy. Our strategy uniquely circumvents the need for ultra-high vacuum preparation of clean surfaces or films. First, we demonstrate the role of ex situ electrochemical etch parameters on Cr tip apex geometry, using scanning electron micrographs of over 70 etched tips. Second, we describe the suitability of the in situ cleaved surface of the layered antiferromagnet La 1.4Sr 1.6Mn 2O 7 to evaluate the spin characteristics of the Cr tip, replacing the ultra-high vacuum-prepared test samples that have been usedmore » in prior studies. Third, we outline a statistical algorithm that can effectively delineate closely spaced or irregular cleaved step edges, to maximize the accuracy of step height and spin-polarization measurements.« less

Improving detection probabilities for pests in stored grain.

PubMed

Elmouttie, David; Kiermeier, Andreas; Hamilton, Grant

2010-12-01

The presence of insects in stored grain is a significant problem for grain farmers, bulk grain handlers and distributors worldwide. Inspection of bulk grain commodities is essential to detect pests and thereby to reduce the risk of their presence in exported goods. It has been well documented that insect pests cluster in response to factors such as microclimatic conditions within bulk grain. Statistical sampling methodologies for grain, however, have typically considered pests and pathogens to be homogeneously distributed throughout grain commodities. In this paper, a sampling methodology is demonstrated that accounts for the heterogeneous distribution of insects in bulk grain. It is shown that failure to account for the heterogeneous distribution of pests may lead to overestimates of the capacity for a sampling programme to detect insects in bulk grain. The results indicate the importance of the proportion of grain that is infested in addition to the density of pests within the infested grain. It is also demonstrated that the probability of detecting pests in bulk grain increases as the number of subsamples increases, even when the total volume or mass of grain sampled remains constant. This study underlines the importance of considering an appropriate biological model when developing sampling methodologies for insect pests. Accounting for a heterogeneous distribution of pests leads to a considerable improvement in the detection of pests over traditional sampling models. Copyright © 2010 Society of Chemical Industry.

Surface-Directed Synthesis of Erbium-Doped Yttrium Oxide Nanoparticles within Organosilane Zeptoliter Containers

PubMed Central

2015-01-01

We introduce an approach to synthesize rare earth oxide nanoparticles using high temperature without aggregation of the nanoparticles. The dispersity of the nanoparticles is controlled at the nanoscale by using small organosilane molds as reaction containers. Zeptoliter reaction vessels prepared from organosilane self-assembled monolayers (SAMs) were used for the surface-directed synthesis of rare earth oxide (REO) nanoparticles. Nanopores of octadecyltrichlorosilane were prepared on Si(111) using particle lithography with immersion steps. The nanopores were filled with a precursor solution of erbium and yttrium salts to confine the crystallization step to occur within individual zeptoliter-sized organosilane reaction vessels. Areas between the nanopores were separated by a matrix film of octadecyltrichlorosilane. With heating, the organosilane template was removed by calcination to generate a surface array of erbium-doped yttria nanoparticles. Nanoparticles synthesized by the surface-directed approach retain the periodic arrangement of the nanopores formed from mesoparticle masks. While bulk rare earth oxides can be readily prepared by solid state methods at high temperature (>900 °C), approaches for preparing REO nanoparticles are limited. Conventional wet chemistry methods are limited to low temperatures according to the boiling points of the solvents used for synthesis. To achieve crystallinity of REO nanoparticles requires steps for high-temperature processing of samples, which can cause self-aggregation and dispersity in sample diameters. The facile steps for particle lithography address the problems of aggregation and the requirement for high-temperature synthesis. PMID:25163977

Methods for Producing High-Performance Silicon Carbide Fibers, Architectural Preforms, and High-Temperature Composite Structures

NASA Technical Reports Server (NTRS)

Yun, Hee-Mann (Inventor); DiCarlo, James A. (Inventor)

2014-01-01

Methods are disclosed for producing architectural preforms and high-temperature composite structures containing high-strength ceramic fibers with reduced preforming stresses within each fiber, with an in-situ grown coating on each fiber surface, with reduced boron within the bulk of each fiber, and with improved tensile creep and rupture resistance properties tier each fiber. The methods include the steps of preparing an original sample of a preform formed from a pre-selected high-strength silicon carbide ceramic fiber type, placing the original sample in a processing furnace under a pre-selected preforming stress state and thermally treating the sample in the processing furnace at a pre-selected processing temperature and hold time in a processing gas having a pre-selected composition, pressure, and flow rate. For the high-temperature composite structures, the method includes additional steps of depositing a thin interphase coating on the surface of each fiber and forming a ceramic or carbon-based matrix within the sample.

Single Crystal Synthesis and STM Studies of High Temperature Superconductors

NASA Technical Reports Server (NTRS)

Barrientos, Alfonso

1997-01-01

This is a final report for the work initiated in September of 1994 under the grant NAG8-1085 - NASA/OMU, on the fabrication of bulk and single crystal synthesis, specific heat measuring and STM studies of high temperature superconductors. Efforts were made to fabricate bulk and single crystals of mercury based superconducting material. A systematic thermal analysis on the precursors for the corresponding oxides and carbonates were carried out to synthesized bulk samples. Bulk material was used as seed in an attempt to grow single crystals by a two-step self flux process. On the other hand bulk samples were characterized by x-ray diffraction, electrical resistivity and magnetic susceptibility, We studied the specific heat behavior in the range from 80 to 300 K. Some preliminary attempts were made to study the atomic morphology of our samples. As part of our efforts we built an ac susceptibility apparatus for measuring the transition temperature of our sintered samples.

A Robust Analysis Method For Δ13c Signal Of Bulk Organic Matter In Speleothems

NASA Astrophysics Data System (ADS)

Bian, F.; Blyth, A. J.; Smith, C.; Baker, A.

2017-12-01

Speleothems preserve organic matter that is derived from both the surface soil and cave environments. This organic matter can be used to understand paleoclimate and paleoenvironments. However, a stable and quick micro-analysis method to measure the δ13C signals from speleothem organic matter separate from the total δ13C remains absent. And speleothem organic geochemistry is still relatively unexplored compared to inorganic geochemistry. In this research, for the organic matter analysis, bulk homogeneous power samples were obtained from one large stalagmite. These were dissolved by phosphoric acid to produce the aqueous solution. Then, the processed solution was degassed through a rotational vacuum concentrator. A liquid chromatograph was coupled to IRMS to control the oxidization and the measurement of analytes. This method is demonstrated to be robust for the analysis of speleothem d13C organic matter analysis under different preparation and instrumental settings, with the low standard deviation ( 0.2‰), and low sample consumption (<25 mg). Considering the complexity of cave environments, this method will be useful in further investigations the δ13C of entrapped organic matter and environmental controls in other climatic and ecological contexts, including the determination of whether vegetation or soil microbial activity is the dominant control on speleothem d13C of organic matter.

Detection of multiple Mycoplasma species in bulk tank milk samples using real-time PCR and conventional culture and comparison of test sensitivities.

PubMed

Justice-Allen, A; Trujillo, J; Goodell, G; Wilson, D

2011-07-01

The objective of this study was to further validate a SYBR PCR protocol for Mycoplasma spp. by comparing it with standard microbial culture in the detection of Mycoplasma spp. in bulk tank milk samples. Additionally, we identified Mycoplasma spp. present by analysis of PCR-generated amplicons [dissociation (melt) temperature (T(m)), length, and DNA sequence]. The research presented herein tests the hypothesis that the SYBR PCR protocol is as sensitive as conventional culture for the detection of Mycoplasma spp. in bulk tank milk samples. Mycoplasmas cause several important disease syndromes in cattle, including mastitis in dairy cows. The standard diagnostic method at the herd level has been microbial isolation of mycoplasmas on 1 of several specialized media and speciation through biochemical or immunological techniques; repeated sampling schemes are recommended. The development of a real-time SYBR PCR protocol offers advantages in decrease of time to detection, cost, and complexity. The T(m) of the double-stranded DNA generated from the PCR reaction was used to detect the presence of and tentatively identify the species of mycoplasmas other than Mycoplasma bovis. In the SYBR PCR protocol, the presence of multiple species of mycoplasmas is indicated by an atypical dissociation curve. Gel electrophoresis and sequencing of the amplicons was used to confirm the mycoplasma species present when a non-M. bovis organism was detected (T(m) not equal to M. bovis) and used to identify all the mycoplasma species present for the samples with atypical dissociation curves. Mycoplasma bovis was identified in 83% of SYBR PCR mycoplasma-positive bulk tank samples. Another mycoplasma was identified either alone or in addition to M. bovis in 25% of SYBR PCR mycoplasma-positive bulk tank milk samples. Four species of mycoplasma other than M. bovis (Mycoplasma alkalescens, Mycoplasma arginini, Mycoplasma bovigenitalium, and Mycoplasma gateae) were identified in bulk tank milk samples tested with this method. Five farms had 2 mycoplasma species occurring at different times in their bulk tanks. Two mycoplasma species were identified in the same bulk tank sample in 7 instances on 2 farms. The finding of multiple Mycoplasma spp. coexisting on a farm and even in the same bulk tank milk sample indicates that the clinical significance of multiple mycoplasma species in the pathology of intramammary infections should be investigated further. In comparison with conventional culture, the SYBR PCR protocol was slightly (but not statistically significantly) more sensitive in the detection of mycoplasmas in bulk tank milk. Copyright © 2011 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Photocatalytic activity of SnO{sub 2} nanoparticles in methylene blue degradation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kim, Sung Phil; Choi, Myong Yong, E-mail: mychoi@gnu.ac.kr; Choi, Hyun Chul, E-mail: chc12@chonnam.ac.kr

2016-02-15

Highlights: • Nanosized SnO{sub 2} photocatalysts were prepared with a precipitation method. • SnO{sub 2} nanoparticles displayed high photocatalytic activities for the MB degradation. • OH radicals are the main active species in photocatalysis on the SnO{sub 2} nanoparticles. - Abstract: Nanosized SnO{sub 2} photocatalysts were prepared with a precipitation method and were characterized by performing transmission electron microscopy (TEM), powder X-ray diffraction (XRD), and X-ray absorption spectroscopy (XAS). The powder XRD results revealed that the SnO{sub 2} nanoparticles have a typical tetragonal rutile (cassiterite) structure and the average crystallite size was found to be approximately 4.5 nm by usingmore » the Debye–Scherrer equation. The prepared SnO{sub 2} nanoparticles consist of agglomerated particles with a mean diameter of around 4–5 nm according to the analysis of TEM images. The XAS data confirmed that the prepared samples have cassiterite structures with tin oxidation state of +4. The prepared SnO{sub 2} nanoparticles were found to exhibit approximately 3.8 times higher activity than bulk SnO{sub 2} in the photodegradation of methylene blue. On the basis of a trapping experiment, we developed a possible mechanism for the photodegradation on SnO{sub 2} nanoparticles.« less

Improved dehydrogenation performance of LiBH4 by 3D hierarchical flower-like MoS2 spheres additives

NASA Astrophysics Data System (ADS)

Zhao, Yan; Liu, Yongchang; Liu, Huiqiao; Kang, Hongyan; Cao, Kangzhe; Wang, Qinghong; Zhang, Chunling; Wang, Yijing; Yuan, Huatang; Jiao, Lifang

2015-12-01

In this work, 3D hierarchical flower-like MoS2 spheres are successfully fabricated via a hydrothermal method followed by a heat treatment. The obtained product is composed of few-layered MoS2 nanosheets with enlarged interlayer distance (ca. 0.66 nm) of the (002) plane. Meanwhile, the hydrogen storage properties of the as-prepared MoS2 ball milled with LiBH4 are systematically investigated. The results of temperature programmed desorption (TPD) and isothermal measurement suggest that the LiBH4-MoS2 (as-prepared) mixture exhibits favorable dehydrogenation properties in both lowering the hydrogen release temperature and improving kinetics of hydrogen release rate. LiBH4-MoS2 (as-prepared) sample (the preparation mass ratio is 1:1) starts to release hydrogen at 171 °C, and roughly 5.6 wt% hydrogen is released within 1 h when isothermally heated to 320 °C, which presents superior dehydrogenation performance compared to that of the bulk LiBH4. The excellent dehydrogenation performance of the LiBH4-MoS2 (as-prepared) mixture may be attributed to the high active site density and enlarged interlayer distance of the MoS2 nanosheets, 3D architectures and hierarchical structures.

Dense garnet-like Li5La3Nb2O12 solid electrolyte prepared by self-consolidation method

NASA Astrophysics Data System (ADS)

Zhao, Pengcheng; Xiang, Yu; Xu, Yan; Wen, Yuehua; Zhang, Wenfeng; Zhu, Xiayu; Li, Meng; Zhang, Sontong; Ming, Hai; Jin, Zhaoqing; Cao, Gaoping

2018-06-01

Li5La3Nb2O12 (LLNO) is a typical garnet-like solid electrolyte with solitary cubic structure. However, its ionic conductivity is relatively low due to the low relative density when prepared by cold isostatic pressing method, which usually involves high-pressure machines, poor productivity, tedious pressing operations, and low density. In this paper, self-consolidation method is developed to sinter dense LLNO electrolyte. Although not any pressing operations are employed in the entire process, the relative density of LLNO is promoted up to 95%, which is much higher than the reported values of 45-80%. SEM images reveal that the sample is built by huge particles in size of 80 μm indicating that there are few boundaries in the sample. Moreover, a rich content of Li-Al-O compounds is detected out in the boundary areas, which may act as sintering aids for the sample to consolidate automatically. According to the highest density, the bulk ionic conductivity of LLNO sample reaches up to 1.61 × 10-4 S cm-1 at 30 °C, which is in the same order of magnitude as the value of cubic Li7La3Zr2O12 electrolyte. This work verifies the self-consolidation mechanism for the sintering of ceramic electrolytes and could significantly facilitate the development of LLNO membrane technology.

Effects of flux concentrations and sintering temperature on dental porcelain

NASA Astrophysics Data System (ADS)

Ghose, Polash; Gafur, Md. Abdul; Das, Sujan Kumar; Ranjan Chakraborty, Shyamal; Mohsin, Md.; Deb, Arun Kumar; Rakibul Qadir, Md.

2014-02-01

In this study, samples of dental porcelain bodies have been made by using the materials collected from selected deposits employing different mixing proportions of clay, quartz and feldspar. Dental porcelain ceramics have been successfully fabricated by using the sintering technique together with some Na2CO3 additive. The dental porcelain powder has been pressed into pellets at first and subsequently sintered at 700, 800, 900, 1000 and 1100 °C for 2 h. The physical and mechanical properties of the prepared samples have been investigated. The sintering behavior of the fired samples has been evaluated by bulk density, linear shrinkage, water absorption and apparent porosity measurements. This study includes the evaluation of the Vickers's microhardness by microhardness tester. Phase analysis and microstructural study have been performed by XRD and optical microscope respectively. Optical properties have been investigated using UV-visible spectroscopy. Influence of firing conditions on leucite formation, densification and microstructural development of the sintered samples has been investigated. It has been found that the choice of sintering temperature is one of the key factors in controlling leucite crystallization in dental porcelain ceramics. It has also been found that the flux concentration of material and the effect of temperature on preparation of dental porcelain contribute to the firing shrinkage and hardness, which has been found to increase with the increase of treatment temperature.

Silicon nanostructure arrays prepared by single step metal assisted chemical etching from single crystal wafer

NASA Astrophysics Data System (ADS)

Sarkar, Kalyan; Das, Debajyoti

2018-04-01

Arrays of silicon nanostructures have been produced by single step Metal Assisted Chemical Etching (MACE) of single crystal Si-wafers at room temp and normal atmospheric condition. By studying optical and structural properties of the silicon nanowire like structures synthesized by Ag catalyst assisted chemical etching, a significant change in the reflectance spectra has been obtained leading to a gross reduction in reflectance from ˜31% to less than 1%. In comparison with bulk c-Si, the surface areas of the nanostructured samples have been increased significantly with the etching time, leading to an efficient absorption of light, favorable for photovoltaic applications.

ICESCAPE Mission

NASA Image and Video Library

2010-07-03

Scientists on the sea ice in the Chukchi Sea off the north coast of Alaska disperse equipment on July 4, 2010, as they prepare to collect data on and below the ice. The research is part of NASA's ICESCAPE mission onboard the U.S. Coast Guard icebreaker Healy to sample the physical, chemical and biological characteristics of the ocean and sea ice. Impacts of Climate change on the Eco-Systems and Chemistry of the Arctic Pacific Environment (ICESCAPE) is a multi-year NASA shipborne project. The bulk of the research will take place in the Beaufort and Chukchi Sea’s in summer of 2010 and fall of 2011. Photo Credit: (NASA/Kathryn Hansen)

Carrier-doped aromatic hydrocarbons: a new platform in condensed matter chemistry and physics.

PubMed

Heguri, Satoshi; Tanigaki, Katsumi

2018-02-27

High-quality bulk samples of the first four polyacenes, which are naphthalene, anthracene, tetracene, and pentacene, doped with alkali metal in 1 : 1 and 1 : 2 stoichiometries were prepared and their fundamental properties were systematically studied. A new systematic understanding on the electronic states of electron-doped polyacenes sensitive to the energetic balance among on-site Coulomb repulsion, bandwidth and the Peierls instability was provided. The carrier-doped typical aromatic hydrocarbons showed a large variety of properties as well as charge transfer complexes and metal-doped fullerides. We open a new avenue for organometallic and inorganic chemistry.

Phase Transitions of KIO3 Ferroelectrics in Al2O3-Based Nanoporous Matrices

NASA Astrophysics Data System (ADS)

Milinskii, A. Yu.; Baryshnikov, S. V.

2018-03-01

Temperature dependences of the linear permittivity ɛ' and the third harmonic amplitude γ3ω of composites prepared by introducing ferroelectrics KIO3 into matrices of porous aluminum oxide Al2O3 with pore sizes of 240 nm were studied. It is found that the IV → III and III → II structural transition temperatures of potassium iodide in Al2O3 pores decrease by 5 K and 24 K, respectively, with respect to bulk KIO3. The measurements of the dielectric properties do not reveal V → IV and II → I phase transitions in the composite samples.

Evidence for Electromagnetic Granularity in the Polycrystalline Iron-Based Superconductor LaO(0.89)F(0.11)FeAs

DTIC Science & Technology

2008-01-01

oriented grain-boundaries. In this work we show considerable evidence for such weak-coupling by study of the dependence of magnetization in bulk and...powdered samples. Bulk sample magnetization curves show very little hysteresis while remanent magnetization shows almost no sample size dependence...K Fig. 2 (Color online) Magnetization hysteresis loops at 5 and 20 K for the bulk LaO0.89F0.11FeAs. Inset shows the temperature dependence of

Within-herd prevalence thresholds for herd-level detection of mastitis pathogens using multiplex real-time PCR in bulk tank milk samples.

PubMed

Soltau, J B; Einax, E; Klengel, K; Katholm, J; Failing, K; Wehrend, A; Donat, K

2017-10-01

The objective of the study was to assess the value of quantitative multiplex real-time PCR examination of bulk tank milk samples for bovine mastitis pathogens as a tool for herd level diagnosis. Using a logistic regression model, this study is aimed at calculating the threshold level of the apparent within-herd prevalence as determined by quarter milk sample cultivation of all lactating cows, thus allowing the detection of a herd positive for a specific pathogen within certain probability levels. A total of 6,335 quarter milk samples were collected and cultured from 1,615 cows on 51 farms in Germany. Bulk tank milk samples were taken from each farm and tested by bacterial culture as well as the commercial PCR assay Mastit 4A (DNA Diagnostic A/S, Risskov, Denmark) identifying Staphylococcus aureus, Streptococcus dysgalactiae, Streptococcus agalactiae, and Streptococcus uberis. In addition, PCR was performed on pooled herd milk samples containing milk aliquots from all lactating cows in each of the 51 herds. Only 1 out of the 51 herds was found PCR positive for Streptococcus agalactiae in bulk tank and pooled herd milk samples, and cultured quarter milk samples. Spearman's rank correlations between the cycle threshold value of bulk tank milk PCR and the apparent within-herd prevalence were calculated in regard to Staphylococcus aureus, Streptococcus dysgalactiae, and Streptococcus uberis. For these pathogens, significant correlations were found. If 1 bulk tank milk sample per herd was tested, the estimated within-herd prevalence thresholds for 90% probability of detection were 27.6% for Staphylococcus aureus, 9.2% for Streptococcus dysgalactiae, and 13.8% for Streptococcus uberis on the cow level. On the quarter level, the within-herd prevalence had to be at least 32.6% for Staphylococcus aureus, 1.7% for Streptococcus dysgalactiae, and 4.3% for Streptococcus uberis to detect a herd as positive using a single bulk milk sample. The results indicate that mastitis pathogens in bulk tank milk can be identified by the applied PCR assay. Bulk tank milk examination is not a reliable tool for the identification of the named pathogens by single testing, but might be a valuable monitoring tool when used frequently with repeated testing. Furthermore, this approach could be a useful monitoring tool for detecting new pathogen occurrence in the herd. Copyright © 2017 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

The Miniaturized Raman System and Detection of Traces of Life in Halite from the Atacama Desert: Some Considerations for the Search for Life Signatures on Mars

PubMed Central

Jehlička, Jan; Edwards, Howell G.M.; Hutchinson, Ian; Ascaso, Carmen; Wierzchos, Jacek

2012-01-01

Abstract Raman spectroscopy is being adopted as a nondestructive instrumentation for the robotic exploration of Mars to search for traces of life in the geological record. Here, miniaturized Raman spectrometers of two different types equipped with 532 and 785 nm lasers for excitation, respectively, were compared for the detection of microbial biomarkers in natural halite from the hyperarid region of the Atacama Desert. Measurements were performed directly on the rock as well as on the homogenized, powdered samples prepared from this material—the effects of this sample preparation and the excitation wavelength employed in the analysis are compared and discussed. From these results, 532 nm excitation was found to be superior for the analysis of powdered specimens due to its high sensitivity toward carotenoids and hence a higher capability for their detection at relatively low concentration in bulk powdered specimens. For the same reason, this wavelength was a better choice for the detection of carotenoids in direct measurements made on the rock samples. The 785 nm excitation wavelength, in contrast, proved to be more sensitive toward the detection of scytonemin. Key Words: Miniaturized portable Raman—Atacama—Mars—Biomarker detection. Astrobiology 12, 1095–1099. PMID:23151300

ZnS, CdS and HgS nanoparticles via alkyl-phenyl dithiocarbamate complexes as single source precursors.

PubMed

Onwudiwe, Damian C; Ajibade, Peter A

2011-01-01

The synthesis of II-VI semiconductor nanoparticles obtained by the thermolysis of certain group 12 metal complexes as precursors is reported. Thermogravimetric analysis of the single source precursors showed sharp decomposition leading to their respective metal sulfides. The structural and optical properties of the prepared nanoparticles were characterized by means of X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) UV-Vis and photoluminescence spectroscopy. The X-ray diffraction pattern showed that the prepared ZnS nanoparticles have a cubic sphalerite structure; the CdS indicates a hexagonal phase and the HgS show the presence of metacinnabar phase. The TEM image demonstrates that the ZnS nanoparticles are dot-shaped, the CdS and the HgS clearly showed a rice and spherical morphology respectively. The UV-Vis spectra exhibited a blue-shift with respect to that of the bulk samples which is attributed to the quantum size effect. The band gap of the samples have been calculated from absorption spectra and werefound to be about 4.33 eV (286 nm), 2.91 eV (426 nm) and 4.27 eV (290 nm) for the ZnS, CdS and HgS samples respectively.

ZnS, CdS and HgS Nanoparticles via Alkyl-Phenyl Dithiocarbamate Complexes as Single Source Precursors

PubMed Central

Onwudiwe, Damian C.; Ajibade, Peter A.

2011-01-01

The synthesis of II-VI semiconductor nanoparticles obtained by the thermolysis of certain group 12 metal complexes as precursors is reported. Thermogravimetric analysis of the single source precursors showed sharp decomposition leading to their respective metal sulfides. The structural and optical properties of the prepared nanoparticles were characterized by means of X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) UV-Vis and photoluminescence spectroscopy. The X-ray diffraction pattern showed that the prepared ZnS nanoparticles have a cubic sphalerite structure; the CdS indicates a hexagonal phase and the HgS show the presence of metacinnabar phase. The TEM image demonstrates that the ZnS nanoparticles are dot-shaped, the CdS and the HgS clearly showed a rice and spherical morphology respectively. The UV-Vis spectra exhibited a blue-shift with respect to that of the bulk samples which is attributed to the quantum size effect. The band gap of the samples have been calculated from absorption spectra and werefound to be about 4.33 eV (286 nm), 2.91 eV (426 nm) and 4.27 eV (290 nm) for the ZnS, CdS and HgS samples respectively. PMID:22016607

230Th/U dating of Last Interglacial brain corals from Bonaire (southern Caribbean) using bulk and theca wall material

NASA Astrophysics Data System (ADS)

Obert, J. Christina; Scholz, Denis; Felis, Thomas; Brocas, William M.; Jochum, Klaus P.; Andreae, Meinrat O.

2016-04-01

We compared the suitability of two skeletal materials of the Atlantic brain coral Diploria strigosa for 230Th/U-dating: the commonly used bulk material comprising all skeletal elements and the denser theca wall material. Eight fossil corals of presumably Last Interglacial age from Bonaire, southern Caribbean Sea, were investigated, and several sub-samples were dated from each coral. For four corals, both the ages and the activity ratios of the bulk material and theca wall agree within uncertainty. Three corals show significantly older ages for their bulk material than for their theca wall material as well as substantially elevated 232Th content and (230Th/238U) ratios. The bulk material samples of another coral show younger ages and lower (230Th/238U) ratios than the corresponding theca wall samples. This coral also contains a considerable amount of 232Th. The application of the available open-system models developed to account for post-depositional diagenetic effects in corals shows that none of the models can successfully be applied to the Bonaire corals. The most likely explanation for this observation is that the assumptions of the models are not fulfilled by our data set. Comparison of the theca wall and bulk material data enables us to obtain information about the open-system processes that affected the corals. The corals showing apparently older ages for their bulk material were probably affected by contamination with a secondary (detrital) phase. The most likely source of the detrital material is carbonate sand. The higher (230Th/232Th) ratio of this material implies that detrital contamination would have a much stronger impact on the ages than a contaminant with a bulk Earth (230Th/232Th) ratio and that the threshold for the commonly applied 232Th reliability criterion would be much lower than the generally used value of 1 ng g-1. The coral showing apparently younger ages for its bulk material was probably influenced by more than one diagenetic process. A potential scenario is a combination of detrital contamination and U addition by secondary pore infillings. Our results show that the dense theca wall material of D. strigosa is generally less affected by post-depositional open-system behaviour and better suited for 230Th/U-dating than the bulk material. This is also obvious from the fact that all ages of theca wall material reflect a Last Interglacial origin (∼125 ka), whereas the bulk material samples are either substantially older or younger. However, for some corals, the 230Th/U-ages and activity ratios of the bulk material and the theca wall samples are similar. This shows that strictly reliable 230Th/U-ages can also be obtained from bulk material samples of exceptionally well-preserved corals. However, the bulk material samples more frequently show elevated activity ratios and ages than the corresponding theca wall samples. Our findings should be generally applicable to brain corals (Mussidae) that are found in tropical oceans worldwide and may enable reliable 230Th/U-dating of fossil corals with similar skeletal architecture, even if their bulk skeleton is altered by diagenesis. The 230Th/U-ages we consider reliable (120-130 ka), along with a recently published age of 118 ka, provide the first comprehensive dating of the elevated lower reef terrace at Bonaire (118-130 ka), which is in agreement in timing and duration with other Last Interglacial records.

Contrasting the microbiomes from forest rhizosphere and deeper bulk soil from an Amazon rainforest reserve.

PubMed

Fonseca, Jose Pedro; Hoffmann, Luisa; Cabral, Bianca Catarina Azeredo; Dias, Victor Hugo Giordano; Miranda, Marcio Rodrigues; de Azevedo Martins, Allan Cezar; Boschiero, Clarissa; Bastos, Wanderley Rodrigues; Silva, Rosane

2018-02-05

Pristine forest ecosystems provide a unique perspective for the study of plant-associated microbiota since they host a great microbial diversity. Although the Amazon forest is one of the hotspots of biodiversity around the world, few metagenomic studies described its microbial community diversity thus far. Understanding the environmental factors that can cause shifts in microbial profiles is key to improving soil health and biogeochemical cycles. Here we report a taxonomic and functional characterization of the microbiome from the rhizosphere of Brosimum guianense (Snakewood), a native tree, and bulk soil samples from a pristine Brazilian Amazon forest reserve (Cuniã), for the first time by the shotgun approach. We identified several fungi and bacteria taxon significantly enriched in forest rhizosphere compared to bulk soil samples. For archaea, the trend was the opposite, with many archaeal phylum and families being considerably more enriched in bulk soil compared to forest rhizosphere. Several fungal and bacterial decomposers like Postia placenta and Catenulispora acidiphila which help maintain healthy forest ecosystems were found enriched in our samples. Other bacterial species involved in nitrogen (Nitrobacter hamburgensis and Rhodopseudomonas palustris) and carbon cycling (Oligotropha carboxidovorans) were overrepresented in our samples indicating the importance of these metabolic pathways for the Amazon rainforest reserve soil health. Hierarchical clustering based on taxonomic similar microbial profiles grouped the forest rhizosphere samples in a distinct clade separated from bulk soil samples. Principal coordinate analysis of our samples with publicly available metagenomes from the Amazon region showed grouping into specific rhizosphere and bulk soil clusters, further indicating distinct microbial community profiles. In this work, we reported significant shifts in microbial community structure between forest rhizosphere and bulk soil samples from an Amazon forest reserve that are probably caused by more than one environmental factors such as rhizosphere and soil depth. Copyright © 2017 Elsevier B.V. All rights reserved.

Bacterial Flagella as a Model Rigid Rod of Tunable Shape

NASA Astrophysics Data System (ADS)

Schwenger, Walter; Yardimci, Sevim; Gibaud, Thomas; Snow, Henry; Urbach, Jeff; Dogic, Zvonimir

In this research, we study the physical properties of suspensions of bacterial flagella from Salmonella typhimurium prepared in a variety of rigid polymorphic shapes. Flagella act as a rigid colloidal particle that can exhibit non-trivial geometry including helices of varying dimensions, straight rods, or a combination of the two in the same filament. By controlling the conditions in which flagella are prepared, the polymorphic shape assumed by the filament can be controlled. Utilizing different polymorphic shapes, we combine results from optical microscopy observations of single filaments with bulk rheological measurements to help understand the role that constituent colloidal geometry plays in complex bulk behavior.

The prominent photoinduced voltage effect of as-prepared macroscopically long Ag core/Ni shell nanoheterojunctions.

PubMed

Sun, Jia-Lin; Zhao, Xingchen; Zhu, Jia-Lin

2008-02-27

Macroscopically long Ag core/Ni shell nanoheterojunctions have been well prepared by a dynamic growth approach. The structure characterized in detail by scanning electron microscopy reveals that the Ag nanowire bundles are wrapped in Ni nanoshields and form multicore coaxial cable frames. Notable photoinduced voltage with a fine repeatability, for irradiation with a laser, is exhibited compared with the case for bulk Ag pole/Ni shell heterojunctions and Ag nanowire bundle/bulk Ni heterojunctions. The prominent photoinduced voltage and the substantial metal nanoscale Ohmic interconnects provided by this kind of nanoheterojunction may have a wide range of applications in the future.

Aromatic organic contaminant removal from an aqueous environment by p(4-VP)-based materials.

PubMed

Sahiner, Nurettin; Ozay, Ozgur; Aktas, Nahit

2011-10-01

p(4-vinylpyridine) (p(4-VP)) hydrogels were prepared in bulk (macro, 5 × 6 mm) and in nanosizes (370 nm) dimensions. The prepared hydrogels were used to remove organic aromatic contaminates such as 4-nitrophenol (4-NP), 2-nitrophenol (2-NP), phenol (Ph) and nitrobenzene (NB) from an aqueous environment. Important parameters affecting the absorption phenomena, such as the initial concentration of the organic species and the absorbent, absorption rate, absorption capacity, pH and the temperature of the medium, were evaluated for both hydrogel sizes. The absorption capacity of bulk and microgels were found to be 4-NP>2-NP>Ph>NB. Furthermore, p(4-VP) microgels were embedded in poly(acrylamide) (p(AAm)) bulk hydrogel as a microgel-hydrogel interpenetrating polymer network and proved to be very practical in overcoming the difficulty of using the microgels in real applications. Moreover, it was demonstrated that separately prepared magnetic ferrite particles inserted inside p(4-VP) microgels during synthesis allowed for trouble-free removal of p(4-VP)-magnetic composite microgels from the aqueous environment by an externally applied magnetic field upon completion of their task. Copyright © 2011 Elsevier Ltd. All rights reserved.

Application of the laser induced deflection (LID) technique for low absorption measurements in bulk materials and coatings

NASA Astrophysics Data System (ADS)

Triebel, W.; Mühlig, C.; Kufert, S.

2005-10-01

Precise absorption measurements of bulk materials and coatings upon pulsed ArF laser irradiation are presented using a compact experimental setup based on the laser induced deflection technique (LID). For absorption measurements of bulk materials the influence of pure bulk and pure surface absorption on the temperature and refractive index profile and thus for the probe beam deflection is analyzed in detail. The separation of bulk and surface absorption via the commonly used variation of the sample thickness is carried out for fused silica and calcium fluoride. The experimental results show that for the given surface polishing quality the bulk absorption coefficient of fused silica can be obtained by investigating only one sample. To avoid the drawback of different bulk and surface properties amongst a thickness series, we propose a strategy based on the LID technique to generally obtain surface and bulk absorption separately by investigating only one sample. Apart from measuring bulk absorption coefficients the LID technique is applied to determine the absorption of highly reflecting (HR) coatings on CaF2 substrates. Beside the measuring strategy the experimental results of a AlF3/LaF3 based HR coating are presented. In order to investigate a larger variety of coatings, including high transmitting coatings, a general measuring strategy based on the LID technique is proposed.

Short communication: Repeatability of differential goat bulk milk culture and associations with somatic cell count, total bacterial count, and standard plate count.

PubMed

Koop, G; Dik, N; Nielen, M; Lipman, L J A

2010-06-01

The aims of this study were to assess how different bacterial groups in bulk milk are related to bulk milk somatic cell count (SCC), bulk milk total bacterial count (TBC), and bulk milk standard plate count (SPC) and to measure the repeatability of bulk milk culturing. On 53 Dutch dairy goat farms, 3 bulk milk samples were collected at intervals of 2 wk. The samples were cultured for SPC, coliform count, and staphylococcal count and for the presence of Staphylococcus aureus. Furthermore, SCC (Fossomatic 5000, Foss, Hillerød, Denmark) and TBC (BactoScan FC 150, Foss) were measured. Staphylococcal count was correlated to SCC (r=0.40), TBC (r=0.51), and SPC (r=0.53). Coliform count was correlated to TBC (r=0.33), but not to any of the other variables. Staphylococcus aureus did not correlate to SCC. The contribution of the staphylococcal count to the SPC was 31%, whereas the coliform count comprised only 1% of the SPC. The agreement of the repeated measurements was low. This study indicates that staphylococci in goat bulk milk are related to SCC and make a significant contribution to SPC. Because of the high variation in bacterial counts, repeated sampling is necessary to draw valid conclusions from bulk milk culturing. 2010 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Effects of microstructures on the performance of rare-earth-free MnBi magnetic materials and magnets

NASA Astrophysics Data System (ADS)

Nguyen, Vuong Van; Nguyen, Truong Xuan

2018-03-01

Since the solidification of MnBi alloys is peritectic, their microstructures always consist of the starting phases of Mn and Bi and the productive phase MnBi. The high performance of MnBi bulk magnets requires appropriate routes of preparing MnBi powders of high spontaneous magnetization Ms and large coercivity iHc as well a route of producing bulk magnets thereof. In these routes, the microstructures of arc-melted alloys, annealed alloys and magnets strongly related to the quality of powders and the performance of magnets. The paper proves that: i) The microstructure of fine Mn-inclusions embedded in the matrix of Bi is preferred for arc-melted alloys to realize the rapid evolution of the ferromagnetic phase inside them during their sequent annealing process; ii) The time-controlled annealing process plays a key role in controlling the microstructure with the main ferromagnetic phase matrix, in which the rest of Mn and the Bi accumulations are embedded; iii) The cold (in-liquid-nitrogen) ball milling annealed alloys is required for preparing a high quality powders with the preferred sub-micrometer microstructure without a Bi-decomposition; iv) The short-time warm compaction is crucial to fabricate dense, highly textured bulk magnets with the micrometer microstructure. The realization and control of these preferred microstructures figured in these routes enhance the chance of preparing MnBi bulk magnets with the energy product (BH)max larger than 8 MGOe.

Identification of 210Pb and 210Po in the bulk of copper samples with a low-background alpha particle counter

NASA Astrophysics Data System (ADS)

Abe, K.; Hiraide, K.; Ichimura, K.; Kishimoto, Y.; Kobayashi, K.; Kobayashi, M.; Moriyama, S.; Nakahata, M.; Norita, T.; Ogawa, H.; Sato, K.; Sekiya, H.; Takachio, O.; Takeda, A.; Tasaka, S.; Yamashita, M.; Yang, B. S.; Kim, N. Y.; Kim, Y. D.; Itow, Y.; Kanzawa, K.; Kegasa, R.; Masuda, K.; Takiya, H.; Fushimi, K.; Kanzaki, G.; Martens, K.; Suzuki, Y.; Xu, B. D.; Fujita, R.; Hosokawa, K.; Miuchi, K.; Oka, N.; Takeuchi, Y.; Kim, Y. H.; Lee, K. B.; Lee, M. K.; Fukuda, Y.; Miyasaka, M.; Nishijima, K.; Nakamura, S.

2018-03-01

We established a method to assay 210Pb and 210Po contaminations in the bulk of copper samples using a low-background alpha particle counter. The achieved sensitivity for the 210Pb and 210Po contaminations reaches a few mBq/kg. Due to this high sensitivity, the 210Pb and 210Po contaminations in oxygen free copper bulk were identified and measured for the first time. The 210Pb contaminations of our oxygen free copper samples were 17-40 mBq/kg. Based on our investigation of copper samples in each production step, the 210Pb in oxygen free copper was understood to be a small residual of an electrolysis process. This method to measure bulk contaminations of 210Pb and 210Po could be applied to other materials.

Identification of 210Pb and 210Po in the bulk of copper samples with a low-background alpha particle counter

NASA Astrophysics Data System (ADS)

Kobayashi, Kazuyoshi

2018-01-01

We established a method to assay 210Pb and 210Po contaminations in the bulk of copper samples using a low-background alpha particle counter. The achieved sensitivity for the 210Pb and 210Po contaminations reaches a few mBq/kg. Due to this high sensitivity, the 210Pb and 210Po contaminations in oxygen free copper bulk were identified and measured for the first time. The 210Pb contaminations of our oxygen free copper samples were 17-40 mBq/kg. Based on our investigation of copper samples in each production step, the 210Pb in oxygen free copper was understood to be a small residual of an electrolysis process. This method to measure bulk contaminations of 210Pb and 210Po could be applied to other materials.

Synthesis and Explosive Consolidation of Titanium, Aluminium, Boron and Carbon Containing Powders

NASA Astrophysics Data System (ADS)

Chikhradze, Mikheil; Oniashvili, George; Chikhradze, Nikoloz; D. S Marquis, Fernand

2016-10-01

The development of modern technologies in the field of materials science has increased the interest towards the bulk materials with improved physical, chemical and mechanical properties. Composites, fabricated in Ti-Al-B-C systems are characterized by unique physical and mechanical properties. They are attractive for aerospace, power engineering, machine and chemical applications. The technologies to fabricate ultrafine grained powder and bulk materials in Ti-Al-B-C system are described in the paper. It includes results of theoretical and experimental investigation for selection of powders composition and determination of thermodynamic conditions for bland preparation, as well as optimal technological parameters for mechanical alloying and adiabatic compaction. The crystalline coarse Ti, Al, C powders and amorphous B were used as precursors and blends with different compositions of Ti-Al, Ti-Al-C, Ti-B-C and Ti-Al-B were prepared. Preliminary determination/selection of blend compositions was made on the basis of phase diagrams. The powders were mixed according to the selected ratios of components to produce the blend. Blends were processed in “Fritsch” Planetary premium line ball mill for mechanical alloying, syntheses of new phases, amorphization and ultrafine powder production. The blends processing time was variable: 1 to 20 hours. The optimal technological regimes of nano blend preparation were determined experimentally. Ball milled nano blends were placed in metallic tube and loaded by shock waves for realization of consolidation in adiabatic regime. The structure and properties of the obtained ultrafine grained materials depending on the processing parameters are investigated and discussed. For consolidation of the mixture, explosive compaction technology is applied at room temperatures. The prepared mixtures were located in low carbon steel tube and blast energies were used for explosive consolidation compositions. The relationship of ball milling technological parameters and explosive consolidation conditions on the structure/properties of the obtained samples are described in the paper.

Analysis of Structure and Composition of Bacterial Core Communities in Mature Drinking Water Biofilms and Bulk Water of a Citywide Network in Germany

PubMed Central

Henne, Karsten; Kahlisch, Leila; Brettar, Ingrid

2012-01-01

The bacterial core communities of bulk water and corresponding biofilms of a more than 20-year-old drinking water network were compared using 16S rRNA single-strand confirmation polymorphism (SSCP) fingerprints based on extracted DNA and RNA. The structure and composition of the bacterial core community in the bulk water was highly similar (>70%) across the city of Braunschweig, Germany, whereas all biofilm samples contained a unique community with no overlapping phylotypes from bulk water. Biofilm samples consisted mainly of Alphaproteobacteria (26% of all phylotypes), Gammaproteobacteria (11%), candidate division TM6 (11%), Chlamydiales (9%), and Betaproteobacteria (9%). The bulk water community consisted primarily of Bacteroidetes (25%), Betaproteobacteria (20%), Actinobacteria (16%), and Alphaproteobacteria (11%). All biofilm communities showed higher relative abundances of single phylotypes and a reduced richness compared to bulk water. Only biofilm communities sampled at nearby sampling points showed similar communities irrespective of support materials. In all of our bulk water studies, the community composition determined from 16S rRNA was completely different from the 16S rRNA gene-based community composition, whereas in biofilms both molecular fractions resulted in community compositions that were similar to each other. We hypothesize that a higher fraction of active bacterial phylotypes and a better protection from oxidative stress in drinking water biofilms are responsible for this higher similarity. PMID:22389373

Analysis of structure and composition of bacterial core communities in mature drinking water biofilms and bulk water of a citywide network in Germany.

PubMed

Henne, Karsten; Kahlisch, Leila; Brettar, Ingrid; Höfle, Manfred G

2012-05-01

The bacterial core communities of bulk water and corresponding biofilms of a more than 20-year-old drinking water network were compared using 16S rRNA single-strand confirmation polymorphism (SSCP) fingerprints based on extracted DNA and RNA. The structure and composition of the bacterial core community in the bulk water was highly similar (>70%) across the city of Braunschweig, Germany, whereas all biofilm samples contained a unique community with no overlapping phylotypes from bulk water. Biofilm samples consisted mainly of Alphaproteobacteria (26% of all phylotypes), Gammaproteobacteria (11%), candidate division TM6 (11%), Chlamydiales (9%), and Betaproteobacteria (9%). The bulk water community consisted primarily of Bacteroidetes (25%), Betaproteobacteria (20%), Actinobacteria (16%), and Alphaproteobacteria (11%). All biofilm communities showed higher relative abundances of single phylotypes and a reduced richness compared to bulk water. Only biofilm communities sampled at nearby sampling points showed similar communities irrespective of support materials. In all of our bulk water studies, the community composition determined from 16S rRNA was completely different from the 16S rRNA gene-based community composition, whereas in biofilms both molecular fractions resulted in community compositions that were similar to each other. We hypothesize that a higher fraction of active bacterial phylotypes and a better protection from oxidative stress in drinking water biofilms are responsible for this higher similarity.

Influence of Soap Characteristics and Food Service Facility Type on the Degree of Bacterial Contamination of Open, Refillable Bulk Soaps.

PubMed

Schaffner, Donald W; Jensen, Dane; Gerba, Charles P; Shumaker, David; Arbogast, James W

2018-02-01

Concern has been raised regarding the public health risks from refillable bulk-soap dispensers because they provide an environment for potentially pathogenic bacteria to grow. This study surveyed the microbial quality of open refillable bulk soap in four different food establishment types in three states. Two hundred ninety-six samples of bulk soap were collected from food service establishments in Arizona, New Jersey, and Ohio. Samples were tested for total heterotrophic viable bacteria, Pseudomonas, coliforms and Escherichia coli, and Salmonella. Bacteria were screened for antibiotic resistance. The pH, solids content, and water activity of all soap samples were measured. Samples were assayed for the presence of the common antibacterial agents triclosan and parachlorometaxylenol. More than 85% of the soap samples tested contained no detectable microorganisms, but when a sample contained any detectable microorganisms, it was most likely contaminated at a very high level (∼7 log CFU/mL). Microorganisms detected in contaminated soap included Klebsiella oxytoca, Serratia liquefaciens, Shigella sonnei, Enterobacter gergoviae, Serratia odorifera, and Enterobacter cloacae. Twenty-three samples contained antibiotic-resistant organisms, some of which were resistant to two or more antibiotics. Every sample containing less than 4% solids had some detectable level of bacteria, whereas no samples with greater than 14% solids had detectable bacteria. This finding suggests the use of dilution and/or low-cost formulations as a cause of bacterial growth. There was a statistically significant difference ( P = 0.0035) between the fraction of bacteria-positive samples with no detected antimicrobial agent (17%) and those containing an antimicrobial agent (7%). Fast food operations and grocery stores were more likely to have detectable bacteria in bulk-soap samples compared with convenience stores ( P < 0.05). Our findings underscore the risk to public health from use of refillable bulk-soap dispensers in food service establishments.

The use of bulk collectors in monitoring wet deposition at high-altitude sites in winter

USGS Publications Warehouse

Ranalli, A.J.; Turk, J.T.; Campbell, D.H.

1997-01-01

Concentrations of dissolved ions from samples collected by wet/dry collectors were compared to those collected by bulk collectors at Halfmoon Creek and Ned Wilson Lake in western Colorado to determine if bulk collectors can be used to monitor wet deposition chemistry in remote, high-altitude regions in winter. Hydrogen-ion concentration was significantly lower (p 0.05) at Halfmoon Creek. Wet deposition concentrations were predicated from bulk deposition concentrations through linear regression analysis. Results indicate that anions (chloride, nitrate and sulfate) can be predicted with a high degree of confidence. Lack of significant differences between seasonal (winter and summer) ratios of bulk to wet deposition concentrations indicates that at sites where operation of a wet/dry collector during the winter is not practical, wet deposition concentrations can be predicted from bulk collector samples through regression analysis of wet and bulk deposition data collected during the summer.

Evaluation methods and evaporation conditions for low-resistivity contacts on high Tc superconductors

NASA Astrophysics Data System (ADS)

Liu, Y. P.; Warner, K.; Chan, C.; Chen, K.; Markiewicz, R.

1989-12-01

Low-resistivity contacts to bulk high-Tc superconductors have been prepared by resistive evaporation with values of rho-s (ohm sq cm) as low as 10 to the -10th (77 K) for Ag/YBaCuO, 10 to the -9th (77 K) for Ag/TlPbBaCaCuO, and 10 to the 7th (60 K) for Ag/BiCaSrCuO. It was found that rho-s is improved by increasing the length of a preevaporation step. This effect has been further investigated by secondary ion-mass spectrometry analysis on several Ag/Si samples. Both three-terminal and four-terminal methods have been used to determine rho-s; the three-terminal method shows less dependency on the sample/contact geometry for measurements taken above Tc.

Effect of olive mill waste addition on the properties of porous fired clay bricks using Taguchi method.

PubMed

Sutcu, Mucahit; Ozturk, Savas; Yalamac, Emre; Gencel, Osman

2016-10-01

Production of porous clay bricks lightened by adding olive mill waste as a pore making additive was investigated. Factors influencing the brick manufacturing process were analyzed by an experimental design, Taguchi method, to find out the most favorable conditions for the production of bricks. The optimum process conditions for brick preparation were investigated by studying the effects of mixture ratios (0, 5 and 10 wt%) and firing temperatures (850, 950 and 1050 °C) on the physical, thermal and mechanical properties of the bricks. Apparent density, bulk density, apparent porosity, water absorption, compressive strength, thermal conductivity, microstructure and crystalline phase formations of the fired brick samples were measured. It was found that the use of 10% waste addition reduced the bulk density of the samples up to 1.45 g/cm(3). As the porosities increased from 30.8 to 47.0%, the compressive strengths decreased from 36.9 to 10.26 MPa at firing temperature of 950 °C. The thermal conductivities of samples fired at the same temperature showed a decrease of 31% from 0.638 to 0.436 W/mK, which is hopeful for heat insulation in the buildings. Increasing of the firing temperature also affected their mechanical and physical properties. This study showed that the olive mill waste could be used as a pore maker in brick production. Copyright © 2016 Elsevier Ltd. All rights reserved.

Effect of Soft Phase on Magnetic Properties of Bulk Sm-Co/alpha-Fe Nanocomposite Magnets (Postprint)

DTIC Science & Technology

2012-11-01

plasma sintering , and warm compaction [4][5]–[9]. In our previous study [10], bulk Sm–Co –Fe nanocomposite magnets were fabricated by hot pressing of...no. 5, pp. 2974–2976, Jul. 2003. [8] T. Saito and H. Miyoshi, “Magnetic properties of Sm5Fe17/Fe com- posite magnets produces by spark plasma ...Fe and Fe-Co. Bulk composite magnets have been prepared using compaction techniques such as hot pressing/deforma- tion, dynamic shock compaction, spark

Fabrication and evaluation of low fiber content alumina fiber/aluminum composites

NASA Technical Reports Server (NTRS)

Hack, J. E.; Strempek, G. C.

1980-01-01

The mechanical fabrication of low volume percent fiber, polycrystalline alumina fiber reinforced aluminum composites was accomplished. Wire preform material was prepared by liquid-metal infiltration of alumina fiber bundles. The wires were subsequently encapsulated with aluminum foil and fabricated into bulk composite material by hot-drawing. Extensive mechanical, thermal and chemical testing was conducted on preform and bulk material to develop a process and material data base. In addition, a preliminary investigation of mechanical forming of bulk alumina fiber reinforced aluminum composite material was conducted.

40 CFR 761.265 - Sampling bulk PCB remediation waste and porous surfaces.

Code of Federal Regulations, 2011 CFR

2011-07-01

... 40 Protection of Environment 31 2011-07-01 2011-07-01 false Sampling bulk PCB remediation waste and porous surfaces. 761.265 Section 761.265 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY..., DISTRIBUTION IN COMMERCE, AND USE PROHIBITIONS Cleanup Site Characterization Sampling for PCB Remediation Waste...

40 CFR 761.265 - Sampling bulk PCB remediation waste and porous surfaces.

Code of Federal Regulations, 2014 CFR

2014-07-01

... 40 Protection of Environment 31 2014-07-01 2014-07-01 false Sampling bulk PCB remediation waste and porous surfaces. 761.265 Section 761.265 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY..., DISTRIBUTION IN COMMERCE, AND USE PROHIBITIONS Cleanup Site Characterization Sampling for PCB Remediation Waste...

40 CFR 761.265 - Sampling bulk PCB remediation waste and porous surfaces.

Code of Federal Regulations, 2013 CFR

2013-07-01

... 40 Protection of Environment 32 2013-07-01 2013-07-01 false Sampling bulk PCB remediation waste and porous surfaces. 761.265 Section 761.265 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY..., DISTRIBUTION IN COMMERCE, AND USE PROHIBITIONS Cleanup Site Characterization Sampling for PCB Remediation Waste...

40 CFR 761.265 - Sampling bulk PCB remediation waste and porous surfaces.

Code of Federal Regulations, 2012 CFR

2012-07-01

... 40 Protection of Environment 32 2012-07-01 2012-07-01 false Sampling bulk PCB remediation waste and porous surfaces. 761.265 Section 761.265 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY..., DISTRIBUTION IN COMMERCE, AND USE PROHIBITIONS Cleanup Site Characterization Sampling for PCB Remediation Waste...

Appendix D - Sample Bulk Storage Facility Plan

EPA Pesticide Factsheets

This sample Spill Prevention, Control and Countermeasure (SPCC) Plan in Appendix D is intended to provide examples and illustrations of how a bulk storage facility could address a variety of scenarios in its SPCC Plan.

Investigation of Preparation and Mechanisms of a Dispersed Particle Gel Formed from a Polymer Gel at Room Temperature

PubMed Central

Zhao, Guang; Dai, Caili; Zhao, Mingwei; You, Qing; Chen, Ang

2013-01-01

A dispersed particle gel (DPG) was successfully prepared from a polymer gel at room temperature. The polymer gel system, morphology, viscosity changes, size distribution, and zeta potential of DPG particles were investigated. The results showed that zirconium gel systems with different strengths can be cross-linked within 2.5 h at low temperature. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), and atomic force microscopy (AFM) results showed that the particles were polygonal particles with nano-size distribution. According to the viscosity changes, the whole preparation process can be divided into two major stages: the bulk gel cross-linking reaction period and the DPG particle preparation period. A polymer gel with a 3-dimensional network was formed in the bulk gel cross-linking reaction period whereas shearing force and frictional force were the main driving forces for the preparation of DPG particles, and thus affected the morphology of DPG particles. High shearing force and frictional force reduced the particle size distribution, and then decreased the zeta potential (absolute value). The whole preparation process could be completed within 3 h at room temperature. It could be an efficient and energy-saving technology for preparation of DPG particles. PMID:24324817

Synthesis and Characterization of BaFeO3, (Ba,Bi)FeO3, and Related Epitaxial Thin Films and Nanostructures

DTIC Science & Technology

2009-01-01

measured magnetizations of Ba-doped bulk BiFeO3 samples65, 68 The coercivity, or resistance of the sample to 72 demagnetization , is about 6000 Oe on...methods for sample analysis are briefly discussed. Investigation of BaFeO3 and its structural and magnetic properties, which differ from that of the bulk ...at the atomic level. The interfaces comprised of a magnetic and ferroelectric material layered on one another has great advantage over bulk

Plexcitonics: Coupled and Plasmon-Exciton Systems with Tailorable Properties

DTIC Science & Technology

2013-11-14

demonstrated efficient steam generation from aqueous nanoparticles solutions without heating the bulk volume of the liquid. Application in ethanol ...solutions without heating the bulk volume of the liquid. Applications in ethanol distillation and sanitation have been demonstrated. Key Accomplishments...nanoparticle surface. This state-selective population of adsorbate resonances could be exploited to prepare reactants in specific states on nanoparticle

Quantitation of repaglinide and metabolites in mouse whole-body thin tissue sections using droplet-based liquid microjunction surface sampling-high-performance liquid chromatography-electrospray ionization tandem mass spectrometry.

PubMed

Chen, Weiqi; Wang, Lifei; Van Berkel, Gary J; Kertesz, Vilmos; Gan, Jinping

2016-03-25

Herein, quantitation aspects of a fully automated autosampler/HPLC-MS/MS system applied for unattended droplet-based surface sampling of repaglinide dosed thin tissue sections with subsequent HPLC separation and mass spectrometric analysis of parent drug and various drug metabolites were studied. Major organs (brain, lung, liver, kidney and muscle) from whole-body thin tissue sections and corresponding organ homogenates prepared from repaglinide dosed mice were sampled by surface sampling and by bulk extraction, respectively, and analyzed by HPLC-MS/MS. A semi-quantitative agreement between data obtained by surface sampling and that by employing organ homogenate extraction was observed. Drug concentrations obtained by the two methods followed the same patterns for post-dose time points (0.25, 0.5, 1 and 2 h). Drug amounts determined in the specific tissues was typically higher when analyzing extracts from the organ homogenates. In addition, relative comparison of the levels of individual metabolites between the two analytical methods also revealed good semi-quantitative agreement. Copyright © 2015 Elsevier B.V. All rights reserved.

Quantitation of repaglinide and metabolites in mouse whole-body thin tissue sections using droplet-based liquid microjunction surface sampling-high-performance liquid chromatography-electrospray ionization tandem mass spectrometry

DOE PAGES

Chen, Weiqi; Wang, Lifei; Van Berkel, Gary J.; ...

2015-11-03

Herein, quantitation aspects of a fully automated autosampler/HPLC-MS/MS system applied for unattended droplet-based surface sampling of repaglinide dosed thin tissue sections with subsequent HPLC separation and mass spectrometric analysis of parent drug and various drug metabolites was studied. Major organs (brain, lung, liver, kidney, muscle) from whole-body thin tissue sections and corresponding organ homogenates prepared from repaglinide dosed mice were sampled by surface sampling and by bulk extraction, respectively, and analyzed by HPLC-MS/MS. A semi-quantitative agreement between data obtained by surface sampling and that by employing organ homogenate extraction was observed. Drug concentrations obtained by the two methods followed themore » same patterns for post-dose time points (0.25, 0.5, 1 and 2 h). Drug amounts determined in the specific tissues was typically higher when analyzing extracts from the organ homogenates. Furthermore, relative comparison of the levels of individual metabolites between the two analytical methods also revealed good semi-quantitative agreement.« less

Quantitation of repaglinide and metabolites in mouse whole-body thin tissue sections using droplet-based liquid microjunction surface sampling-high-performance liquid chromatography-electrospray ionization tandem mass spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, Weiqi; Wang, Lifei; Van Berkel, Gary J.

Herein, quantitation aspects of a fully automated autosampler/HPLC-MS/MS system applied for unattended droplet-based surface sampling of repaglinide dosed thin tissue sections with subsequent HPLC separation and mass spectrometric analysis of parent drug and various drug metabolites was studied. Major organs (brain, lung, liver, kidney, muscle) from whole-body thin tissue sections and corresponding organ homogenates prepared from repaglinide dosed mice were sampled by surface sampling and by bulk extraction, respectively, and analyzed by HPLC-MS/MS. A semi-quantitative agreement between data obtained by surface sampling and that by employing organ homogenate extraction was observed. Drug concentrations obtained by the two methods followed themore » same patterns for post-dose time points (0.25, 0.5, 1 and 2 h). Drug amounts determined in the specific tissues was typically higher when analyzing extracts from the organ homogenates. Furthermore, relative comparison of the levels of individual metabolites between the two analytical methods also revealed good semi-quantitative agreement.« less

Use of thermal neutron reflection method for chemical analysis of bulk samples

NASA Astrophysics Data System (ADS)

Papp, A.; Csikai, J.

2014-09-01

Microscopic, σβ, and macroscopic, Σβ, reflection cross-sections of thermal neutrons averaged over bulk samples as a function of thickness (z) are given. The σβ values are additive even for bulk samples in the z=0.5-8 cm interval and so the σβmol(z) function could be given for hydrogenous substances, including some illicit drugs, explosives and hiding materials of ~1000 cm3 dimensions. The calculated excess counts agree with the measured R(z) values. For the identification of concealed objects and chemical analysis of bulky samples, different neutron methods need to be used simultaneously.

Critical assessment of the performance of electronic moisture analyzers for small amounts of environmental samples and biological reference materials.

PubMed

Krachler, M

2001-12-01

Two electronic moisture analyzers were critically evaluated with regard to their suitability for determining moisture in small amounts (< or = 200 mg) of various environmental matrices such as leaves, needles, soil, peat, sediments, and sewage sludge, as well as various biological reference materials. To this end, several homogeneous bulk materials were prepared which were subsequently employed for the development and optimization of all analytical procedures. The key features of the moisture analyzers included a halogen or ceramic heater and an integrated balance with a resolution of 0.1 mg, which is an essential prerequisite for obtaining precise results. Oven drying of the bulk materials in a conventional oven at 105 degrees C until constant mass served as reference method. A heating temperature of 65degrees C was found to provide accurate and precise results for almost all matrices investigated. To further improve the accuracy and precision, other critical parameters such as handling of sample pans, standby temperature, and measurement delay were optimized. Because of its ponderous heating behavior, the performance of the ceramic radiator was inferior to that of the halogen heater, which produced moisture results comparable to those obtained by oven drying. The developed drying procedures were successfully applied to the fast moisture analysis (1.4-6.3 min) of certified biological reference materials of similar provenance to the investigated the bulk materials. Moisture results for 200 mg aliquots ranged from 1.4 to 7.8% and good agreement was obtained between the recommended drying procedure for the reference materials and the electronic moisture analyzers with absolute uncertainties amounting to 0.1% and 0.2-0.3%, respectively.

Lithium Assisted “Dissolution–Alloying” Synthesis of Nanoalloys from Individual Bulk Metals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Barkholtz, Heather M.; Gallagher, James R.; Li, Tao

2016-04-12

We report new fundamental chemistry involved in the synthesis of bimetallic nanoalloys via dissolving the pure bulk transition metals in molten lithium. It is revealed at the atomic level that when two pure bulk transition metals such as Pd and Pt are placed in molten lithium (similar to 200 degrees C), they undergo a dissolution process in which the metal-metal bonds in pure bulk transition metals are completely ruptured, which results in the existence of individual Pd and Pt atoms surrounded by lithium atoms, as is evident by synchrotron X-ray adsorption techniques. Then, upon the conversion of metal lithium tomore » LiOH in humid air, the Pd and Pt atoms undergo an alloying process to aggregate into nanoalloys. This method was further expanded to include PdZn, which is notoriously difficult to prepare via traditional nanoalloy synthesis methods due to the easily oxidizable Zn component. The constantly reducing environment of metallic Li allowed for preparation of PdZn nanoalloys with minimal Zn oxidation via dissolution-alloying of individual bulk transition metals in molten lithium. Additionally, this lithium assisted "dissolution-alloying" method bypasses many complications intrinsic to conventional ion reduction-based nanoalloy synthesis including the necessity of ligated metal ions, the use of proper reducing agents and dispersing surfactants, and the presence of segregated phases due to different reduction potentials of the constituent metal ions.« less

Lithium assisted “dissolution–alloying” synthesis of nanoalloys from individual bulk metals

DOE PAGES

Barkholtz, Heather M.; Gallagher, James R.; Li, Tao; ...

2016-03-27

Here, we report new fundamental chemistry involved in the synthesis of bimetallic nanoalloys via dissolving the pure bulk transition metals in molten lithium. It is revealed at the atomic level that when two pure bulk transition metals such as Pd and Pt are placed in molten lithium (~200°C), they undergo a dissolution process in which the metal-metal bonds in pure bulk transition metals are completely ruptured, resulting in the existence of individual Pd and Pt atoms surrounded by lithium atoms, as is evident by synchrotron Xray adsorption techniques. Then, upon the conversion of metal lithium to LiOH in humid air,more » the Pd and Pt atoms undergo an alloying process, to aggregate into nanoalloys. This method was further expanded to include PdZn, which is notoriously difficult to prepare via traditional nanoalloy synthesis methods due to the easily oxidizable Zn component. The constantly reducing environment of metallic Li allowed for preparation of PdZn nanoalloys with minimal Zn oxidation via dissolution-alloying of individual bulk transition metals in molten lithium. Additionally, this lithium assisted “dissolutionalloying” method bypasses many complications intrinsic to conventional ion reductionbased nanoalloy synthesis including the necessity of ligated metal ions, the use of proper reducing agents and dispersing surfactants, and the presence of segregated phases due to different reduction potentials of the constituent metal ions.« less

Microplastic analysis in the South Funen Archipelago, Baltic Sea, implementing manta trawling and bulk sampling.

PubMed

Tamminga, Matthias; Hengstmann, Elena; Fischer, Elke Kerstin

2018-03-01

Microplastic contamination in surface waters of the South Funen Archipelago in Denmark was assessed. Therefore, ten manta trawls were conducted in June 2015. Moreover, 31 low-volume bulk samples were taken to evaluate, whether consistent results in comparison to the net-based approach can be obtained. Microplastic contamination in the South Funen Archipelago (0.07 ± 0.02 particles/m3) is slightly below values reported before. The sheltered position of the study area, low population pressure on adjacent islands and the absence of any major potential point sources were identified as major factors explaining the low concentration of microplastics. Within the Archipelago, harbors or marinas and the associated vessel traffic are the most probable sources of microplastics. The concentration of microplastics in low-volume bulk samples is not comparable to manta trawl results. This is mainly due to insufficient representativeness of the bulk sample volumes.

Preparation of electrochemically active silicon nanotubes in highly ordered arrays

PubMed Central

Grünzel, Tobias; Lee, Young Joo; Kuepper, Karsten

2013-01-01

Summary Silicon as the negative electrode material of lithium ion batteries has a very large capacity, the exploitation of which is impeded by the volume changes taking place upon electrochemical cycling. A Si electrode displaying a controlled porosity could circumvent the difficulty. In this perspective, we present a preparative method that yields ordered arrays of electrochemically competent silicon nanotubes. The method is based on the atomic layer deposition of silicon dioxide onto the pore walls of an anodic alumina template, followed by a thermal reduction with lithium vapor. This thermal reduction is quantitative, homogeneous over macroscopic samples, and it yields amorphous silicon and lithium oxide, at the exclusion of any lithium silicides. The reaction is characterized by spectroscopic ellipsometry for thin silica films, and by nuclear magnetic resonance and X-ray photoelectron spectroscopy for nanoporous samples. After removal of the lithium oxide byproduct, the silicon nanotubes can be contacted electrically. In a lithium ion electrolyte, they then display the electrochemical waves also observed for other bulk or nanostructured silicon systems. The method established here paves the way for systematic investigations of how the electrochemical properties (capacity, charge/discharge rates, cyclability) of nanoporous silicon negative lithium ion battery electrode materials depend on the geometry. PMID:24205460

Nanocrystalline silicon: Lattice dynamics and enhanced thermoelectric properties

DOE PAGES

Claudio, Tania; Stein, Niklas; Stroppa, Daniel G.; ...

2014-12-21

In this study, silicon has several advantages when compared to other thermoelectric materials, but until recently it was not used for thermoelectric applications due to its high thermal conductivity, 156 W K -1 m -1 at room temperature. Nanostructuration as means to decrease thermal transport through enhanced phonon scattering has been a subject of many studies. In this work we have evaluated the effects of nanostructuration on the lattice dynamics of bulk nanocrystalline doped silicon. The samples were prepared by gas phase synthesis, followed by current and pressure assisted sintering. The heat capacity, density of phonons states, and elastic constantsmore » were measured, which all reveal a significant, ≈25%, reduction in the speed of sound. The samples present a significantly decreased lattice thermal conductivity, ≈25 W K -1 m -1, which, combined with a very high carrier mobility, results in a dimensionless figure of merit with a competitive value that peaks at ZT ≈ 0.57 at 973 °C. Due to its easily scalable and extremely low-cost production process, nanocrystalline Si prepared by gas phase synthesis followed by sintering could become the material of choice for high temperature thermoelectric generators.« less

Enhanced Raman spectroscopy of 2,4,6-TNT in anatase and rutile titania nanocrystals

NASA Astrophysics Data System (ADS)

De La Cruz-Montoya, Edwin; Jeréz, Jaqueline I.; Balaguera-Gelves, Marcia; Luna-Pineda, Tatiana; Castro, Miguel E.; Hernández-Rivera, Samuel P.

2006-05-01

The majority of explosives found in antipersonnel and antitank landmines contain 2,4,6-trinitrotoluene (TNT). Chemical sensing of landmines and Improvised Explosive Devices (IED) requires detecting the chemical signatures of the explosive components in these devices. Nanotechnology is ideally suited to needs in microsensors development by providing new materials and methods that can be employed for trace explosive detection. This work is focused on modification of nano-scaled colloids of titanium dioxide (Titania: anatase, rutile and brookite) and thin layer of the oxides as substrates for use in Enhanced Raman Scattering (ERS) spectroscopy. Ultrafine particles have been generated by hydrothermally treating the sol-gel derived hydrous oxides. ERS spectra of nanocrystalline anatase Titania samples prepared with different average sizes: 38 nm (without acid), 24 nm (without acid) and 7 nm (with HCl). Bulk phase (commercial) and KBr were also used to prepare mixtures with TNT to look for Enhanced Raman Effect of the nitroaromatic explosive on the test surfaces. The studies clearly indicated that the anatase crystal size affects the enhancement of the TNT Raman signal. This enhancement was highest for the samples with Titania average crystal size of 7 nm.

Shear bond strength of bulk-fill and nano-restorative materials to dentin.

PubMed

Colak, Hakan; Ercan, Ertugrul; Hamidi, Mehmet Mustafa

2016-01-01

Bulk-fill composite materials are being developed for preparation depths of up to 4 mm in an effort to simplify and improve the placement of direct composite posterior restorations. The aim of our study was to compare shear-bond strength of bulk-fill and conventional posterior composite resins. In this study, 60 caries free extracted human molars were used and sectioned parallel to occlusal surface to expose midcoronal dentin. The specimens were randomly divided into four groups. Total-etch dentine bonding system (Adper Scotchbond 1XT, 3M ESPE) was applied to dentin surface in all the groups to reduce variability in results. Then, dentine surfaces covered by following materials. Group I: SonicFill Bulk-Fill, Group II: Tetric EvoCeram (TBF), Group III: Herculite XRV Ultra, and Group IV: TBF Bulk-Fill, 2 mm × 3 mm cylindrical restorations were prepared by using application apparatus. Shear bond testing was measured by using a universal testing machine. Kruskal-Wallis and Mann-Whitney U-tests were performed to evaluate the data. The highest value was observed in Group III (14.42 ± 4.34) and the lowest value was observed in Group IV (11.16 ± 2.76) and there is a statistically significant difference between these groups (P = 0.046). However, there is no statistically significant difference between the values of other groups. In this study, Group III was showed higher strength values. There is a need for future studies about long-term bond strength and clinical success of these adhesive and bulk-fill systems.

A superconducting conveyer system using multiple bulk Y-Ba-Cu-O superconductors and permanent magnets

NASA Astrophysics Data System (ADS)

Kinoshita, T.; Koshizuka, N.; Nagashima, K.; Murakami, M.

Developments of non-contact superconducting devices like superconducting magnetic levitation transfer and superconducting flywheel energy storage system have been performed based on the interactions between bulk Y-Ba-Cu-O superconductors and permanent magnets, in that the superconductors can stably be levitated without any active control. The performances of noncontact superconducting devices are dependent on the interaction forces like attractive forces and stiffness. In the present study, we constructed a non-contact conveyer for which the guide rails were prepared by attaching many Fe-Nd-B magnets onto an iron base plate. Along the translational direction, all the magnets were arranged as to face the same pole, and furthermore their inter-distance was made as small as possible. The guide rail has three magnet rows, for which the magnets were glued on the iron plate such that adjacent magnet rows have opposite poles like NSN. At the center row, the magnetic field at zero gap reached 0.61T, while the field strengths of two rows on the side edges were only 0.48T due to magnetic interactions among permanent magnets. We then prepared a cryogenic box made with FRP that can store several bulk Y-Ba-Cu-O superconductors 25 mm in diameter cooled by liquid nitrogen. It was found that the levitation forces and stiffness increased with increasing the number of bulk superconductors installed in the box, although the levitation force per unit bulk were almost the same. We also confirmed that these forces are dependent on the configuration of bulk superconductors.

Estimation of the deoxynivalenol and moisture contents of bulk wheat grain samples by FT-NIR spectroscopy

USDA-ARS?s Scientific Manuscript database

Deoxynivalenol (DON) levels in harvested grain samples are used to evaluate the Fusarium head blight (FHB) resistance of wheat cultivars and breeding lines. Fourier transform near-infrared (FT-NIR) calibrations were developed to estimate the DON and moisture content (MC) of bulk wheat grain samples ...

Measured acoustic properties of variable and low density bulk absorbers

NASA Technical Reports Server (NTRS)

Dahl, M. D.; Rice, E. J.

1985-01-01

Experimental data were taken to determine the acoustic absorbing properties of uniform low density and layered variable density samples using a bulk absober with a perforated plate facing to hold the material in place. In the layered variable density case, the bulk absorber was packed such that the lowest density layer began at the surface of the sample and progressed to higher density layers deeper inside. The samples were placed in a rectangular duct and measurements were taken using the two microphone method. The data were used to calculate specific acoustic impedances and normal incidence absorption coefficients. Results showed that for uniform density samples the absorption coefficient at low frequencies decreased with increasing density and resonances occurred in the absorption coefficient curve at lower densities. These results were confirmed by a model for uniform density bulk absorbers. Results from layered variable density samples showed that low frequency absorption was the highest when the lowest density possible was packed in the first layer near the exposed surface. The layers of increasing density within the sample had the effect of damping the resonances.

Guideline on Isotope Dilution Mass Spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gaffney, Amy

Isotope dilution mass spectrometry is used to determine the concentration of an element of interest in a bulk sample. It is a destructive analysis technique that is applicable to a wide range of analytes and bulk sample types. With this method, a known amount of a rare isotope, or ‘spike’, of the element of interest is added to a known amount of sample. The element of interest is chemically purified from the bulk sample, the isotope ratio of the spiked sample is measured by mass spectrometry, and the concentration of the element of interest is calculated from this result. Thismore » method is widely used, although a mass spectrometer required for this analysis may be fairly expensive.« less

Fast Scanning Calorimetry Studies of Supercooled Liquids and Glasses

NASA Astrophysics Data System (ADS)

Bhattacharya, Deepanjan

This dissertation is a compilation of research results of extensive Fast Scanning Calorimetry studies of two non-crystalline materials: Toluene and Water. Motivation for fundamental studies of non-crystalline phases, a brief overview of glassy materials and concepts and definitions related to them is provided in Chapter 1. Chapter 2 provides fundamentals and details of experimental apparata, experimental protocol and calibration procedure. Chapter 3 & 4 provides extensive studies of stable non-crystalline toluene films of micrometer and nanometer thicknesses grown by vapor deposition at distinct deposition rates and temperatures and probed by Fast Scanning Calorimetry. Fast scanning calorimetry is shown to be extremely sensitive to the structure of the vapor-deposited phase and was used to characterize simultaneously its kinetic stability and its thermodynamic properties. According to our analysis, transformation of vapor -deposited samples of toluene during heating with rates in excess 100,000 K/s follows the zero-order kinetics. The transformation rate correlates strongly with the initial enthalpy of the sample, which increases with the deposition rate according to sub-linear law. Analysis of the transformation kinetics of vapor deposited toluene films of various thicknesses reveal a sudden increase in the transformation rate for films thinner than 250 nm. The change in kinetics correlates with the surface roughness scale of the substrate, which is interpreted as evidence for kinetic anisotropy of the samples. We also show that out-of-equilibrium relaxation kinetics and possibly the enthalpy of vapor-deposited (VD) films of toluene are distinct from those of ordinary supercooled (OS) phase even when the deposition takes place at temperatures above the glass softening (Tg). The implications of these findings for the formation mechanism and structure of vapor deposited stable glasses are discussed. Chapter 5 and 6 provide detailed Fast Scanning Calorimetry studies of amorphous solid water in bulk and confining geometry (ultrathin films and nano-aggregates). Bulk-like water samples were prepared by vapor-deposition on the surface of a tungsten filament near 140 K where vapor-deposition results in low enthalpy glassy water films. The vapor deposition approach was also used to grow nano-aggregates (2- 20 nm thick) and multiple ultrathin (approximately 50 nm thick) water films alternated with benzene and methanoic films of similar dimensions. When heated from cryogenic temperatures, the ultrathin water films underwent a well manifested glass softening transition at temperatures 20 degrees below the onset of crystallization. The thermograms of nano-aggregates of ASW films show two endotherms at 40 and 10 K below the onset temperatures of crystallization. However, no such transition was observed in bulk-like water samples prior to their crystallization. These results indicate that water in confined geometry demonstrates glass softening dynamics which are dramatically distinct from those of the bulk phase. We attribute these differences to water's interfacial glass transition which occurs at temperatures tens of degrees lower than that in the bulk. Implications of these finding for past studies of glass softening dynamics in various glassy water samples are discussed in chapter 5 and 6.

Stress remagnetization in pyrrhotite-calcite synthetic aggregates

NASA Astrophysics Data System (ADS)

Robion, Philippe; Borradaile, Graham J.

2001-01-01

Stress-induced remagnetization has been applied to multidomain pyrrhotite-calcite synthetic aggregates in a triaxial rig. Experimental deformation used 150MPa confining pressure, a constant strain rate of 10-5 s-1 and applied differential stresses of up to 70MPa. New components of magnetization, parallel to the direction of the pressure vessel field, were added to the pre-deformational magnetization. The intensity of remagnetization (M'-M0) increases with the intensity of the applied differential stress and affects the coercivity fraction below 15mT. Bulk shortening is less than 8 per cent, thus grain rotation cannot explain selective remagnetization of the low-coercivity fraction. Remagnetization is thus attributed to deformational viscous remanent magnetization (DVRM). It is observed that high-coercivity (>15mT) grains do not remagnetize. There is, however, slight progressive rotation of pre-deformational magnetization with increasing strain up to 8 per cent of bulk shortening. The lack of piezoremanent magnetization in the high-coercivity range may be due to defects introduced in pyrrhotite during sample preparation. Experiments using synthetic pyrrhotite, expected to show low dislocation densities, would be necessary to test this effect.

Interface spins in polycrystalline FeMn/Fe bilayers with small exchange bias

NASA Astrophysics Data System (ADS)

Pires, M. J. M.

2018-04-01

The magnetic moments at the interface between ferromagnetic and antiferromagnetic layers play a central role in exchange biased systems, but their behavior is still not completely understood. In this work, the FeMn/Fe interface in polycrystalline thin films has been studied using conversion electron Mössbauer spectroscopy (CEMS), magneto-optic Kerr effect (MOKE) and micromagnetic simulations. Samples were prepared with 57Fe layers at two distinct depths in order to probe the interface and bulk behaviors. At the equilibrium, the interface moments are randomly oriented while the bulk of the Fe layer has an in-plane magnetic anisotropy. Several models for the interface and anisotropies of the layers were used in the simulations of spin configurations and hysteresis loops. From the whole set of simulations, one can conclude the direct analysis of hysteresis curves is not enough to infer whether the interface has a configuration with spins tilted out of the film plane at equilibrium since different choices of parameters provide similar curves. The simulations have also shown the occurrence of spin clusters at the interface is compatible with CEMS and MOKE measurements.

Non-conventional photocathodes based on Cu thin films deposited on Y substrate by sputtering

NASA Astrophysics Data System (ADS)

Perrone, A.; D'Elia, M.; Gontad, F.; Di Giulio, M.; Maruccio, G.; Cola, A.; Stankova, N. E.; Kovacheva, D. G.; Broitman, E.

2014-07-01

Copper (Cu) thin films were deposited on yttrium (Y) substrate by sputtering. During the deposition, a small central area of the Y substrate was shielded to avoid the film deposition and was successively used to study its photoemissive properties. This configuration has two advantages: the cathode presents (i) the quantum efficiency and the work function of Y and (ii) high electrical compatibility when inserted into the conventional radio-frequency gun built with Cu bulk. The photocathode was investigated by scanning electron microscopy to determine surface morphology. X-ray diffraction and atomic force microscopy studies were performed to compare the structure and surface properties of the deposited film. The measured electrical resistivity value of the Cu film was similar to that of high purity Cu bulk. Film to substrate adhesion was also evaluated using the Daimler-Benz Rockwell-C adhesion test method. Finally, the photoelectron performance in terms of quantum efficiency was obtained in a high vacuum photodiode cell before and after laser cleaning procedures. A comparison with the results obtained with a twin sample prepared by pulsed laser deposition is presented and discussed.

High thermal behavior of a new glass ceramic developed from silica xerogel/SnO{sub 2} composite

DOE Office of Scientific and Technical Information (OSTI.GOV)

Aripin, H., E-mail: aripin@unsil.ac.id; Mitsudo, Seitaro, E-mail: mitsudo@fir.u-fukui.ac.jp; Sudiana, I. Nyoman, E-mail: sudiana75@yahoo.com

2016-02-08

In this investigation, a new glass ceramics have been produced by mixing SnO{sub 2} and amorphous silica xerogel (ASX) extracted from sago waste ash. The composition has been prepared by adding 10 mol% of SnO{sub 2} into SX. The samples have been dry pressed and sintered in the temperature range between 800 °C and 1500 °C. The effects of temperature on the crystallization of silica xerogel after adding SnO{sub 2} and their relationship to bulk density have been studied. The crystallization process of the silica xerogel/SnO{sub 2} composite has been examined by an X-ray diffraction (XRD) and the bulk density hasmore » been characterized on the basis of the experimental data obtained using Archimedes′ principle. It has been found that an addition of SnO{sub 2} confers an appreciable effect on the grain and from the interpretation of XRD patterns allow one to explain the increase in the density by an increased crystallite size of SnO{sub 2} in the composite.« less

High thermal behavior of a new glass ceramic developed from silica xerogel/SnO2 composite

NASA Astrophysics Data System (ADS)

Aripin, H.; Mitsudo, Seitaro; Sudiana, I. Nyoman; Priatna, Edvin; Sabchevski, Svilen

2016-02-01

In this investigation, a new glass ceramics have been produced by mixing SnO2 and amorphous silica xerogel (ASX) extracted from sago waste ash. The composition has been prepared by adding 10 mol% of SnO2 into SX. The samples have been dry pressed and sintered in the temperature range between 800 °C and 1500 °C. The effects of temperature on the crystallization of silica xerogel after adding SnO2 and their relationship to bulk density have been studied. The crystallization process of the silica xerogel/SnO2 composite has been examined by an X-ray diffraction (XRD) and the bulk density has been characterized on the basis of the experimental data obtained using Archimedes' principle. It has been found that an addition of SnO2 confers an appreciable effect on the grain and from the interpretation of XRD patterns allow one to explain the increase in the density by an increased crystallite size of SnO2 in the composite.

Structure-Dependent Optical Properties of Self-Organized Bi2Se3 Nanostructures: From Nanocrystals to Nanoflakes.

PubMed

Yang, Shang-Dong; Yang, Liao; Zheng, Yu-Xiang; Zhou, Wen-Jie; Gao, Meng-Yu; Wang, Song-You; Zhang, Rong-Jun; Chen, Liang-Yao

2017-08-30

Bismuth selenide (Bi 2 Se 3 ), with a wide bulk band gap and single massless Dirac cone at the surface, is a promising three-dimensional topological insulator. Bi 2 Se 3 possesses gapless surface states and an insulator-like bulk band gap as a new type of quantum matter. Different Bi 2 Se 3 nanostructures were prepared using electron beam evaporation with high production efficiency. Structural investigations by energy-dispersive X-ray analysis, scanning electron microscopy, and X-ray diffraction revealed the sample stoichiometries and the structural transition mechanism from nanocrystals to nanoflakes. The optical properties systematically probed and analyzed by spectroscopic ellipsometry showed strong dependence on the nanostructures and were also predicted to have structure-modifiable technological prospects. The optical parameters, plasma frequencies, scattering rates of the free electrons, and optical band gaps were related to the topological properties of the Bi 2 Se 3 nanostructures via light-matter interactions, offering new opportunities and approaches for studies on topological insulators and spintronics. The high-quality Bi 2 Se 3 nanostructures provide advantages in exploring novel physics and exploiting prospective applications.

Boron Arsenide and Boron Phosphide for High Temperature and Luminescent Devices. [semiconductor devices - crystal growth/crystal structure

NASA Technical Reports Server (NTRS)

Chu, T. L.

1975-01-01

The crystal growth of boron arsenide and boron phosphide in the form of bulk crystals and epitaxial layers on suitable substrates is discussed. The physical, chemical, and electrical properties of the crystals and epitaxial layers are examined. Bulk crystals of boron arsenide were prepared by the chemical transport technique, and their carrier concentration and Hall mobility were measured. The growth of boron arsenide crystals from high temperature solutions was attempted without success. Bulk crystals of boron phosphide were also prepared by chemical transport and solution growth techniques. Techniques required for the fabrication of boron phosphide devices such as junction shaping, diffusion, and contact formation were investigated. Alloying techniques were developed for the formation of low-resistance ohmic contacts to boron phosphide. Four types of boron phosphide devices were fabricated: (1) metal-insulator-boron phosphide structures, (2) Schottky barriers; (3) boron phosphide-silicon carbide heterojunctions; and (4) p-n homojunctions. Easily visible red electroluminescence was observed from both epitaxial and solution grown p-n junctions.

Effect of sample thickness on the extracted near-infrared bulk optical properties of Bacillus subtilis in liquid culture.

PubMed

Dzhongova, Elitsa; Harwood, Colin R; Thennadil, Suresh N

2011-11-01

In order to determine the bulk optical properties of a Bacillus subtilis culture during growth phase we investigated the effect of sample thickness on measurements taken with different measurement configurations, namely total diffuse reflectance and total diffuse transmittance. The bulk optical properties were extracted by inverting the measurements using the radiative transfer theory. While the relationship between reflectance and biomass changes with sample thickness and the intensity (absorbance) levels vary significantly for both reflectance and transmittance measurements, the extracted optical properties show consistent behavior in terms of both the relationship with biomass and magnitude. This observation indicates the potential of bulk optical properties for building models that could be more easily transferable compared to those built using raw measurements.

Study on the influence of X-ray tube spectral distribution on the analysis of bulk samples and thin films: Fundamental parameters method and theoretical coefficient algorithms

NASA Astrophysics Data System (ADS)

Sitko, Rafał

2008-11-01

Knowledge of X-ray tube spectral distribution is necessary in theoretical methods of matrix correction, i.e. in both fundamental parameter (FP) methods and theoretical influence coefficient algorithms. Thus, the influence of X-ray tube distribution on the accuracy of the analysis of thin films and bulk samples is presented. The calculations are performed using experimental X-ray tube spectra taken from the literature and theoretical X-ray tube spectra evaluated by three different algorithms proposed by Pella et al. (X-Ray Spectrom. 14 (1985) 125-135), Ebel (X-Ray Spectrom. 28 (1999) 255-266), and Finkelshtein and Pavlova (X-Ray Spectrom. 28 (1999) 27-32). In this study, Fe-Cr-Ni system is selected as an example and the calculations are performed for X-ray tubes commonly applied in X-ray fluorescence analysis (XRF), i.e., Cr, Mo, Rh and W. The influence of X-ray tube spectra on FP analysis is evaluated when quantification is performed using various types of calibration samples. FP analysis of bulk samples is performed using pure-element bulk standards and multielement bulk standards similar to the analyzed material, whereas for FP analysis of thin films, the bulk and thin pure-element standards are used. For the evaluation of the influence of X-ray tube spectra on XRF analysis performed by theoretical influence coefficient methods, two algorithms for bulk samples are selected, i.e. Claisse-Quintin (Can. Spectrosc. 12 (1967) 129-134) and COLA algorithms (G.R. Lachance, Paper Presented at the International Conference on Industrial Inorganic Elemental Analysis, Metz, France, June 3, 1981) and two algorithms (constant and linear coefficients) for thin films recently proposed by Sitko (X-Ray Spectrom. 37 (2008) 265-272).

On the role of API in determining porosity, pore structure and bulk modulus of the skeletal material in pharmaceutical tablets formed with MCC as sole excipient.

PubMed

Ridgway, Cathy; Bawuah, Prince; Markl, Daniel; Zeitler, J Axel; Ketolainen, Jarkko; Peiponen, Kai-Erik; Gane, Patrick

2017-06-30

The physical properties and mechanical integrity of pharmaceutical tablets are of major importance when loading with active pharmaceutical ingredient(s) (API) in order to ensure ease of processing, control of dosage and stability during transportation and handling prior to patient consumption. The interaction between API and excipient, acting as functional extender and binder, however, is little understood in this context. The API indomethacin is combined in this study with microcrystalline cellulose (MCC) at increasing loading levels. Tablets from the defined API/MCC ratios are made under conditions of controlled porosity and tablet thickness, resulting from different compression conditions, and thus compaction levels. Mercury intrusion porosimetry is used to establish the accessible pore volume, pore size distribution and, adopting the observed region of elastic intrusion-extrusion at high pressure, an elastic bulk modulus of the skeletal material is recorded. Porosity values are compared to previously published values derived from terahertz (THz) refractive index data obtained from exactly the same tablet sample sets. It is shown that the elastic bulk modulus is dependent on API wt% loading under constant tablet preparation conditions delivering equal dimensions and porosity. The findings are considered of novel value in respect to establishing consistency of tablet production and optimisation of physical properties. Copyright © 2017 Elsevier B.V. All rights reserved.

X-Ray Nanoscopy of a Bulk Heterojunction

NASA Astrophysics Data System (ADS)

Patil, Nilesh; Torbjørn, Eirik; Skjønsfjell, Bakken; Van den Brande, Niko; Chavez Panduro, Elvia Anabela; Claessens, Raf; Guizar-Sicairos, Manuel; Van Mele, Bruno; Breiby, Dag Werner

2016-07-01

Optimizing the morphology of bulk heterojunctions is known to significantly improve the photovoltaic performance of organic solar cells, but available quantitative imaging techniques are few and have severe limitations. We demonstrate X-ray ptychographic coherent diffractive imaging applied to all-organic blends. Specifically, the phase-separated morphology in bulk heterojunction photoactive layers for organic solar cells, prepared from a 50:50 blend of poly(3-hexylthiophene) (P3HT) and phenyl-C61-butyric acid methyl ester (PCBM) and thermally treated for different annealing times is imaged to high resolution. Moreover, using a fast-scanning calorimetry chip setup, the nano-morphological changes caused by repeated thermal annealing applied to the same sample could be monitored. X-ray ptychography resolves to better than 100 nm the phase-segregated domains of electron donor and electron acceptor materials over a large field of view within the active layers. The quantitative phase contrast images further allow us to estimate the local volume fraction of PCBM across the photovoltaically active layers. The volume fraction gradient for different regions provides insight on the PCBM diffusion across the depletion zone surrounding PCBM aggregates. Phase contrast X-ray microscopy is under rapid development, and the results presented here are promising for future studies of organic-organic blends, also under in situ conditions, e.g., for monitoring the structural stability during UV-Vis irradiation.

X-Ray Nanoscopy of a Bulk Heterojunction.

PubMed

Patil, Nilesh; Skjønsfjell, Eirik Torbjørn Bakken; Van den Brande, Niko; Chavez Panduro, Elvia Anabela; Claessens, Raf; Guizar-Sicairos, Manuel; Van Mele, Bruno; Breiby, Dag Werner

2016-01-01

Optimizing the morphology of bulk heterojunctions is known to significantly improve the photovoltaic performance of organic solar cells, but available quantitative imaging techniques are few and have severe limitations. We demonstrate X-ray ptychographic coherent diffractive imaging applied to all-organic blends. Specifically, the phase-separated morphology in bulk heterojunction photoactive layers for organic solar cells, prepared from a 50:50 blend of poly(3-hexylthiophene) (P3HT) and phenyl-C61-butyric acid methyl ester (PCBM) and thermally treated for different annealing times is imaged to high resolution. Moreover, using a fast-scanning calorimetry chip setup, the nano-morphological changes caused by repeated thermal annealing applied to the same sample could be monitored. X-ray ptychography resolves to better than 100 nm the phase-segregated domains of electron donor and electron acceptor materials over a large field of view within the active layers. The quantitative phase contrast images further allow us to estimate the local volume fraction of PCBM across the photovoltaically active layers. The volume fraction gradient for different regions provides insight on the PCBM diffusion across the depletion zone surrounding PCBM aggregates. Phase contrast X-ray microscopy is under rapid development, and the results presented here are promising for future studies of organic-organic blends, also under in situ conditions, e.g., for monitoring the structural stability during UV-Vis irradiation.

Rapid Assessment of the Ce-Co-Fe-Cu System for Permanent Magnetic Applications

NASA Astrophysics Data System (ADS)

Meng, F.; Chaudhary, R. P.; Gandha, K.; Nlebedim, I. C.; Palasyuk, A.; Simsek, E.; Kramer, M. J.; Ott, R. T.

2018-06-01

This work focuses on the rapid synthesis and characterization of quaternary Ce(CoFeCu)5 alloy libraries to assess their potential viability as permanent magnets. Arrays of bulk specimens with controlled compositions were synthesized via laser engineered net shaping (LENS) by feeding different ratios of alloy powders into a melt pool created by a laser. Based on the assessment of the magnetic properties of the LENS printed samples, arc-melted and cast ingots were prepared with varying Fe (5-20 at.%) and Co (60-45 at.%) compositions while maintaining constant Ce (16 at.%) and Cu (19 at.%) content. The evolution of the microstructure and phases with varying chemical compositions and their dependence on magnetic properties are analyzed in as-cast and heat-treated samples. In both the LENS printed and cast samples, we find the best magnetic properties correspond to a predominantly single-phase Ce(CoFeCu)5 microstructure in which high coercivity ( H c > 10 kOe) can be achieved without any microstructural refinement.

Practicable group testing method to evaluate weight/weight GMO content in maize grains.

PubMed

Mano, Junichi; Yanaka, Yuka; Ikezu, Yoko; Onishi, Mari; Futo, Satoshi; Minegishi, Yasutaka; Ninomiya, Kenji; Yotsuyanagi, Yuichi; Spiegelhalter, Frank; Akiyama, Hiroshi; Teshima, Reiko; Hino, Akihiro; Naito, Shigehiro; Koiwa, Tomohiro; Takabatake, Reona; Furui, Satoshi; Kitta, Kazumi

2011-07-13

Because of the increasing use of maize hybrids with genetically modified (GM) stacked events, the established and commonly used bulk sample methods for PCR quantification of GM maize in non-GM maize are prone to overestimate the GM organism (GMO) content, compared to the actual weight/weight percentage of GM maize in the grain sample. As an alternative method, we designed and assessed a group testing strategy in which the GMO content is statistically evaluated based on qualitative analyses of multiple small pools, consisting of 20 maize kernels each. This approach enables the GMO content evaluation on a weight/weight basis, irrespective of the presence of stacked-event kernels. To enhance the method's user-friendliness in routine application, we devised an easy-to-use PCR-based qualitative analytical method comprising a sample preparation step in which 20 maize kernels are ground in a lysis buffer and a subsequent PCR assay in which the lysate is directly used as a DNA template. This method was validated in a multilaboratory collaborative trial.

Characterization of stoichiometric nanocrystalline spinel ferrites dispersed on porous silica aerogel.

PubMed

Casula, M F; Concas, G; Congiu, F; Corrias, A; Loche, D; Marras, C; Spano, G

2011-11-01

Stoichiometric magnetic nanosized ferrites MFe2O4 (M = Mn, Co, Ni) were prepared in form of nearly spherical nanocrystals supported on a highly porous silica aerogel matrix, by a sol-gel procedure. X-ray diffraction and transmission electron microscopy indicate that these materials are made out of non-agglomerated ferrite nanocrystals having size in the 5-10 nm range. Investigation by Mössbauer Spectroscopy was used to gain insights on the superparamagnetic relaxation and on the inversion degree. Magnetic ordering at room temperature varies from superparamagnetic in the NiFe2O4 sample, highly blocked (approximately 70%) in the MnFe2O4 sample and nearly fully blocked in the CoFe2O4 sample. A fitting procedure of the Mössbauer data has been used in order to resolve the spectrum into the tetrahedral and octahedral components; in this way, an inversion degree of 0.68 (very close to bulk values) was obtained for 6 nm silica-supported CoFe2O4 nanocrystals.

Rapid Assessment of the Ce-Co-Fe-Cu System for Permanent Magnetic Applications

NASA Astrophysics Data System (ADS)

Meng, F.; Chaudhary, R. P.; Gandha, K.; Nlebedim, I. C.; Palasyuk, A.; Simsek, E.; Kramer, M. J.; Ott, R. T.

2018-04-01

This work focuses on the rapid synthesis and characterization of quaternary Ce(CoFeCu)5 alloy libraries to assess their potential viability as permanent magnets. Arrays of bulk specimens with controlled compositions were synthesized via laser engineered net shaping (LENS) by feeding different ratios of alloy powders into a melt pool created by a laser. Based on the assessment of the magnetic properties of the LENS printed samples, arc-melted and cast ingots were prepared with varying Fe (5-20 at.%) and Co (60-45 at.%) compositions while maintaining constant Ce (16 at.%) and Cu (19 at.%) content. The evolution of the microstructure and phases with varying chemical compositions and their dependence on magnetic properties are analyzed in as-cast and heat-treated samples. In both the LENS printed and cast samples, we find the best magnetic properties correspond to a predominantly single-phase Ce(CoFeCu)5 microstructure in which high coercivity (H c > 10 kOe) can be achieved without any microstructural refinement.

19 CFR 151.24 - Unlading facilities for bulk sugar.

Code of Federal Regulations, 2010 CFR

2010-04-01

... 19 Customs Duties 2 2010-04-01 2010-04-01 false Unlading facilities for bulk sugar. 151.24 Section... OF THE TREASURY (CONTINUED) EXAMINATION, SAMPLING, AND TESTING OF MERCHANDISE Sugars, Sirups, and Molasses § 151.24 Unlading facilities for bulk sugar. When dutiable sugar is to be imported in bulk, a full...

19 CFR 151.24 - Unlading facilities for bulk sugar.

Code of Federal Regulations, 2011 CFR

2011-04-01

... 19 Customs Duties 2 2011-04-01 2011-04-01 false Unlading facilities for bulk sugar. 151.24 Section... OF THE TREASURY (CONTINUED) EXAMINATION, SAMPLING, AND TESTING OF MERCHANDISE Sugars, Sirups, and Molasses § 151.24 Unlading facilities for bulk sugar. When dutiable sugar is to be imported in bulk, a full...

19 CFR 151.24 - Unlading facilities for bulk sugar.

Code of Federal Regulations, 2014 CFR

2014-04-01

... 19 Customs Duties 2 2014-04-01 2014-04-01 false Unlading facilities for bulk sugar. 151.24 Section... OF THE TREASURY (CONTINUED) EXAMINATION, SAMPLING, AND TESTING OF MERCHANDISE Sugars, Sirups, and Molasses § 151.24 Unlading facilities for bulk sugar. When dutiable sugar is to be imported in bulk, a full...

19 CFR 151.24 - Unlading facilities for bulk sugar.

Code of Federal Regulations, 2012 CFR

2012-04-01

... 19 Customs Duties 2 2012-04-01 2012-04-01 false Unlading facilities for bulk sugar. 151.24 Section... OF THE TREASURY (CONTINUED) EXAMINATION, SAMPLING, AND TESTING OF MERCHANDISE Sugars, Sirups, and Molasses § 151.24 Unlading facilities for bulk sugar. When dutiable sugar is to be imported in bulk, a full...

19 CFR 151.24 - Unlading facilities for bulk sugar.

Code of Federal Regulations, 2013 CFR

2013-04-01

... 19 Customs Duties 2 2013-04-01 2013-04-01 false Unlading facilities for bulk sugar. 151.24 Section... OF THE TREASURY (CONTINUED) EXAMINATION, SAMPLING, AND TESTING OF MERCHANDISE Sugars, Sirups, and Molasses § 151.24 Unlading facilities for bulk sugar. When dutiable sugar is to be imported in bulk, a full...

Colossal magnetocapacitive effect in differently synthesized and doped CdCr 2S 4

NASA Astrophysics Data System (ADS)

Krohns, S.; Schrettle, F.; Lunkenheimer, P.; Tsurkan, V.; Loidl, A.

2008-12-01

In the present work, we address the question of an impurity-related origin of the colossal magnetocapacitive effect in the spinel system CdCr 2S 4. We demonstrate that a strong variation in the dielectric constant below the magnetic transition temperature or in external magnetic fields also arises in crystals prepared without chlorine. This excludes that an inhomogeneous distribution of chlorine impurities at the surface or in the bulk material gives rise to the unusual effects in the spinel multiferroics. In addition, we show that the colossal magnetocapacitive effects can also be generated in chlorine-free ceramic samples of CdCr 2S 4, doped with indium.

Thermoelectric Properties of Hot-Pressed and PECS-Sintered Magnesium-Doped Copper Aluminum Oxide

NASA Astrophysics Data System (ADS)

Liu, Chang; Morelli, Donald T.

2011-05-01

Copper aluminum oxide (CuAlO2) is considered as a potential candidate for thermoelectric applications. Partially magnesium-doped CuAlO2 bulk pellets were fabricated using solid-state reactions, hot-pressing, and pulsed electric current sintering (PECS) techniques. X-ray diffraction and scanning electron microscopy were adopted for structural analysis. High-temperature transport property measurements were performed on hot-pressed samples. Electrical conductivity increased with Mg doping before secondary phases became significant, while the Seebeck coefficient displayed the opposite trend. Thermal conductivity was consistently reduced as the Mg concentration increased. Effects of Mg doping, preparation conditions, and future modification on this material's properties are discussed.

Should bulk cloudwater or fogwater samples obey Henry's law?

NASA Astrophysics Data System (ADS)

Pandis, Spyros N.; Seinfeld, John H.

1991-06-01

Mixing of droplets with different pH that are individually in Henry's law equilibrium with the surrounding atmosphere always results in a bulk mixture that is supersaturated with weak acids like S(IV) and HCOOH, and bases like NH3 with respect to the original atmosphere. High supersaturations result only when the pH of the bulk droplet mixture exceeds the pKa of the species, in which pH range large pH differences among droplets of different sizes lead to large deviations from Henry's law for the bulk mixture. The deviation is shown to depend on the ratio of the arithmetic mean to the harmonic mean of the hydrogen ion concentrations of the droplets with the liquid water content used as weighting factor in the calculation of the means. The theory developed can explain observed discrepancies from Henry's law in atmospheric samples and also other observed phenomena like the reported increase of pH values of bulk aqueous samples during storage.

Measurement of host-to-activator transfer efficiency in nano-crystalline Y{sub 2}O{sub 3}:Eu{sup 3+} under VUV excitation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Waite, Christopher; Mann, Rusty; Diaz, Anthony L., E-mail: DiazA@cwu.edu

2013-02-15

We have conducted a systematic study of the excitation and reflectance spectra of nano-crystalline Y{sub 2}O{sub 3}:Eu prepared by combustion synthesis. Excitation through the host lattice becomes relatively more efficient as the firing temperature of the precursor is increased, while reflectance properties remain essentially unchanged. Using these data, host-to-activator transfer efficiencies were calculated for excitation at the band edge of Y{sub 2}O{sub 3}, and evaluated using a competition kinetics model. From this analysis we conclude that the relatively low luminous efficiency of these materials is due more to poor bulk crystallinity than to surface loss effects. - Graphical abstract: Themore » low luminous efficiency of nano-crystalline Y{sub 2}O{sub 3}:Eu{sup 3+} prepared by combustion synthesis is due to poor bulk crystallinity rather than surface loss effects. Highlights: Black-Right-Pointing-Pointer We report on the optical properties of Y{sub 2}O{sub 3}:Eu{sup 3+} prepared by combustion synthesis. Black-Right-Pointing-Pointer Host-to-activator transfer efficiencies under VUV excitation were calculated. Black-Right-Pointing-Pointer The low luminous efficiency of these materials is due to poor bulk crystallinity.« less

Direct Comparison of Surface and Bulk Relaxation of PS - A Temperature Dependent Study

NASA Astrophysics Data System (ADS)

Wu, Wen-Li; Sambasivan, Sharadha; Wang, Chia-Ying; Genzer, Jan; Fischer, Daniel A.

2005-03-01

Near-edge X-ray absorption fine structure (NEXAFS) spectroscopy was used to measure simultaneously the relaxation rates of polystyrene (PS) molecules at the free surface and in the bulk. The samples were uniaxially oriented at room temperature via a modified cold rolling process. The density of the oriented samples as determined by liquid immersion technique is identical to that of bulk PS. At temperatures below its bulk glass transition temperature the rate of surface and bulk chain relaxation was monitored by measuring the partial-electron yield (PEY) and the fluorescence NEXAFS yields (FS), respectively, both parallel and perpendicular to the stretching direction. The decay rate of the dichroic ratios from both PEY and FY at various temperatures was taken as a measure of the relaxation rate of surface and bulk molecules respectively. In addition, the decay rate of the optical birefringence was also measured to provide an independent measure of the bulk relaxation. Relaxation of PS chains was found to occur faster on the surface relative to the bulk. The magnitude of the surface glass transition temperature suppression over the bulk was estimated to be 18 C based on the measured temperature dependence of the relaxation rates.

9 CFR 113.111 - Clostridium Perfringens Type C Toxoid and Bacterin-Toxoid.

Code of Federal Regulations, 2013 CFR

2013-01-01

... a prescribed test shall not be released. (a) Purity test. Final container samples of completed... § 113.26. (b) Safety test. Bulk or final container samples of completed product from each serial shall be tested for safety as provided in § 113.33(b). (c) Potency test. Bulk or final container samples of...

9 CFR 113.111 - Clostridium Perfringens Type C Toxoid and Bacterin-Toxoid.

Code of Federal Regulations, 2014 CFR

2014-01-01

... a prescribed test shall not be released. (a) Purity test. Final container samples of completed... § 113.26. (b) Safety test. Bulk or final container samples of completed product from each serial shall be tested for safety as provided in § 113.33(b). (c) Potency test. Bulk or final container samples of...

9 CFR 113.111 - Clostridium Perfringens Type C Toxoid and Bacterin-Toxoid.

Code of Federal Regulations, 2012 CFR

2012-01-01

... a prescribed test shall not be released. (a) Purity test. Final container samples of completed... § 113.26. (b) Safety test. Bulk or final container samples of completed product from each serial shall be tested for safety as provided in § 113.33(b). (c) Potency test. Bulk or final container samples of...

Synthesis and spectroscopic study of CdS nanoparticles using hydrothermal method

NASA Astrophysics Data System (ADS)

AL-Mamoori, Mohammed H. K.; Mahdi, Dunia K.; Al-Shrefi, Saif M.

2018-05-01

In this work, cadmium sulfide nanoparticles (powder) with diameter 50.8 nm was prepared using hydrothermal method. The structural and optical properties of CdS nanoparticles was studied by X-ray diffraction, FESEM, EDS, FTIR, UV-Diffuse Reflectance spectroscopy and Photoluminance spectrum. X-ray diffraction reveal the formation the purity of prepared phase of CdS particles with hexagonal wurtzite structure with particle size 31.8nm by using sheerer equation. The energy dispersion scattering (EDS) examination explains that the sample is composed of a large amount of Cd and S which are exactly CdS nanoparticles and there is a very small trace of (Zn) and (O) element observed because of there is a small pollutions in the measurement place of samples. FESEM shows the spherical shape of nanoparticles with around 50.8 nm diameter. The optical absorption spectral study identified the red shift of the sample in comparison to bulk ZnO in three dimensions. Photoluminance spectrum (PL) at room temperature showed that there are two luminescence peaks at 433.14 nm and 518.21nm. Samples demonstrate a sharp emission band at around 433.18 nm, which is attributed to the typical exciton luminescence. The broad band at 518.21nm which were attributed to the trapped luminescence. The green emission band at 518.21 nm was associated with the emission due to electronic transition from the conduction band to an accepter level due to interstitial sulphur ion.

Microfluidic Preparation of Polymer-Nucleic Acid Nanocomplexes Improves Nonviral Gene Transfer

NASA Astrophysics Data System (ADS)

Grigsby, Christopher L.; Ho, Yi-Ping; Lin, Chao; Engbersen, Johan F. J.; Leong, Kam W.

2013-11-01

As the designs of polymer systems used to deliver nucleic acids continue to evolve, it is becoming increasingly apparent that the basic bulk manufacturing techniques of the past will be insufficient to produce polymer-nucleic acid nanocomplexes that possess the uniformity, stability, and potency required for their successful clinical translation and widespread commercialization. Traditional bulk-prepared products are often physicochemically heterogeneous and may vary significantly from one batch to the next. Here we show that preparation of bioreducible nanocomplexes with an emulsion-based droplet microfluidic system produces significantly improved nanoparticles that are up to fifty percent smaller, more uniform, and are less prone to aggregation. The intracellular integrity of nanocomplexes prepared with this microfluidic method is significantly prolonged, as detected using a high-throughput flow cytometric quantum dot Förster resonance energy transfer nanosensor system. These physical attributes conspire to consistently enhance the delivery of both plasmid DNA and messenger RNA payloads in stem cells, primary cells, and human cell lines. Innovation in processing is necessary to move the field toward the broader clinical implementation of safe and effective nonviral nucleic acid therapeutics, and preparation with droplet microfluidics represents a step forward in addressing the critical barrier of robust and reproducible nanocomplex production.

Implanted Deuterium Retention and Release in Carbon-Coated Beryllium

NASA Astrophysics Data System (ADS)

Anderl, R. A.; Longhurst, G. R.; Pawelko, R. J.; Oates, M. A.

1997-06-01

Deuterium implantation experiments have been conducted on samples of clean and carbon-coated beryllium. These studies entailed preparation and characterization of beryllium samples coated with carbon thicknesses of 100, 500, and 1000 Å. Heat treatment of a beryllium sample coated with carbon to a thickness of approximately 100 Å revealed that exposure to a temperature of 400°C under high vacuum conditions was sufficient to cause substantial diffusion of beryllium through the carbon layer, resulting in more beryllium than carbon at the surface. Comparable concentrations of carbon and beryllium were observed in the bulk of the coating layer. Higher than expected oxygen levels were observed throughout the coating layer as well. Samples were exposed to deuterium implantation followed by thermal desorption without exposure to air. Differences were observed in deuterium retention and postimplantation release behavior in the carbon-coated samples as compared with bare samples. For comparable implantation conditions (sample temperature of 400°C and an incident deuterium flux of approximately 6 × 1019 D/m2-s), the quantity of deuterium retained in the bare sample was less than that retained in the carbon-coated samples. Further, the release of the deuterium took place at lower temperatures for the bare beryllium surfaces than for carbon-coated beryllium samples.

Herd-level prevalence of Map infection in dairy herds of southern Chile determined by culture of environmental fecal samples and bulk-tank milk qPCR.

PubMed

Kruze, J; Monti, G; Schulze, F; Mella, A; Leiva, S

2013-09-01

Paratuberculosis, an infectious disease of domestic and wild ruminants caused by Mycobacterium avium subsp. paratuberculosis (Map), is an economically important disease in dairy herds worldwide. In Chile the disease has been reported in domestic and wildlife animals. However, accurate and updated estimations of the herd-prevalence in cattle at national or regional level are not available. The objectives of this study were to determine the herd-level prevalence of dairy herds with Map infected animals of Southern Chile, based on two diagnostic tests: culture of environmental fecal samples and bulk-tank milk qPCR. Two composite environmental fecal samples and one bulk-tank milk sample were collected during September 2010 and September 2011 from 150 dairy farms in Southern Chile. Isolation of Map from environmental fecal samples was done by culture of decontaminated samples on a commercial Herrold's Egg Yolk Medium (HEYM) with and without mycobactin J. Suspicious colonies were confirmed to be Map by conventional IS900 PCR. Map detection in bulk-tank milk samples was done by real time IS900 PCR assay. PCR-confirmed Map was isolated from 58 (19.3%) of 300 environmental fecal samples. Holding pens and manure storage lagoons were the two more frequent sites found positive for Map, representing 35% and 33% of total positive samples, respectively. However, parlor exits and cow alleyways were the two sites with the highest proportion of positive samples (40% and 32%, respectively). Herd prevalence based on environmental fecal culture was 27% (true prevalence 44%) compared to 49% (true prevalence 87%) based on bulk-tank milk real time IS900 PC. In both cases herd prevalence was higher in large herds (>200 cows). These results confirm that Map infection is wide spread in dairy herds in Southern Chile with a rough herd-level prevalence of 28-100% depending on the herd size, and that IS900 PCR on bulk-tank milk samples is more sensitive than environmental fecal culture to detect Map-infected dairy herds. Copyright © 2013 Elsevier B.V. All rights reserved.

Fused Bead Analysis of Diogenite Meteorites

NASA Technical Reports Server (NTRS)

Mittlefehldt, D.W.; Beck, B.W.; McSween, H.Y.; Lee, C.T. A.

2009-01-01

Bulk rock chemistry is an essential dataset in meteoritics and planetary science [1]. A common method used to obtain the bulk chemistry of meteorites is ICP-MS. While the accuracy, precision and low detection limits of this process are advantageous [2], the sample size used for analysis (approx.70 mg) can be a problem in a field where small and finite samples are the norm. Fused bead analysis is another bulk rock analytical technique that has been used in meteoritics [3]. This technique involves forming a glass bead from 10 mg of sample and measuring its chemistry using a defocused beam on a microprobe. Though the ICP-MS has lower detection limits than the microprobe, the fused bead method destroys a much smaller sample of the meteorite. Fused bead analysis was initially designed for samples with near-eutectic compositions and low viscosities. Melts generated of this type homogenize at relatively low temperatures and produce primary melts near the sample s bulk composition [3]. The application of fused bead analysis to samples with noneutectic melt compositions has not been validated. The purpose of this study is to test if fused bead analysis can accurately determine the bulk rock chemistry of non-eutectic melt composition meteorites. To determine this, we conduct two examinations of the fused bead. First, we compare ICP-MS and fused bead results of the same samples using statistical analysis. Secondly, we inspect the beads for the presence of crystals and chemical heterogeneity. The presence of either of these would indicate incomplete melting and quenching of the bead.

DEVELOPMENT OF A TAMPER RESISTANT/INDICATING AEROSOL COLLECTION SYSTEM FOR ENVIRONMENTAL SAMPLING AT BULK HANDLING FACILITIES

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sexton, L.

2012-06-06

Environmental sampling has become a key component of International Atomic Energy Agency (IAEA) safeguards approaches since its approval for use in 1996. Environmental sampling supports the IAEA's mission of drawing conclusions concerning the absence of undeclared nuclear material or nuclear activities in a Nation State. Swipe sampling is the most commonly used method for the collection of environmental samples from bulk handling facilities. However, augmenting swipe samples with an air monitoring system, which could continuously draw samples from the environment of bulk handling facilities, could improve the possibility of the detection of undeclared activities. Continuous sampling offers the opportunity tomore » collect airborne materials before they settle onto surfaces which can be decontaminated, taken into existing duct work, filtered by plant ventilation, or escape via alternate pathways (i.e. drains, doors). Researchers at the Savannah River National Laboratory and Oak Ridge National Laboratory have been working to further develop an aerosol collection technology that could be installed at IAEA safeguarded bulk handling facilities. The addition of this technology may reduce the number of IAEA inspector visits required to effectively collect samples. The principal sample collection device is a patented Aerosol Contaminant Extractor (ACE) which utilizes electrostatic precipitation principles to deposit particulates onto selected substrates. Recent work has focused on comparing traditional swipe sampling to samples collected via an ACE system, and incorporating tamper resistant and tamper indicating (TRI) technologies into the ACE system. Development of a TRI-ACE system would allow collection of samples at uranium/plutonium bulk handling facilities in a manner that ensures sample integrity and could be an important addition to the international nuclear safeguards inspector's toolkit. This work was supported by the Next Generation Safeguards Initiative (NGSI), Office of Nonproliferation and International Security (NIS), National Nuclear Security Administration (NNSA).« less

Effect of Sintering Temperature to Physical, Magnetic Properties and Crystal Structure on Permanent Magnet BaFe12O19 Prepared From Mill Scale

NASA Astrophysics Data System (ADS)

Ramlan; Muljadi; Sardjono, Priyo; Gulo, Fakhili; Setiabudidaya, Dedi

2017-07-01

Permanent magnet of Barium hexa Ferrite with formula BaFe12O19 has been made by metallurgy powder method from raw materials : Barium carbonate (BaCO3 E-merck) and Iron Oxide (Fe2O3 from mill scale). Both of raw materials have been mixed with stoichiometry composition by using a ball mill for 24 hours. The fine powder obtained from milling process was formed by using a hydraulic press at pressure 50 MPa and continued with sintering process. The sintering temperature was varied : 1150°C, 1200°C, 1250°C and 1300°C with holding time for 1 hour. The sintered samples were characterized such as : physical properties (bulk density, porosity and shrinkage), magnetic properties (flux density, remanence, coercivity and magnetic saturation) by using VSM and crystal structure by using XRD. According characterization results show that the crystal structure of BaFe12O19 does not change after sintering process, but the grain size tends to increase. The optimum condition is achieved at temperature 1250°C, and at this condition, the sample has characterization such as : bulk density = 4.35 g/cm3, porosity = 1.03% and firing shrinkage = 11.63%, flux density = 681.1 Gauss, remanence (σr) = 20.78 emu/g, coercivity (Hc) = 2058 Oe and magnetic saturation (σs) 45.16 emu/g.

The effects of Nd2O3 concentration in the laser emission of TeO2-ZnO glasses

NASA Astrophysics Data System (ADS)

Moreira, L. M.; Anjos, V.; Bell, M. J. V.; Ramos, C. A. R.; Kassab, L. R. P.; Doualan, D. J. L.; Camy, P.; Moncorgé, R.

2016-08-01

The present work reports the modification introduced by different Nd2O3 concentration on optical properties and the laser operation of Nd3+ doped (TeO2-ZnO) bulk tellurite glass. The spectroscopic data are analyzed within the Judd Ofelt formalism framework and the results are compared to the fluorescence lifetime and emission measurements to derive values for the quantum efficiency and the stimulated emission cross section of the considered 4F3/2 → 4I11/2 infrared laser transition around 1062.5 nm. Continuous-wave laser action is achieved with this bulk tellurite glass by pumping the sample inside a standard plan-concave mirror laser cavity with different output couplers. It is possible to observe coherent emission only for the lower concentration (0.5%(wt.) of Nd2 O3). Also laser action could only be observed for this sample with threshold pump power of 73 mW associated with a laser slope efficiency of 8% for an output coupler transmission of 4% indicating that TeO2-ZnO are potential materials for laser action. The results presented in this work together with those previously reported with higher concentration (1.0% (wt) of Nd2O3) determine the adequate Nd2O3 concentration for laser action and guide the correct experimental procedure for TeO2-ZnO glasses preparation.

Non-equilibrium character of resistive switching and negative differential resistance in Ga-doped Cr2O3 system

NASA Astrophysics Data System (ADS)

Bhowmik, R. N.; Siva, K. Venkata

2018-07-01

The samples of Ga-doped Cr2O3 system in rhombohedral crystal structure with space group R 3 bar C were prepared by chemical co-precipitation route and annealing at 800 °C. The current-voltage (I-V) curves exhibited many unique non-linear properties, e.g., hysteresis loop, resistive switching, and negative differential resistance (NDR). In this work, we report non-equilibrium properties of resistive switching and NDR phenomena. The non-equilibrium I-V characteristics were confirmed by repetiting measurement and time relaxation of current. The charge conduction process was understood by analysing the I-V curves using electrode-limited and bulk-limited charge conduction mechanisms, which were proposed for metal electrode/metal oxide/metal electrode structure. The I-V curves in the NDR regime and at higher bias voltage regime in our samples did not obey Fowler-Nordheim equation, which was proposed for charge tunneling mechanism in many thin film junctions. The non-equilibrium I-V phenomena were explained by considering the competitions between the injection of charge carriers from metal electrode to metal oxide, the charge flow through bulk material mediated by trapping/de-trapping and recombination of charge carriers at the defect sites of ions, the space charge effects at the junctions of electrodes and metal oxides, and finally, the out flow of electrons from metal oxide to metal electrode.

Synthesis and characterization of biopolymer protected zinc sulphide nanoparticles

NASA Astrophysics Data System (ADS)

Senapati, U. S.; Sarkar, D.

2015-09-01

Zinc sulphide (ZnS) nanoparticles are prepared by a simple, economic and green synthesis route. X-ray diffraction patterns confirm zinc blend structure. ZnS formation is confirmed through chemical analysis by energy dispersive analysis of X-rays. Transmission electron microscopy reveals formation of nanosize with dimension in the range of 8-2 nm. Band gap of the nanocrystals is found to lie in the range of 4.51-4.65 eV. Photoluminescence study indicate defect like vacancies. The growth mechanism of ZnS nanoparticles is discussed with the help of Fourier transform infrared spectroscopy and thermogravimetric analysis. The materials show high dielectric constant compared to its bulk counterpart. The dielectric loss of the samples shows anomalous behaviour. The frequency dependent A.C. conductivity of the samples is discussed both in high and low frequency regimes. Current-voltage (I-V) characteristic performed under dark and under illumination, shows excellent light response of the material.

The equilibrium sedimentation of hyaluronic acid and of two synthetic polymers

PubMed Central

Nichol, L. W.; Ogston, A. G.; Preston, B. N.

1967-01-01

1. The method of equilibrium sedimentation has been investigated as an alternative to osmotic-pressure measurement for determining thermodynamic properties of polymer solutions at relatively high concentrations. 2. The simplifications that must be made in the theoretical treatment are discussed. 3. Measurements have been made on samples of polyethylene glycol, neutralized polymethacrylic acid and hyaluronic acid. With the first and third, values of the `non-ideality coefficients' have been obtained that agree with those obtained from osmotic measurements on the same materials. 4. Evidence has been obtained of the presence in hyaluronic acid preparations of a fraction that has either a lower degree of thermodynamic non-ideality or a higher density increment than the bulk of the sample. This fraction is not protein. ImagesFig. 3.Fig. 4.Fig. 5.Fig. 7.Fig. 8.Fig. 9.Fig. 11.Fig. 12.Fig. 13.Fig. 14. PMID:6029600

Susceptibility measurements on the superconducting properties of Nb-Ge alloys

NASA Technical Reports Server (NTRS)

Rathz, T. J.

1981-01-01

A susceptibility apparatus to measure superconducting properties of samples made in the MSFC Drop Tube was used to measure the transition temperature (Tc) and susceptibilities of Nb and Nb Ge Alloys prepared in bulk spherical (2-4 mm diameter) form using a 32 m drop tube in which containerless low gravity solidification could take place. Results indicate that a drop tube processing environment was beneficial for increasing the Tc of the superconducting phase of the material over that of arc melted material. The increase in Tc is found to be related to the amount of solidification of the total sample that took place before reaching the bottom of the drop tube. In phase and quadrature phase measurements of the specimen's susceptibility indicated that some improvement in homogeneity takes place in drop tube processing. These phase measurements also indicated little or no shielding of a lower Tc phase by a higher Tc filamentary structure.

Health hazard evaluation report HETA 83-248-1515, Arco Philadelphia refinery, Philadelphia, Pennsylvania

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lewis, F.A.; Parrish, G.

1984-10-01

A bulk sample of fractionator residue was analyzed for polynuclear aromatic (PNA) compounds at the catalytic cracking unit of ARCO Philadelphia Refinery (SIC-2911), Philadelphia, Pennsylvania in May, 1983. The study was requested by the Atlantic Independent Union to determine if skin rashes and skin irritation occurring among refinery workers were caused by PNA in the fractionators. The authors conclude that a health hazard from exposure to chemicals at the cracking unit may exist. No specific chemical agent can be identified. Dust from the catalyst and oily residues that could contaminate workers shoes and clothing may have contributed to some ofmore » the dermatitis cases. Recommendations include laundering workers coveralls by dry cleaning to insure the removal of oily residues, providing workers with oil resistant or oil proof work boots, and repairing the ventilator in the sample preparation room adjacent to the block house.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nandihalli, Nagaraj; Gorsse, Stéphane; Kleinke, Holger, E-mail: kleinke@uwaterloo.ca

To prepare Ni{sub 0.05}Mo{sub 3}Sb{sub 5.4}Te{sub 1.6}, the starting materials were loaded in the stoichiometric ratio into silica tubes and then heated at 1000 K. The reaction products were mixed and divided into four equal parts. The first sample was used as a reference sample called bulk. For the remaining samples, 1%, 2% and 3% by mass of MWCNT (multi-wall carbon nanotubes) were added by ball-milling. These materials were then subjected to consolidation by hot-pressing at 850 K and 56 MPa. Their transport properties were determined and compared to study the influence of MWCNT on the transport properties of Ni{submore » 0.05}Mo{sub 3}Sb{sub 5.4}Te{sub 1.6}. Scanning and transmission electron microscopy were used to study the microstructural and nanostructural features of the samples, and Raman characterization was performed to look for changes induced by ball-milling and hot-pressing of the nanotubes. Mainly due to a largely reduced thermal conductivity by 40% and a slightly reduced power factor, the figure-of-merit was improved by 25% after addition of 3 mass% of MWCNT. - Graphical abstract: Figure-of-merit of various Ni{sub 0.05}Mo{sub 3}Sb{sub 5.4}Te{sub 1.6}/CNT composites. - Highlights: • Various composites of Ni{sub 0.05}Mo{sub 3}Sb{sub 5.4}Te{sub 1.6} with carbon nanotubes were synthesized and characterized. • In each case, the thermoelectric figure-of-merit increases rapidly with increasing temperature. • With increasing amount of carbon nanotubes, the thermal conductivity decreases more than the electrical conductivity. • The composite with 3% carbon nanotubes performs better than the bulk material by 25%.« less

Somatic cell counts in bulk milk and their importance for milk processing

NASA Astrophysics Data System (ADS)

Savić, N. R.; Mikulec, D. P.; Radovanović, R. S.

2017-09-01

Bulk tank milk somatic cell counts are the indicator of the mammary gland health in the dairy herds and may be regarded as an indirect measure of milk quality. Elevated somatic cell counts are correlated with changes in milk composition The aim of this study was to assess the somatic cell counts that significantly affect the quality of milk and dairy products. We examined the somatic cell counts in bulk tank milk samples from 38 farms during the period of 6 months, from December to the May of the next year. The flow cytometry, Fossomatic was used for determination of somatic cell counts. In the same samples content of total proteins and lactose was determined by Milcoscan. Our results showed that average values for bulk tank milk samples were 273,605/ml from morning milking and 292,895/ml from evening milking. The average values for total proteins content from morning and evening milking are 3,31 and 3,34%, respectively. The average values for lactose content from morning and evening milking are 4,56 and 4,63%, respectively. The highest somatic cell count (516,000/ml) was detected in bulk tank milk sample from evening milk in the Winter and the lowest content of lactose was 4,46%. Our results showed that obtained values for bulk tank milk somatic cell counts did not significantly affected the content of total proteins and lactose.

Bulk-scaffolded hydrogen storage and releasing materials and methods for preparing and using same

DOEpatents

Autrey, S Thomas [West Richland, WA; Karkamkar, Abhijeet J [Richland, WA; Gutowska, Anna [Richland, WA; Li, Liyu [Richland, WA; Li, Xiaohong S [Richland, WA; Shin, Yongsoon [Richland, WA

2011-06-21

Compositions are disclosed for storing and releasing hydrogen and methods for preparing and using same. These hydrogen storage and releasing materials exhibit fast release rates at low release temperatures without unwanted side reactions, thus preserving desired levels of purity and enabling applications in combustion and fuel cell applications.

A magnetic resonance study of MoS(2) fullerene-like nanoparticles.

PubMed

Panich, A M; Shames, A I; Rosentsveig, R; Tenne, R

2009-09-30

We report on the first nuclear magnetic resonance (NMR) and electron paramagnetic resonance (EPR) investigation of inorganic fullerene-like MoS(2) nanoparticles. Spectra of bulk 2H-MoS(2) samples have also been measured for comparison. The similarity between the measured quadrupole coupling constants and chemical shielding anisotropy parameters for bulk and fullerene-like MoS(2) reflects the nearly identical local crystalline environments of the Mo atoms in these two materials. EPR measurements show that fullerene-like MoS(2) exhibits a larger density of dangling bonds carrying unpaired electrons, indicative of them having a more defective structure than the bulk sample. The latter observation explains the increase in the spin-lattice relaxation rate observed in the NMR measurements for this sample in comparison with the bulk 2H- MoS(2) ones.

A magnetic resonance study of MoS2 fullerene-like nanoparticles

NASA Astrophysics Data System (ADS)

Panich, A. M.; Shames, A. I.; Rosentsveig, R.; Tenne, R.

2009-09-01

We report on the first nuclear magnetic resonance (NMR) and electron paramagnetic resonance (EPR) investigation of inorganic fullerene-like MoS2 nanoparticles. Spectra of bulk 2H-MoS2 samples have also been measured for comparison. The similarity between the measured quadrupole coupling constants and chemical shielding anisotropy parameters for bulk and fullerene-like MoS2 reflects the nearly identical local crystalline environments of the Mo atoms in these two materials. EPR measurements show that fullerene-like MoS2 exhibits a larger density of dangling bonds carrying unpaired electrons, indicative of them having a more defective structure than the bulk sample. The latter observation explains the increase in the spin-lattice relaxation rate observed in the NMR measurements for this sample in comparison with the bulk 2H- MoS2 ones.

Influence of Osmotic Drying with an Aqueous Poly(ethylene Glycol) Liquid Desiccant on Alumina Objects Gelcast with Gelatin

DOE PAGES

Hammel, E. C.; Campa, J. A.; Armbrister, C. E.; ...

2017-09-06

Gelcasting and liquid desiccant drying are novel forming and drying methods used to mitigate common issues associated with the fabrication of complex advanced ceramic objects. Here, the molecular weight and osmotic pressure of aqueous poly(ethylene glycol) (PEG) desiccant solutions were simultaneously varied to understand their influence on the net mass loss rates of gelcast alumina samples prepared using gelatin as a gelling agent. Additionally, the amount of PEG diffusion and water diffusion to and from the ceramic samples after 150 min of immersion in the liquid desiccant was correlated to the solution properties as was the final bulk density ofmore » the sintered samples. Furthermore, solutions with high molecular weight and low osmotic pressure resulted in low PEG gain and low water loss, while solutions with low molecular weight and high osmotic pressure resulted in high PEG gain and high water loss. In some cases, more than 40 wt% of the total water per sample was removed through the liquid desiccant drying process.« less

Study of the Effect on Ionic Conductivity and Structral Morphology of the SR Doped Lanthanum Gallate Solid Electrolyte

NASA Astrophysics Data System (ADS)

Sood, Kapil; Singh, K.; Pandey, O. P.

2013-07-01

In the present study, lanthanum gallate and Sr-doped lanthanum gallate samples were prepared by conventional solid state reaction method. The phase conformation has been performed by using X-ray diffraction (XRD) study. The elemental composition has been confirmed using energy dispersive spectroscopy (EDS) analysis. Ac conductivity of the samples has been measured in the frequency range 0.1-106 Hz and from 50-800 °C. The impedance plots among real and complex impedances at particular temperature have been discussed. The behavior shows the effect of bulk and grain boundary effects of the doped sample. The impedance plots with frequency have been analyzed. The plots have been well fitted to equivalent circuit model. The conductivity shows the Arrhenius type of behavior. The activation energy has been calculated from the plots and represents that the conductivity through the material is mainly ionic. The structural morphology of the samples has been investigated using scanning electron microscope (SEM). The micrograph shows that the porosity and grain size both decreases with Sr-doping.

Comparison of quartz crystallographic preferred orientations identified with optical fabric analysis, electron backscatter and neutron diffraction techniques.

PubMed

Hunter, N J R; Wilson, C J L; Luzin, V

2017-02-01

Three techniques are used to measure crystallographic preferred orientations (CPO) in a naturally deformed quartz mylonite: transmitted light cross-polarized microscopy using an automated fabric analyser, electron backscatter diffraction (EBSD) and neutron diffraction. Pole figure densities attributable to crystal-plastic deformation are variably recognizable across the techniques, particularly between fabric analyser and diffraction instruments. Although fabric analyser techniques offer rapid acquisition with minimal sample preparation, difficulties may exist when gathering orientation data parallel with the incident beam. Overall, we have found that EBSD and fabric analyser techniques are best suited for studying CPO distributions at the grain scale, where individual orientations can be linked to their source grain or nearest neighbours. Neutron diffraction serves as the best qualitative and quantitative means of estimating the bulk CPO, due to its three-dimensional data acquisition, greater sample area coverage, and larger sample size. However, a number of sampling methods can be applied to FA and EBSD data to make similar approximations. © 2016 The Authors Journal of Microscopy © 2016 Royal Microscopical Society.

Influence of Osmotic Drying with an Aqueous Poly(ethylene Glycol) Liquid Desiccant on Alumina Objects Gelcast with Gelatin

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hammel, E. C.; Campa, J. A.; Armbrister, C. E.

Gelcasting and liquid desiccant drying are novel forming and drying methods used to mitigate common issues associated with the fabrication of complex advanced ceramic objects. Here, the molecular weight and osmotic pressure of aqueous poly(ethylene glycol) (PEG) desiccant solutions were simultaneously varied to understand their influence on the net mass loss rates of gelcast alumina samples prepared using gelatin as a gelling agent. Additionally, the amount of PEG diffusion and water diffusion to and from the ceramic samples after 150 min of immersion in the liquid desiccant was correlated to the solution properties as was the final bulk density ofmore » the sintered samples. Furthermore, solutions with high molecular weight and low osmotic pressure resulted in low PEG gain and low water loss, while solutions with low molecular weight and high osmotic pressure resulted in high PEG gain and high water loss. In some cases, more than 40 wt% of the total water per sample was removed through the liquid desiccant drying process.« less

The Fabrication of (bismuth, LEAD)(2) STRONTIUM(2) CALCIUM(2) COPPER(3) Oxygen(x) Superconductor in Bulk and Tape Forms

NASA Astrophysics Data System (ADS)

Lim, Hanjin

High-T_{rm c}<=ad doped rm Bi_2Sr_2Ca_2Cu _2Cu_3O_{x} (BSCCO 2223) superconductor bulk materials were prepared using conventional powder metallurgy techniques, which were made from precursors having different histories. The ease of formation of superconducting phases was highly dependent on the processing of primitive powder. With the three -powder process that combines three kinds of calcined precursor powders, the formation of the BSCCO superconductor was accelerated and the amount of the secondary phase (e.g., Ca_2CuO_3) was reduced. The critical transition temperature (T _{rm c}) of the superconductor from the three-powder process is higher than that from the one-powder process. In lead-doped BSCCO 2223, positron trapping and annihilation evidently occur in the open BiO double layers rather than in the superconducting CuO_2 layers of the structure. Both positron annihilation parameters (tau_1, tau _2, overlinetau) and Doppler parameters (P, W, P/W) were insensitive to the superconducting transition in this material. This is quite opposite to the case of YBCO and Dy doped YBCO where positron annihilation is sensitive to the superconducting transition. High-T_{rm c} BSCCO superconducting tapes were fabricated using the powder -in-tube (PIT) method that includes heat treatments as well as mechanical processing such as drawing, rolling, and pressing. The highest critical current densities (J _{rm c}) at 5 and 77 K were 5.12 times 10^5 A/cm^2 and 1.77 times 10^4 A/cm^2 , respectively, for the tape sample which was solid state processed at 840^circC with three short sintering steps. J_{ rm c} values at 5 and 77 K of tape samples were 1 and 2 orders of magnitude higher than those of bulk samples, respectively. The preferred orientations of the BSCCO 2212 phase in the tape samples were basal and (1 1 13) textures; for the BSCCO 2223 phase preferred orientations were also basal and (1 1 19) textures. By taking the ratios of the texture coefficients (TCs) for (0 0 1) and (1 1 0) reflections, one can describe the strength of the basal texture for each superconducting phase in both bulk and tape. From these ratios one can say that the best basal texture for the tape BSCCO 2212 was produced by the procedure which included partial melting at 850^circ C for 0.3 h. The best treatment for BSCCO 2223 was the tape sample with solid state processing at 840 ^circC in 10% oxygen.

Depletion region surface effects in electron beam induced current measurements.

PubMed

Haney, Paul M; Yoon, Heayoung P; Gaury, Benoit; Zhitenev, Nikolai B

2016-09-07

Electron beam induced current (EBIC) is a powerful characterization technique which offers the high spatial resolution needed to study polycrystalline solar cells. Current models of EBIC assume that excitations in the p - n junction depletion region result in perfect charge collection efficiency. However we find that in CdTe and Si samples prepared by focused ion beam (FIB) milling, there is a reduced and nonuniform EBIC lineshape for excitations in the depletion region. Motivated by this, we present a model of the EBIC response for excitations in the depletion region which includes the effects of surface recombination from both charge-neutral and charged surfaces. For neutral surfaces we present a simple analytical formula which describes the numerical data well, while the charged surface response depends qualitatively on the location of the surface Fermi level relative to the bulk Fermi level. We find the experimental data on FIB-prepared Si solar cells is most consistent with a charged surface, and discuss the implications for EBIC experiments on polycrystalline materials.

Determining and analyzing the strength and impact resistance of high modulus glass

NASA Technical Reports Server (NTRS)

Bacon, J. F.

1972-01-01

A number of new glass compositions have been prepared with increased emphasis on compositions without beryllia. Glass preparations have been much more broadly based and have included the eutectic glass fields, and the mullite-rare earth glass systems. Of the new glasses, the best non-toxic composition is UARL 472 with a bulk modulus of only 18.20 million psi. A second experimental glass, UARL 417, was chosen for research in making large quantities of fiber in monofilament form. Tests of these UARL 417 epoxy resin samples in comparison to similar composites made with the DuPont organic fiber, PRD-49-1, show that the UARL composites have a compressive strength 41/2 times higher and a specific compressive strength at least 21/2 times greater. Much of the research effort attempted to answer the question of why a given glass should have an impact strength superior to other glasses. No definitive answer to the question was found.

Preparation of 110K (Bi, Pb)-Sr-Ca-Cu-O superconductor from glass precursor

NASA Technical Reports Server (NTRS)

Bansal, Narottam P.

1989-01-01

The Bi1.5Pb0.5Sr2Ca2Cu3O(x) glass, prepared by rapid quenching of the melt, showed T(sub g) of 383 C, crystallization temperature of approx. 446 C, melting temperature of approx. 855 C, and bulk density of 5.69 g/cu. cm. in air. The as-quenched glass was oxygen deficient. On heating in O2, it showed a slow, irreversible, and continuous weight gain starting at approx. 530 C. The influence of annealing conditions on the formation of various phases was investigated by XRD and electrical resistivity measurements. The 110K-T(sub c) phase did not form below 840 C. The amount of this phase increased with the sintering time at 840 C. A sample annealed at 840 C for 243 h in air and furnace cooled showed the highest T(sub c)(R=0) of 107.2K and transition width delta T(sub c)(10 to 90 percent) of approx. 2 K.

Preparation of 110K (Bi, Pb)-Sr-Ca-Cu-O superconductor from glass precursor

NASA Technical Reports Server (NTRS)

Bansal, Narottam P.

1990-01-01

The Bi1.5Pb0.5Sr2Ca2Cu3O(x) glass, prepared by rapid quenching of the melt, showed T(sub g) of 383 C, crystallization temperature of approx. 446 C, melting temperature of approx. 855 C, and bulk density of 5.69 g/cu. cm. in air. The as-quenched glass was oxygen deficient. On heating in O2, it showed a slow, irreversible, and continuous weight gain starting at approx. 530 C. The influence of annealing conditions on the formation of various phases was investigated by XRD and electrical resistivity measurements. The 110K-T(sub c) phase did not form below 840 C. The amount of this phase increased with the sintering time at 840 C. A sample annealed at 840 C for 243 h in air and furnace cooled showed the highest T(sub c) (R=0) of 107.2 K and transition width delta T(sub c) (10 to 90 percent) of approx. 2 K.

A Single Molecular Diels-Alder Crosslinker for Achieving Recyclable Cross-Linked Polymers.

PubMed

Chen, Shengli; Wang, Fenfen; Peng, Yongjin; Chen, Tiehong; Wu, Qiang; Sun, Pingchuan

2015-09-01

A triol-functional crosslinker combining the thermoreversible properties of Diels-Alder (DA) adducts in one molecule is designed, synthesized, and used as an ideal substitute of a traditional crosslinker to prepare thermal recyclable cross-linked polyurethanes with excellent mechanical properties and recyclability in a very simple and efficient way. The recycle property of these materials achieved by the DA/retro-DA reaction at a suitable temperature is verified by differential scanning calorimetry and in situ variable temperature solid-state NMR experiments during the cyclic heating and cooling processes. The thermal recyclability and remending ability of the bulk polyurethanes is demonstrated by three polymer processing methods, including hot-press molding, injection molding, and solution casting. It is notable that all the recycled cross-linked polymers display nearly invariable elongation/stress at break compared to the as-synthesized samples. Further end-group functionalization of this single molecular DA crosslinker provides the potential in preparing a wide range of recyclable cross-linked polymers. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

On the approach to Mott's transition in glass-ceramic nanocomposite due to heat treatment

NASA Astrophysics Data System (ADS)

Mahdy, Iman A.; Heikal, Sh.; Abd-Rabo, A. S.; Abdel Ghany, A.; Bahgat, A. A.

2015-07-01

In the present work, the glass-ceramic nanocomposite (GCNC) of the composition 30[0.75 BaTiO3+0.25 PbTiO3]+70 V2O5 (mol. %) was prepared from the parent glass by isothermal heat treatment (HT) at 723 K for different time intervals 0.25, 0.5, 1.5, 2, and 2.5 h, respectively. The bulk density and some related parameters were calculated. X-ray diffraction and Hi-Resolution Transmission Electron Microscope (HRTEM) were used to identify different phases as well as particle size of the precipitated nanocrystals during the heat treatment process. The DC electrical conductivity was enhanced three orders of magnitudes (3×103) by increasing HT time. The resistivity measurements on the other hand as a function of time show an approach to nonmetallic-metallic transition for the prepared NCGC samples. Mott's VRH conduction mechanism was predicted as a result of the increase of the heat treatment time.

Microstructural Study of Micron-Sized Craters Simulating Stardust Impacts in Aluminum 1100 Targets

NASA Technical Reports Server (NTRS)

Leroux, Hugues; Borg, Janet; Troadec, David; Djouadi, Zahia; Horz, Friedrich

2006-01-01

Various microscopic techniques were used to characterize experimental micro- craters in aluminium foils to prepare for the comprehensive analysis of the cometary and interstellar particle impacts in aluminium foils to be returned by the Stardust mission. First, SEM (Scanning Electron Microscopy) and EDS (Energy Dispersive X-ray Spectroscopy) were used to study the morphology of the impact craters and the bulk composition of the residues left by soda-lime glass impactors. A more detailed structural and compositional study of impactor remnants was then performed using TEM (Transmission Electron Microscopy), EDS, and electron diffraction methods. The TEM samples were prepared by Focused Ion Beam (FIB) methods. This technique proved to be especially valuable in studying impact crater residues and impact crater morphology. Finally, we also showed that InfraRed microscopy (IR) can be a quick and reliable tool for such investigations. The combination of all of these tools enables a complete microscopic characterization of the craters.

First tests of Timepix detectors based on semi-insulating GaAs matrix of different pixel size

NASA Astrophysics Data System (ADS)

Zaťko, B.; Kubanda, D.; Žemlička, J.; Šagátová, A.; Zápražný, Z.; Boháček, P.; Nečas, V.; Mora, Y.; Pichotka, M.; Dudák, J.

2018-02-01

In this work, we have focused on Timepix detectors coupled with the semi-insulating GaAs material sensor. We used undoped bulk GaAs material with the thickness of 350 μm. We prepared and tested four pixelated detectors with 165 μm and 220 μm pixel size with two versions of technology preparation, without and with wet chemically etched trenches around each pixel. We have carried out adjustment of GaAs Timepix detectors to optimize their performance. The energy calibration of one GaAs Timepix detector in Time-over-threshold mode was performed with the use of 241Am and 133Ba radioisotopes. We were able to detect γ-photons with the energy up to 160 keV. The X-ray imaging quality of GaAs Timepix detector was tested with X-ray source using various samples. After flat field we obtained very promising imaging performance of tested GaAs Timepix detectors.

MIPs and Aptamers for Recognition of Proteins in Biomimetic Sensing.

PubMed

Menger, Marcus; Yarman, Aysu; Erdőssy, Júlia; Yildiz, Huseyin Bekir; Gyurcsányi, Róbert E; Scheller, Frieder W

2016-07-18

Biomimetic binders and catalysts have been generated in order to substitute the biological pendants in separation techniques and bioanalysis. The two major approaches use either "evolution in the test tube" of nucleotides for the preparation of aptamers or total chemical synthesis for molecularly imprinted polymers (MIPs). The reproducible production of aptamers is a clear advantage, whilst the preparation of MIPs typically leads to a population of polymers with different binding sites. The realization of binding sites in the total bulk of the MIPs results in a higher binding capacity, however, on the expense of the accessibility and exchange rate. Furthermore, the readout of the bound analyte is easier for aptamers since the integration of signal generating labels is well established. On the other hand, the overall negative charge of the nucleotides makes aptamers prone to non-specific adsorption of positively charged constituents of the sample and the "biological" degradation of non-modified aptamers and ionic strength-dependent changes of conformation may be challenging in some application.

Microfluidic Remote Loading for Rapid Single-Step Liposomal Drug Preparation

PubMed Central

Hood, R.R.; Vreeland, W. N.; DeVoe, D.L.

2014-01-01

Microfluidic-directed formation of liposomes is combined with in-line sample purification and remote drug loading for single step, continuous-flow synthesis of nanoscale vesicles containing high concentrations of stably loaded drug compounds. Using an on-chip microdialysis element, the system enables rapid formation of large transmembrane pH and ion gradients, followed by immediate introduction of amphipathic drug for real-time remote loading into the liposomes. The microfluidic process enables in-line formation of drug-laden liposomes with drug:lipid molar ratios of up to 1.3, and a total on-chip residence time of approximately 3 min, representing a significant improvement over conventional bulk-scale methods which require hours to days for combined liposome synthesis and remote drug loading. The microfluidic platform may be further optimized to support real-time generation of purified liposomal drug formulations with high concentrations of drugs and minimal reagent waste for effective liposomal drug preparation at or near the point of care. PMID:25003823

Non-destructive automated sampling of mycotoxins in bulk food and feed - A new tool for required harmonization.

PubMed

Spanjer, M; Stroka, J; Patel, S; Buechler, S; Pittet, A; Barel, S

2001-06-01

Mycotoxins contamination is highly non-uniformly distributed as is well recog-nized by the EC, by not only setting legal limits in a series of commodities, but also schedule a sampling plan that takes this heterogeneity into account. In practice however, it turns out that it is very difficult to carry out this sampling plan in a harmonised way. Applying the sampling plan to a container filled with pallets of bags (i.e. with nuts or coffee beans) varies from very laborious to almost impossible. The presented non-destructive automated method to sample bulk food could help to overcome these practical problems and to enforcing of EC directives. It is derived from a tested and approved technology for detection of illicit substances in security applications. It has capability to collect and iden-tify ultra trace contaminants, i.e. from a fingerprint of chemical substance in a bulk of goods, a cargo pallet load (~ 1000 kg) with boxes and commodities.The technology, patented for explosives detection, uses physical and chemistry processes for excitation and remote rapid enhanced release of contaminant residues, vapours and particulate, of the inner/outer surfaces of inspected bulk and collect them on selective probes. The process is automated, takes only 10 minutes, is non-destructive and the bulk itself remains unharmed. The system design is based on applicable international regulations for shipped cargo hand-ling and transportation by road, sea and air. After this process the pallet can be loaded on a truck, ship or plane. Analysis can be carried out before the cargo leaves the place of shipping. The potent application of this technology for myco-toxins detection, has been demonstrated by preliminary feasibility experiments. Aflatoxins were detected in pistachios and ochratoxin A in green coffee beans bulk. Both commodities were naturally contaminated, priory found and confirm-ed by common methods as used at routine inspections. Once the contaminants are extracted from a bulk shipment, an appropriate existing analytical method, i.e. a CEN method, can be used to measure the mycotoxins.The system, routinely in use for explosives detection, was able to screen bulk food and feed for mycotoxins, through non-destructive automated sampling of a whole batch/lot/sublot of commodities. The opportunity to sample a whole bulk would provide more effective tools for inspection at seaports, production facili-ties and distri-bution points. It will advance the current process of myco-toxins check because: (i) Checks will be automated and harmonized, (ii) Checks will be non-destructive, (iii) Checks will be faster and allow a greater amount of bulk commodities to be inspected and (iv) The ability to check, with automated equipment, larger portions of lots of a shipment will increase the probability to detect the heterogeneous mycotoxins contamination in bulk foods. The poster provides some results of feasibility experiments indicating the capability of this technology for inspection of commodities bulks for the detection of mycotoxins, at legal limits, in naturally contaminated food.

Preliminary results of thermal conductivity and elastic wave velocity measurements of various rock samples collected from outcrops in hanging wall of the Alpine Fault

NASA Astrophysics Data System (ADS)

Lin, W.; Tadai, O.; Shigematsu, N.; Nishikawa, O.; Mori, H.; Townend, J.; Capova, L.; Saito, S.; Kinoshita, M.

2015-12-01

The Alpine Fault is a mature active fault zone likely to rupture in the near future and DFDP aims to measure physical and chemical conditions within the fault. DFDP-2B borehole was drilled into hanging wall of the Alpine Fault. Downhole temperature measurements carried out in DFDP-2B borehole showed that the geothermal gradient in the hanging wall of the fault is very high, likely reaching to 130-150 °C/km (Sutherland et al., 2015 AGU Fall Meeting). To explain this abnormal feature, the determination of thermal properties of all the rock types in the hanging wall of the Alpine Fault is essential. To measure thermal properties and elastic wave velocities, we collected six typical rock block samples from outcrops in Stony creek and Gaunt creek. These include ultramylonite, mylonite, muscovite schist, garnet amphibolite, protomylonite and schist, which are representative of the hanging wall of the Alpine Fault. Their wet bulk densities are 2.7 - 2.8 g/cm3, and porosities are 1.4 - 3.0%. We prepared a pair of 4 cm cube specimens of each rock type with one flat plane parallel to the foliation. First, we measured thermal conductivity by the transient plane heat source (hot disc) method in a bulk mode, i.e. to deal with the rock as an isotropic material. However, several samples have clearly visible foliation and are likely to be anisotropic. Thus, the data measured in bulk mode provided an average value of the rocks in the range of approximately 2.4 - 3.2 W/mK. The next step will be to measure thermal conductivity in an anisotropic mode. We also measured P wave velocity (Vp) using the same samples, but in two directions, i.e. parallel and perpendicular to the foliation, respectively. Our preliminary results suggested that Vp is anisotropic in all the six rocks. Generally, Vp parallel to foliation is higher than that in the perpendicular direction. Vp in the parallel direction ranged in 5.5 - 6.0 km/s, whereas in the perpendicular direction it was 4.4 - 5.5 km/s. We thank the PIs and onsite staffs of the DFDP-2 project for their helps to collecting rock samples, and the financial support by JSPS (Japan-New Zealand Joint Research Program).

Developments in Impeller/Seal Secondary Flow Path Modeling for Dynamic Force Coefficients and Leakage

NASA Technical Reports Server (NTRS)

Palazzolo, Alan; Bhattacharya, Avijit; Athavale, Mahesh; Venkataraman, Balaji; Ryan, Steve; Funston, Kerry

1997-01-01

This paper highlights bulk flow and CFD-based models prepared to calculate force and leakage properties for seals and shrouded impeller leakage paths. The bulk flow approach uses a Hir's based friction model and the CFD approach solves the Navier Stoke's (NS) equation with a finite whirl orbit or via analytical perturbation. The results show good agreement in most instances with available benchmarks.

Haptoglobin and serum amyloid A in bulk tank milk in relation to raw milk quality.

PubMed

Akerstedt, Maria; Waller, Karin Persson; Sternesjö, Ase

2009-11-01

The aim of the present study was to evaluate relationships between the presence of the two major bovine acute phase proteins haptoglobin (Hp) and serum amyloid A (SAA) and raw milk quality parameters in bulk tank milk samples. Hp and SAA have been suggested as specific markers of mastitis but recently also as markers for raw milk quality. Since mastitis has detrimental effects on milk quality, it is important to investigate whether the presence of Hp or SAA indicates such changes in the composition and properties of the milk. Bulk tank milk samples (n=91) were analysed for Hp, SAA, total protein, casein, whey protein, proteolysis, fat, lactose, somatic cell count and coagulating properties. Samples with detectable levels of Hp had lower casein content, casein number and lactose content, but higher proteolysis than samples without Hp. Samples with detectable levels of SAA had lower casein number and lactose content, but higher whey protein content than samples without SAA. The presence of acute phase proteins in bulk tank milk is suggested as an indicator for unfavourable changes in the milk composition, e.g. protein quality, due to udder health disturbances, with economical implications for the dairy industry.

The thermal and physical characteristics of the Gao-Guenie (H5) meteorite

NASA Astrophysics Data System (ADS)

Beech, Martin; Coulson, Ian M.; Nie, Wenshuang; McCausland, Phil

2009-06-01

Measurements of the bulk density, grain density, porosity, and magnetic susceptibility of 19 Gao-Guenie H5 chondrite meteorite samples are presented. We find average values of bulk density < ρbulk>=3.46±0.07 g/cm 3, grain density < ρgrain>=3.53±0.08 g/cm 3, porosity < P(%)>=2.46±1.39, and bulk mass magnetic susceptibility =5.23±0.11. Measurements of the specific heat capacity for a 3.01-g Gao-Guenie sample, a 61.37-g Gao-Guenie sample, a 62.35-g Jilin H5 chondrite meteorite sample, and a 51.37-g Sikhote-Alin IIAB Iron meteorite sample are also presented. Temperature interpolation formula are further provided for the specific heat capacity, thermal conductivity, and thermal diffusivity of the 3.01-g Gao-Guenie sample in the temperature range 300< T (K)<800. We briefly review the possible effects of the newly deduced specific heat and thermal conductivity values on the ablation of meteoroids within the Earth's atmosphere, the modeling of asteroid interiors and the orbital evolution of meteoroids through the Yarkovsky-O'Keefe-Radzievskii-Paddack (YORP) effect.

Bulk specific gravity round-robin using the Corelok vacuum sealing device

DOT National Transportation Integrated Search

2002-11-01

This project conducted an evaluation of the Corelok device for the determination of the bulk specific gravity of compacted hot mix asphalt samples. The project consisted of the bulk specific gravity determination for compacted HMA mixes utilizing the...

Catalytic performance of Mn 3O 4 and Co 3O 4 nanocrystals prepared by sonochemical method in epoxidation of styrene and cyclooctene

NASA Astrophysics Data System (ADS)

Askarinejad, Azadeh; Bagherzadeh, Mojtaba; Morsali, Ali

2010-09-01

A simple sonochemical method was developed to synthesis uniform sphere-like Co 3O 4 and Mn 3O 4 nanocrystals. Epoxidation of styrene and cyclooctene by anhydrous tert-butyl hydroperoxide over the prepared Co 3O 4 and Mn 3O 4 nanocatalysts was investigated. The results of conversion activity were compared with bulk Co 3O 4 and Mn 3O 4. Under optimized reaction conditions, the nanocatalysts showed a superior catalytic performance as compared to the bulk catalysts. Powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and BET surface area, were used to characterize and investigate the nanocatalysts.

Estimation of Phonon and Carrier Thermal Conductivities for Bulk Thermoelectric Materials Using Transport Properties

NASA Astrophysics Data System (ADS)

Otsuka, Mioko; Homma, Ryoei; Hasegawa, Yasuhiro

2017-05-01

The phonon and carrier thermal conductivities of thermoelectric materials were calculated using the Wiedemann-Franz law, Boltzmann equation, and a method we propose in this study called the Debye specific heat method. We prepared polycrystalline n-type doped bismuth telluride (BiTe) and bismuth antimony (BiSb) bulk alloy samples and measured six parameters (Seebeck coefficient, resistivity, thermal conductivity, thermal diffusivity, magneto-resistivity, and Hall coefficient). The carrier density and mobility were estimated for calculating the carrier thermal conductivity by using the Boltzmann equation. In the Debye specific heat method, the phonon thermal diffusivity, and thermal conductivity were calculated from the temperature dependence of the effective specific heat by using not only the measured thermal conductivity and Debye model, but also the measured thermal diffusivity. The carrier thermal conductivity was also evaluated from the phonon thermal conductivity by using the specific heat. The ratio of carrier thermal conductivity to thermal conductivity was evaluated for the BiTe and BiSb samples, and the values obtained using the Debye specific heat method at 300 K were 52% for BiTe and <5.5% for BiSb. These values are either considerably larger or smaller than those obtained using other methods. The Dulong-Petit law was applied to validate the Debye specific heat method at 300 K, which is significantly greater than the Debye temperature of the BiTe and BiSb samples, and it was confirmed that the phonon specific heat at 300 K has been accurately reproduced using our proposed method.

Determination of residual solvents in bulk pharmaceuticals by thermal desorption/gas chromatography/mass spectrometry.

PubMed

Urakami, K; Saito, Y; Fujiwara, Y; Watanabe, C; Umemoto, K; Godo, M; Hashimoto, K

2000-12-01

Thermal desorption (TD) techniques followed by capillary GC/MS were applied for the analysis of residual solvents in bulk pharmaceuticals. Solvents desorbed from samples by heating were cryofocused at the head of a capillary column prior to GC/MS analysis. This method requires a very small amount of sample and no sample pretreatment. Desorption temperature was set at the point about 20 degrees C higher than the melting point of each sample individually. The relative standard deviations of this method tested by performing six consecutive analyses of 8 different samples were 1.1 to 3.1%, and analytical results of residual solvents were in agreement with those obtained by direct injection of N,N-dimethylformamide solution of the samples into the GC. This novel TD/GC/MS method was demonstrated to be very useful for the identification and quantification of residual solvents in bulk pharmaceuticals.

Occurrence of Staphylococcus aureus in raw milk produced in dairy farms in São Paulo state, Brazil

PubMed Central

Fagundes, Helena; Barchesi, Luciana; Filho, Antonio Nader; Ferreira, Luciano Menezes; Oliveira, Carlos Augusto Fernandes

2010-01-01

The objective of the present study was to evaluate the occurrence of Staphylococcus aureus in milk produced in 37 farms located in the regions of Ribeirão Preto and São Carlos, state of São Paulo, Brazil. Two-hundred and eight samples of milk from individual cows showing subclinical mastitis, and 37 samples of bulk tank milk were analyzed. S. aureus strains were detected in 18 (7.3%) milk samples: 14 (6.7%) from samples of individual cows, and 4 (10.8%) from bulk tank milk. Two individual milk samples (14.3%) and two bulk milk samples contained enterotoxigenic S. aureus. PFGE analysis revealed the genetic heterogeneity of the strains isolated from raw milk, which presented to 13 S. aureus patterns. Results confirmed the potential transmission of staphylococcal food poisoning to consumers via milk of cows affected by subclinical mastitis, mainly when raw milk is ingested. PMID:24031507

Fracture Toughness Properties of Gd123 Superconducting Bulks

NASA Astrophysics Data System (ADS)

Fujimoto, H.; Murakami, A.

Fracture toughness properties of melt growth GdBa2Cu3Ox (Gd123) large single domain superconducting bulks with Ag2O of 10 wt% and Pt of 0.5 wt%; 45 mm in diameter and 25 mm in thickness with low void density were evaluated at 77 K through flexural tests of specimens cut from the bulks, and compared to those of a conventional Gd123 with voids. The densified Gd123 bulks were prepared with a seeding and temperature gradient method; first melt processed in oxygen, then crystal growth in air; two-step regulated atmosphere heat treatment. The plane strain fracture toughness, KIC was obtained by the three point flexure test of the specimens with through precrack, referring to the single edge pre-cracked beam (SEPB) method, according to the JIS-R-1607, Testing Methods for Fracture Toughness of High Performance Ceramics. The results show that the fracture toughness of the densified Gd123 bulk with low void density was higher than that of the standard Gd123 bulk with voids, as well as the flexural strength previously reported. We also compared the fracture toughness of as-grown bulks with that of annealed bulks. The relation between the microstructure and the fracture toughness of the Gd123 bulk was clearly shown.

Exploring the Utilization of Low-Pressure, Piston-Cylinder Experiments to Determine the Bulk Compositions of Finite, Precious Materials

NASA Technical Reports Server (NTRS)

Vander Kaaden, K. E.; McCubbin, F. M.; Harrington, A. D.

2017-01-01

Determining the bulk composition of precious materials with a finite mass (e.g., meteorite samples) is extremely important in the fields of Earth and Planetary Science. From meteorite studies we are able to place constraints on large scale planetary processes like global differentiation and subsequent volcanism, as well as smaller scale processes like crystallization in a magma chamber or sedimentary compaction at the surface. However, with meteorite samples in particular, far too often we are limited by how precious the sample is as well as its limited mass. In this study, we have utilized aliquots of samples previously studied for toxicological hazards, including both the fresh samples (lunar mare basalt NWA 4734, lunar regolith breccia NWA 7611, martian basalt Tissint, martian regolith breccia NWA 7034, a vestian basalt Berthoud, a vestian regolith breccia NWA 2060, and a terrestrial mid-ocean ridge basalt (MORB)), and those that underwent iron leaching (Tissint, NWA 7034, NWA 4734, MORB). With these small masses of material, we performed low pressure (approx. 0.75 GPa), high temperature (greater than 1600 degrees Celsius) melting experiments. Each sample was analyzed using a JEOL 8530F electron microprobe to determine the bulk composition of the materials that were previously examined. When available, the results of our microprobe data were compared with bulk rock compositions in the literature. The results of this study show that with this technique, only approx. 50 mg of sample is required to accurately determine the bulk composition of the materials of interest.

Cell fixation and preservation for droplet-based single-cell transcriptomics.

PubMed

Alles, Jonathan; Karaiskos, Nikos; Praktiknjo, Samantha D; Grosswendt, Stefanie; Wahle, Philipp; Ruffault, Pierre-Louis; Ayoub, Salah; Schreyer, Luisa; Boltengagen, Anastasiya; Birchmeier, Carmen; Zinzen, Robert; Kocks, Christine; Rajewsky, Nikolaus

2017-05-19

Recent developments in droplet-based microfluidics allow the transcriptional profiling of thousands of individual cells in a quantitative, highly parallel and cost-effective way. A critical, often limiting step is the preparation of cells in an unperturbed state, not altered by stress or ageing. Other challenges are rare cells that need to be collected over several days or samples prepared at different times or locations. Here, we used chemical fixation to address these problems. Methanol fixation allowed us to stabilise and preserve dissociated cells for weeks without compromising single-cell RNA sequencing data. By using mixtures of fixed, cultured human and mouse cells, we first showed that individual transcriptomes could be confidently assigned to one of the two species. Single-cell gene expression from live and fixed samples correlated well with bulk mRNA-seq data. We then applied methanol fixation to transcriptionally profile primary cells from dissociated, complex tissues. Low RNA content cells from Drosophila embryos, as well as mouse hindbrain and cerebellum cells prepared by fluorescence-activated cell sorting, were successfully analysed after fixation, storage and single-cell droplet RNA-seq. We were able to identify diverse cell populations, including neuronal subtypes. As an additional resource, we provide 'dropbead', an R package for exploratory data analysis, visualization and filtering of Drop-seq data. We expect that the availability of a simple cell fixation method will open up many new opportunities in diverse biological contexts to analyse transcriptional dynamics at single-cell resolution.

Thermoelectric properties of Si/CoSi2 sub-micrometer composites prepared by melt-spinning technique

NASA Astrophysics Data System (ADS)

Xie, Jun; Ohishi, Yuji; Ichikawa, Satoshi; Muta, Hiroaki; Kurosaki, Ken; Yamanaka, Shinsuke

2017-05-01

We here report on the influence of CoSi2 precipitates on the thermoelectric properties of heavily doped p-type Si. A simple self-assembly process using a melt-spinning technique followed by spark plasma sintering is introduced to prepare bulk Si/CoSi2 composites with a nominal composition of (Si0.99B0.01)95Co5. Scanning and transmission electron microscopy observations present clear evidence of a sub-micrometer CoSi2 phase with a size ranging from 50 to 500 nm. These sub-micrometer precipitates resulted in a retention of the high electrical performance of heavily doped Si, while simultaneously reducing thermal conductivity by over 20% compared to a coarse CoSi2 phase (1-10 μm) in a comparative sample prepared by arc melting and spark plasma sintering. As a result, a figure of merit ZT value of 0.21 at 1073 K was achieved in the sub-micrometer Si/CoSi2, an increase of 16% compared with the ZT value for homogeneous p-type Si with a similar carrier concentration. This suggests that the self-assembled sub-micrometer inclusions effectively enhanced the thermoelectric performance of Si-based thermoelectric materials.

Moderate Bacterial Etching Allows Scalable and Clean Delamination of g-C3N4 with Enriched Unpaired Electrons for Highly Improved Photocatalytic Water Disinfection.

PubMed

Kang, Shifei; Huang, Wei; Zhang, Lu; He, Maofen; Xu, Suyun; Sun, Di; Jiang, Xia

2018-04-25

Delamination treatment is crucial in promoting the activity of bulk graphitic carbon nitride (g-C 3 N 4 ). However, most of the currently used methods of exfoliating bulk g-C 3 N 4 to achieve g-C 3 N 4 thin layers suffer from low yield and environmental pollution. Herein, we developed a facile bacterial etching approach for the preparation of high-quality g-C 3 N 4 nanosheets by exfoliating bulk g-C 3 N 4 under room temperature. Morphology and physicochemical characterizations show that the bacteria-treated g-C 3 N 4 (BT-CN) samples, especially BT-CN-2d, have a lamina-like two-dimensional (2D) in-plane porous structure, a significantly enlarged specific surface area (82.61 m 2 g -1 ), and a remarkable narrow band gap (2.11 eV). X-ray photoelectron spectroscopy and electron paramagnetic resonance spectra confirm the dramatic enrichment of unpaired electron in the BT-CN-2d g-C 3 N 4 nanosheets. EIS spectra and photocurrent tests indicate the fast electron transportation. As a result, the representative BT-CN-2d g-C 3 N 4 photocatalyst shows an optimal visible light-driven photocatalytic performance in water disinfection (fourfold higher than bulk g-C 3 N 4 ), as well as good cycle stability. This moderate and clean bacterial etching process can be realized in tens of gram scale in the laboratory and should be readily extended to kilogram scale. The present work provides fundamental knowledge about the scalable production of high-quality g-C 3 N 4 by bioengineering method, offering extendable availability for designing and fabricating other functional 2D materials.

Cadmium Isotope Variations in Bulk Chondrites: The Effect of Thermal Neutron Capture

NASA Astrophysics Data System (ADS)

Toth, E. R.; Schönbächler, M.; Friebel, M.; Fehr, M. A.

2017-07-01

Cadmium isotope data will be presented for bulk carbonaceous and enstatite chondrites, and acid leachates of Jbilet Winselwan (CM). Results of bulk samples show Cd isotope variations that are in good agreement with models of thermal neutron capture.

New Phases of YBaCuGeO Superconductors Identified from X-ray Diffraction and Infra-red Absorption Measurements

NASA Astrophysics Data System (ADS)

Abo-Arais, Ahmed; Dawoud, Mohamad Ahmad Taher

2005-01-01

X-ray powder diffraction patterns and infra-red absorption spectra have been evaluated and analysed for the Y1 Ba2 Cu3 O7-d - Gex compound samples prepared by the solid state reaction with x values ranging from 0.0 to 1.13. All samples show bulk superconductivity above liquid nitrogen temperature using the levitation test (Meissner effect). Samples with Ge content up to x = 0.2 have offset Tc between 83K and 92K while the sample with x = 1.13 shows semiconducting behavior above 100K. As a result of the solid state interaction between YBCO and Ge, new phases are observed and determined, mainly three phases are concluded from X-ray powder diffraction analysis: (i) Ba2GeO4 (ii) Y2BaCuO5 (iii) BaCO3. The unit cell parameters a, b and c of the orthorhombic superconducting phase are calculated for all the prepared samples. The anisotropy factor is evaluated and related to the new structural phases in YBCO-Ge composite system. The I-R absorption spectra for the samples with orthorhombic symmetry have been determined. The phonon modes between ~ 400 cm-1 and 630 cm-1 are attributed to the Cu - O octahedron and pyramid vibrations for the CuO2 -planes and CuO-chains, while the peaks in the range from ~ 700 cm-1 to ~ 860 cm-1 may be due to defects such as the new phase Ba2GeO4 and the green phase Y2BaCuO5. The obtained results are discussed according to the superconductor - semi-conductor composite model and with the phonon-mediated charge transfer between CuO2 -planes and CuO- chains through apex oxygen (BaO).

Determination of Metal Elements in Wine Using Laser-Induced Breakdown Spectroscopy (LIBS).

PubMed

Bocková, Jana; Tian, Ye; Yin, Hualiang; Delepine-Gilon, Nicole; Chen, Yanping; Veis, Pavel; Yu, Jin

2017-08-01

We developed a method for sensitive elemental analysis of wines using laser-induced breakdown spectroscopy (LIBS). In order to overcome the inefficiency of direct ablation of bulk wine (an organic liquid), a thin layer of wine residue was prepared on a metallic target according to an appropriated heating procedure applied to an amount of liquid wine dropped on the target surface. The obtained ensemble was thus ablated. Such a sample preparation procedure used a very small volume of 2 mL of wine and took only 30 min without reagent or solvent. The results show the detection of tens of metal and non-metal elements including majors (Na, Mg, K, Ca), minors, and traces (Li, B, Si, P, Ti, Mn, Fe, Cu, Zn, Rb, Sr, Ba, and Pb) in wines purchased from local supermarkets and from different production places in France. Commercially available wines were then spiked with certified standard solutions of Ti and Fe. Three series of laboratory reference samples were thus prepared using three different wines (a red wine and a white wine from a same production region and a red wine from another production region) with concentrations of Ti and Fe in the range of 1-40 mg/L. Calibration graphs established with the spiked samples allowed extracting the figures-of-merit parameters of the method for wine analysis such as the coefficient of determination ( R 2 ) and the limits of detection and quantification (LOD and LOQ). The calibration curves built with the three wines were then compared. We studied the residual matrix effect between these wines in the determination of the concentrations of Ti and Fe.

Detection of Mycobacterium avium subspecies paratuberculosis specific IS900 insertion sequences in bulk-tank milk samples obtained from different regions throughout Switzerland

PubMed Central

Corti, Sabrina; Stephan, Roger

2002-01-01

Background Since Mycobacterium avium subspecies paratuberculosis (MAP) was isolated from intestinal tissue of a human patient suffering Crohn's disease, a controversial discussion exists whether MAP have a role in the etiology of Crohn's disease or not. Raw milk may be a potential vehicle for the transmission of MAP to human population. In a previous paper, we have demonstrated that MAP are found in raw milk samples obtained from a defined region in Switzerland. The aim of this work is to collect data about the prevalence of MAP specific IS900 insertion sequence in bulk-tank milk samples in different regions of Switzerland. Furthermore, we examined eventual correlation between the presence of MAP and the somatic cell counts, the total colony counts and the presence of Enterobacteriaceae. Results 273 (19.7%) of the 1384 examined bulk-tank milk samples tested IS900 PCR-positive. The prevalence, however, in the different regions of Switzerland shows significant differences and ranged from 1.7% to 49.2%. Furthermore, there were no statistically significant (p >> 0.05) differences between the somatic cell counts and the total colony counts of PCR-positive and PCR-negative milk samples. Enterobacteriaceae occur as often in IS900 PCR-positive as in PCR-negative milk samples. Conclusion This is the first study, which investigates the prevalence of MAP in bulk-tank milk samples all over Switzerland and infers the herd-level prevalence of MAP infection in dairy herds. The prevalence of 19.7% IS900 PCR-positive bulk-milk samples shows a wide distribution of subclinical MAP-infections in dairy stock in Switzerland. MAP can therefore often be transmitted to humans by raw milk consumption. PMID:12097144

Contrasting effects of non-starch polysaccharide and resistant starch-based diets on the disposition and excretion of the food carcinogen, 2-amino-3-methylimidazo[4,5-f]quinoline (IQ), in a rat model.

PubMed

Ferguson, Lynnette R; Zhu, Shuotun; Kestell, Philip

2003-06-01

It has commonly been believed that increasing fibre in the diet should reduce the incidence of cancers, especially those of the colon and rectum. The earliest definitions of dietary fibre restricted the term to plant cell walls in which non-starch polysaccharides are key chemical components. However, new definitions encompass a wider range of materials, including starches resistant to digestion in the colon (resistant starches). Nevertheless, most definitions require that "dietary fibres" show physiological effects considered beneficial against cancer, including enhanced laxation and faecal bulking. On theoretical grounds, such properties might be expected to dilute the concentration of any carcinogen present and move it more rapidly through the colon, thereby reducing bioavailability. We have compared the properties of two dietary fibre preparations that are primarily non-starch polysaccharides with two resistant starch preparations for effects on carcinogen disposition in a rodent model. Although both preparations enhanced laxation and faecal bulking, only the non-starch polysaccharide preparation reduced carcinogen biovailability. Indeed, carcinogen biovailability was significantly enhanced by resistant starch. We suggest that there may be fundamental differences in the manner by which non-starch polysaccharides or resistant starches affect carcinogen disposition, and express concern that the events seen with the resistant starches [RS] are unlikely to be beneficial with respect to protection against cancer by exogenous carcinogens. Furthermore, the data reveal that the observation of enhanced laxation and faecal bulking does not necessarily imply a reduction in carcinogen bioavailability.

Development of high Tc (greater than 100 K) Bi, Tl and Y-based materials as superconducting circuit elements

NASA Technical Reports Server (NTRS)

Haertling, Gene; Grabert, Gregory; Gilmour, Phillip

1994-01-01

Experimental work on this project over the last four years has resulted in establishing processing and characterization techniques for producing both the Bi-based and Tl-based superconductors in their high temperature (2223) forms. In the bulk, dry pressed form, maximum critical temperatures (Tc) of 108.2 K and 117.8 K, respectively, were measured. Results have further shown that the Bi and Tl-based superconducting materials in bulk form are noticeably different from the Y-based 123 material in that superconductivity is considerably harder to achieve, maintain, and reproduce. This is due primarily to the difficulty in obtaining the higher Tc phase in pure form since it commonly co-exists with other undesirable, lower Tc phases. In particular, it has been found that long processing times for calcining and firing (20 - 200 hrs.) and close control of temperatures which are very near the melting point are required in order to obtain higher proportions of the desirable, high Tc (2223) phase. Thus far, the BSCCO bulk materials has been prepared in uniaxially pressed, hot pressed, and tapecast form. The uniaxially pressed material has been synthesized by the mixed oxide, coprecipitation, and melt quenching processes. The tapecast and hot pressed materials have been prepared via the mixed oxide process. In addition, thick films of BSCCO (2223 phase) have been prepared by screen printing on to yttria and magnesia stabilized zirconia with only moderate success; i.e., superconductivity was achieved in these thick films, but the highest Tc obtained in these films was 89.0 K. The Tc's of the bulk hot pressed, tapecast, and screen printed thick film materials were found to be 108.2, 102.4, and 89.0 K, respectively.

46 CFR 153.935 - Opening of tanks and cargo sampling.

Code of Federal Regulations, 2010 CFR

2010-10-01

... 46 Shipping 5 2010-10-01 2010-10-01 false Opening of tanks and cargo sampling. 153.935 Section 153.935 Shipping COAST GUARD, DEPARTMENT OF HOMELAND SECURITY (CONTINUED) CERTAIN BULK DANGEROUS CARGOES SHIPS CARRYING BULK LIQUID, LIQUEFIED GAS, OR COMPRESSED GAS HAZARDOUS MATERIALS Operations General...

46 CFR 153.935 - Opening of tanks and cargo sampling.

Code of Federal Regulations, 2013 CFR

2013-10-01

... 46 Shipping 5 2013-10-01 2013-10-01 false Opening of tanks and cargo sampling. 153.935 Section 153.935 Shipping COAST GUARD, DEPARTMENT OF HOMELAND SECURITY (CONTINUED) CERTAIN BULK DANGEROUS CARGOES SHIPS CARRYING BULK LIQUID, LIQUEFIED GAS, OR COMPRESSED GAS HAZARDOUS MATERIALS Operations General...

46 CFR 153.935 - Opening of tanks and cargo sampling.

Code of Federal Regulations, 2011 CFR

2011-10-01

... 46 Shipping 5 2011-10-01 2011-10-01 false Opening of tanks and cargo sampling. 153.935 Section 153.935 Shipping COAST GUARD, DEPARTMENT OF HOMELAND SECURITY (CONTINUED) CERTAIN BULK DANGEROUS CARGOES SHIPS CARRYING BULK LIQUID, LIQUEFIED GAS, OR COMPRESSED GAS HAZARDOUS MATERIALS Operations General...

46 CFR 153.935 - Opening of tanks and cargo sampling.

Code of Federal Regulations, 2014 CFR

2014-10-01

... 46 Shipping 5 2014-10-01 2014-10-01 false Opening of tanks and cargo sampling. 153.935 Section 153.935 Shipping COAST GUARD, DEPARTMENT OF HOMELAND SECURITY (CONTINUED) CERTAIN BULK DANGEROUS CARGOES SHIPS CARRYING BULK LIQUID, LIQUEFIED GAS, OR COMPRESSED GAS HAZARDOUS MATERIALS Operations General...

46 CFR 153.935 - Opening of tanks and cargo sampling.

Code of Federal Regulations, 2012 CFR

2012-10-01

... 46 Shipping 5 2012-10-01 2012-10-01 false Opening of tanks and cargo sampling. 153.935 Section 153.935 Shipping COAST GUARD, DEPARTMENT OF HOMELAND SECURITY (CONTINUED) CERTAIN BULK DANGEROUS CARGOES SHIPS CARRYING BULK LIQUID, LIQUEFIED GAS, OR COMPRESSED GAS HAZARDOUS MATERIALS Operations General...

Temperature Dependent Electrical Properties of PZT Wafer

NASA Astrophysics Data System (ADS)

Basu, T.; Sen, S.; Seal, A.; Sen, A.

2016-04-01

The electrical and electromechanical properties of lead zirconate titanate (PZT) wafers were investigated and compared with PZT bulk. PZT wafers were prepared by tape casting technique. The transition temperature of both the PZT forms remained the same. The transition from an asymmetric to a symmetric shape was observed for PZT wafers at higher temperature. The piezoelectric coefficient (d 33) values obtained were 560 pc/N and 234 pc/N, and the electromechanical coupling coefficient (k p) values were 0.68 and 0.49 for bulk and wafer, respectively. The reduction in polarization after fatigue was only ~3% in case of PZT bulk and ~7% for PZT wafer.

In-package inhibition of E. coli O157:H7 on bulk Romaine lettuce using cold plasma.

PubMed

Min, Sea C; Roh, Si Hyeon; Niemira, Brendan A; Boyd, Glenn; Sites, Joseph E; Uknalis, Joseph; Fan, Xuetong

2017-08-01

Dielectric barrier discharge atmospheric cold plasma (DACP) treatment was evaluated for the inactivation of Escherichia coli O157:H7, surface morphology, color, carbon dioxide generation, and weight loss of bulk Romaine lettuce in a commercial plastic clamshell container. The lettuce samples were packed in a model bulk packaging configuration (three rows with either 1, 3, 5, or 7 layers) in the container and treated by DACP (42.6 kV, 10 min). DACP treatment reduced the number of E. coli O157:H7 in the leaf samples in the 1-, 3-, and 5-layer configurations by 0.4-0.8 log CFU/g lettuce, with no significant correlation to the sample location (P > 0.05). In the largest bulk stacking with 7 layers, a greater degree of reduction (1.1 log CFU/g lettuce) was observed at the top layer, but shaking the container increased the uniformity of the inhibition. DACP did not significantly change the surface morphology, color, respiration rate, or weight loss of the samples, nor did these properties differ significantly according to their location in the bulk stack. DACP treatment inhibited E. coli O157:H7 on bulk lettuce in clamshell containers in a uniform manner, without affecting the physical and biological properties and thus holds promise as a post-packaging process for fresh and fresh-cut fruits and vegetables. Published by Elsevier Ltd.

Scanning measurement of Seebeck coefficient of a heated sample

DOE Office of Scientific and Technical Information (OSTI.GOV)

Snyder, G. Jeffrey; Iwanaga, Shiho

2016-04-19

A novel scanning Seebeck coefficient measurement technique is disclosed utilizing a cold scanning thermocouple probe tip on heated bulk and thin film samples. The system measures variations in the Seebeck coefficient within the samples. The apparatus may be used for two dimensional mapping of the Seebeck coefficient on the bulk and thin film samples. This technique can be utilized for detection of defective regions, as well as phase separations in the sub-mm range of various thermoelectric materials.

Retrieving cosmological signal using cosmic flows

NASA Astrophysics Data System (ADS)

Bouillot, V.; Alimi, J.-M.

2011-12-01

To understand the origin of the anomalously high bulk flow at large scales, we use very large simulations in various cosmological models. To disentangle between cosmological and environmental effects, we select samples with bulk flow profiles similar to the observational data Watkins et al. (2009) which exhibit a maximum in the bulk flow at 53 h^{-1} Mpc. The estimation of the cosmological parameters Ω_M and σ_8, done on those samples, is correct from the rms mass fluctuation whereas this estimation gives completely false values when done on bulk flow measurements, hence showing a dependance of velocity fields on larger scales. By drawing a clear link between velocity fields at 53 h^{-1} Mpc and asymmetric patterns of the density field at 85 h^{-1} Mpc, we show that the bulk flow can depend largely on the environment. The retrieving of the cosmological signal is achieved by studying the convergence of the bulk flow towards the linear prediction at very large scale (˜ 150 h^{-1} Mpc).

Effect of surface morphology on friction of graphene on various substrates

NASA Astrophysics Data System (ADS)

Cho, Dae-Hyun; Wang, Lei; Kim, Jin-Seon; Lee, Gwan-Hyoung; Kim, Eok Su; Lee, Sunhee; Lee, Sang Yoon; Hone, James; Lee, Changgu

2013-03-01

The friction of graphene on various substrates, such as SiO2, h-BN, bulk-like graphene, and mica, was investigated to characterize the adhesion level between graphene and the underlying surface. The friction of graphene on SiO2 decreased with increasing thickness and converged around the penta-layers due to incomplete contact between the two surfaces. However, the friction of graphene on an atomically flat substrate, such as h-BN or bulk-like graphene, was low and comparable to that of bulk-like graphene. In contrast, the friction of graphene folded onto bulk-like graphene was indistinguishable from that of mono-layer graphene on SiO2 despite the ultra-smoothness of bulk-like graphene. The characterization of the graphene's roughness before and after folding showed that the corrugation of graphene induced by SiO2 morphology was preserved even after it was folded onto an atomically flat substrate. In addition, graphene deposited on mica, when folded, preserved the same corrugation level as before the folding event. Our friction measurements revealed that graphene, once exfoliated from the bulk crystal, tends to maintain its corrugation level even after it is folded onto an atomically flat substrate and that ultra-flatness in both graphene and the substrate is required to achieve the intimate contact necessary for strong adhesion.The friction of graphene on various substrates, such as SiO2, h-BN, bulk-like graphene, and mica, was investigated to characterize the adhesion level between graphene and the underlying surface. The friction of graphene on SiO2 decreased with increasing thickness and converged around the penta-layers due to incomplete contact between the two surfaces. However, the friction of graphene on an atomically flat substrate, such as h-BN or bulk-like graphene, was low and comparable to that of bulk-like graphene. In contrast, the friction of graphene folded onto bulk-like graphene was indistinguishable from that of mono-layer graphene on SiO2 despite the ultra-smoothness of bulk-like graphene. The characterization of the graphene's roughness before and after folding showed that the corrugation of graphene induced by SiO2 morphology was preserved even after it was folded onto an atomically flat substrate. In addition, graphene deposited on mica, when folded, preserved the same corrugation level as before the folding event. Our friction measurements revealed that graphene, once exfoliated from the bulk crystal, tends to maintain its corrugation level even after it is folded onto an atomically flat substrate and that ultra-flatness in both graphene and the substrate is required to achieve the intimate contact necessary for strong adhesion. Electronic supplementary information (ESI) available: Sample preparation method, identification of graphene thickness, AFM and FFM measurements. See DOI: 10.1039/c3nr34181j

Preparation of extrusions of bulk mixed oxide compounds with high macroporosity and mechanical strength

DOEpatents

Flytzani-Stephanopoulos, Maria; Jothimurugesan, Kandaswami

1990-01-01

A simple and effective method for producing bulk single and mixed oxide absorbents and catalysts is disclosed. The method yields bulk single oxide and mixed oxide absorbent and catalyst materials which combine a high macroporosity with relatively high surface area and good mechanical strength. The materials are prepared in a pellet form using as starting compounds, calcined powders of the desired composition and physical properties these powders are crushed to broad particle size distribution, and, optionally may be combined with an inorganic clay binder. The necessary amount of water is added to form a paste which is extruded, dried and heat treated to yield and desired extrudate strength. The physical properties of the extruded materials (density, macroporosity and surface area) are substantially the same as the constituent powder is the temperature of the heat treatment of the extrudates is approximately the same as the calcination temperature of the powder. If the former is substantially higher than the latter, the surface area decreases, but the macroporosity of the extrusions remains essentially constant.

The performance of spinel bulk-like oxygen-deficient CoGa2O4 as an air-cathode catalyst in microbial fuel cell

NASA Astrophysics Data System (ADS)

Liu, Di; Mo, Xiaoping; Li, Kexun; Liu, Yi; Wang, Junjie; Yang, Tingting

2017-08-01

Nano spinel bulk-like CoGa2O4 prepared via a facile hydrothermal method is used as a high efficient electrochemical catalyst in activated carbon (AC) air-cathode microbial fuel cell (MFC). The maximum power density of the modified MFC is 1911 ± 49 mW m-2, 147% higher than the MFC of untreated AC cathode. Transmission electron microscope (TEM) and X-ray diffraction (XRD) exhibit the morphology and crystal structure of CoGa2O4. Rotating disk electrode (RDE) confirms the four-electron pathway at the cathode during the oxygen reduction reaction (ORR). Thermogravimetric analysis (TGA) and X-ray photoelectron spectroscopy (XPS) illustrate that the high rate oxygen vacancy exist in the CoGa2O4. The oxygen vacancy of CoGa2O4 plays an important role in catalytic activity. In a word, the prepared nano spinel bulk-like CoGa2O4 provides an alternative to the costly Pt in air-cathode for power output.

Preparation of porous lead from shape-controlled PbO bulk by in situ electrochemical reduction in ChCl-EG deep eutectic solvent

NASA Astrophysics Data System (ADS)

Ru, Juanjian; Hua, Yixin; Xu, Cunying; Li, Jian; Li, Yan; Wang, Ding; Zhou, Zhongren; Gong, Kai

2015-12-01

Porous lead with different shapes was firstly prepared from controlled geometries of solid PbO bulk by in situ electrochemical reduction in choline chloride-ethylene glycol deep eutectic solvents at cell voltage 2.5 V and 353 K. The electrochemical behavior of PbO powders on cavity microelectrode was investigated by cyclic voltammetry. It is indicated that solid PbO can be directly reduced to metal in the solvent and a nucleation loop is apparent. Constant voltage electrolysis demonstrates that PbO pellet can be completely converted to metal for 13 h, and the current efficiency and specific energy consumption are about 87.79% and 736.82 kWh t-1, respectively. With the electro-deoxidation progress on the pellet surface, the reduction rate reaches the fastest and decreases along the distance from surface to inner center. The morphologies of metallic products are porous and mainly consisted of uniform particles which connect with each other by finer strip-shaped grains to remain the geometry and macro size constant perfectly. In addition, an empirical model of the electro-deoxidation process from spherical PbO bulk to porous lead is also proposed. These findings provide a novel and simple route for the preparation of porous metals from oxide precursors in deep eutectic solvents at room temperature.

Spectroscopic investigation of the chemical and electronic properties of chalcogenide materials for thin-film optoelectronic devices

NASA Astrophysics Data System (ADS)

Horsley, Kimberly Anne

Chalcogen-based materials are at the forefront of technologies for sustainable energy production. This progress has come only from decades of research, and further investigation is needed to continue improvement of these materials. For this dissertation, a number of chalcogenide systems were studied, which have applications in optoelectronic devices, such as LEDs and Photovoltaics. The systems studied include Cu(In,Ga)Se2 (CIGSe) and CuInSe 2 (CISe) thin-film absorbers, CdTe-based photovoltaic structures, and CdTe-ZnO nanocomposite materials. For each project, a sample set was prepared through collaboration with outside institutions, and a suite of spectroscopy techniques was employed to answer specific questions about the system. These techniques enabled the investigation of the chemical and electronic structure of the materials, both at the surface and towards the bulk. CdS/Cu(In,Ga)Se2 thin-films produced from the roll-to-roll, ambient pressure, Nanosolar industrial line were studied. While record-breaking efficiency cells are usually prepared in high-vacuum (HV) or ultra-high vacuum (UHV) environments, these samples demonstrate competitive mass-production efficiency without the high-cost deposition environment. We found relatively low levels of C contaminants, limited Na and Se oxidation, and a S-Se intermixing at the CdS/CIGSe interface. The surface band gap compared closely to previously investigated CIGSe thin-films deposited under vacuum, illustrating that roll-to-roll processing is a promising and less-expensive alternative for solar cell production. An alternative deposition process for CuInSe2 was also studied, in collaboration with the University of Luxembourg. CuInSe2 absorbers were prepared with varying Cu content and surface treatments to investigate the potential to produce an absorber with a Cu-rich bulk and Cu-poor surface. This is desired to combine the bulk characteristics of reduced defects and larger grains in Cu-rich films, while maintaining a wide surface band gap, as seen in Cu-poor films. A novel absorber was prepared Cu-rich with a final In-Se treatment to produce a Cu-poor surface, and compared directly to Cu-poor and Cu-rich produced samples. Despite reduced Cu at the surface, the novel absorber was found to have a surface band gap similar to that of traditional, Cu-poor grown absorbers. Furthermore, estimation of the near-surface bulk band gap suggests a narrowing of the band gap away from the surface, similar to highly efficient, Cu-poor grown absorbers. Long-term degradation is another concern facing solar cells, as heat and moistures stress can result in reduced efficiencies over time. The interface of the back contact material and absorber layer in (Au/Cu)/CdTe/CdS thin-film structures from the University of Toledo were investigated after a variety of accelerated stress treatments with the aim of further understanding the chemical and/or electronic degradation of this interface. Sulfur migration to the back contact was observed, along with the formation of Au-S and Cu-S bonds. A correlation between heat stress under illumination and the formation of Cu-Cl bonds was also found. Nanocomposite materials hold promise as a next-generation photovoltaic material and for use in LED devices, due in part to the unique ability to tune the absorption edge of the film by adjusting the semiconductor particle size, and the prospective for long-range charge-carrier (exciton) transport through the wide band gap matrix material. Thin films of CdTe were sputter deposited onto ZnO substrates at the University of Arizona and studied before and after a short, high temperature annealing to further understand the effects of annealing on the CdTe/ZnO interface. A clumping of the CdTe layer and the formation of Cd- and Te-oxides was observed using surface microscopy and photoelectron spectroscopy techniques. These findings help to evaluate post-deposition annealing as a treatment to adjust the final crystallinity and optoelectronic properties of these films. Through publication and/or discussion with collaborators, each project presented in this dissertation contributed to the understanding of the chemical and electronic properties of the material surface, near-surface bulk, and/or interfaces formed. The information gained on these unique chalcogenide materials will assist in designing more efficient and successful optoelectronic devices for the next generation of solar cells and LEDs.

Magnetoresistivity and microstructure of YBa2Cu3Oy prepared using planetary ball milling

NASA Astrophysics Data System (ADS)

Hamrita, A.; Ben Azzouz, F.; Madani, A.; Ben Salem, M.

2012-01-01

We have studied the microstructure and the magnetoresistivity of polycrystalline YBa2Cu3Oy (YBCO or Y-123 for brevity) embedded with nanoparticles of Y-deficient YBCO, generated by the planetary ball milling technique. Bulk samples were synthesized from a precursor YBCO powder, which was prepared from commercial high purity Y2O3, Ba2CO3 and CuO via a one-step annealing process in air at 950 °C. After planetary ball milling of the precursor, the powder was uniaxially pressed and subsequently annealed at 950 °C in air. Phase analysis by X-ray diffraction (XRD), granular structure examination by scanning electron microscopy (SEM), microstructure investigation by transmission electron microscopy (TEM) coupled with energy dispersive X-ray spectroscopy (EDXS) were carried out. TEM analyses show that nanoparticles of Y-deficient YBCO, generated by ball milling, are embedded in the superconducting matrix. Electrical resistance as a function of temperature, ρ(T), revealed that the zero resistance temperature, Tco, is 84.5 and 90 K for the milled and unmilled samples respectively. The milled ceramics exhibit a large magnetoresistance in weak magnetic fields at liquid nitrogen temperature. This attractive effect is of high significance as it makes these materials promising candidates for practical application in magnetic field sensor devices.

Synthesis of Hierarchical Self-Assembled CuO and Their Structure-Enhanced Photocatalytic Performance

NASA Astrophysics Data System (ADS)

Wang, Dagui; Yan, Bing; Song, Caixiong; Ye, Ting; Wang, Yongqian

2018-01-01

Hierarchical self-assembled CuO hollow microspheres with superior photocatalytic performance are synthesized via a simple hydrothermal process in the presence of cationic surfactants (cetyltrimethylammonium bromide, CTAB). The structure, morphology, and optical absorption performance of CuO samples prepared with different surfactants including CTAB, nonionic surfactant (polyvinylpyrrolidone, PVP) and anionic surfactant (sodium dodecyl sulfate, SDS) are characterized by x-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), ultraviolet-visible (UV-vis) absorption spectra. Moreover, the photocatalytic performances of the CuO samples are evaluated by the photo-degradation of a simulative contaminant methylene blue. The XRD patterns and FESEM images demonstrate that the category of surfactants have effects on the phase structure and morphology of CuO. Compared with bulk CuO (1.20 eV at room temperature), the band gap of CuO microspheres prepared with different surfactants including CTAB, PVP and SDS are measured at 2.16 eV, 2.29 eV, 2.44 eV, respectively, which exhibits a blue shift in the UV-vis spectra. The synthesized hierarchical self-assembled CuO hollow microspheres reveal commendable photocatalytic activity, in which the photo-degradation rate could rise to 94.1%. Additionally, a reasonable growth mechanism of CuO microspheres synthesized with different surfactants is discussed in detail.

Evolution of microstructural defects of TiO2 nanocrystals by Zr4+ or/and Ge4+ doping lead to high disinfection efficiency for CWAs

NASA Astrophysics Data System (ADS)

Shen, Zhong; Zhong, Jin-Yi; Chai, Na-Na; He, Xin; Zang, Jian-Zheng; Xu, Hui; Han, Xiao-Yuan; Zhang, Peng

2017-06-01

Zr4+, Ge4+ doped and co-doped TiO2 nanoparticles were prepared by a 'one-pot' homogeneous precipitation method. The photocatalytic reaction kinetics of DMMP and the disinfection efficiency of HD, GD and VX on the samples were investigated. By means of a variety of characterization methods, especially the positron annihilation lifetime spectroscopy, the changes in structure and property of TiO2 across doping were studied. The results show that the reasonable engineering design of novel photocatalysts in the field of CWAs decontamination can be realized by adjusting the bulk-to-surface defects ratio, except for crystal structure, specific surface area, pore size distribution and light utilization.

Self-assembled ordered structures in thin films of HAT5 discotic liquid crystal.

PubMed

Morales, Piero; Lagerwall, Jan; Vacca, Paolo; Laschat, Sabine; Scalia, Giusy

2010-05-20

Thin films of the discotic liquid crystal hexapentyloxytriphenylene (HAT5), prepared from solution via casting or spin-coating, were investigated by atomic force microscopy and polarizing optical microscopy, revealing large-scale ordered structures substantially different from those typically observed in standard samples of the same material. Thin and very long fibrils of planar-aligned liquid crystal were found, possibly formed as a result of an intermediate lyotropic nematic state arising during the solvent evaporation process. Moreover, in sufficiently thin films the crystallization seems to be suppressed, extending the uniform order of the liquid crystal phase down to room temperature. This should be compared to the bulk situation, where the same material crystallizes into a polymorphic structure at 68 °C.

The effect of guard ring on leakage current and spectroscopic performance of TlBr planar detectors

NASA Astrophysics Data System (ADS)

Kargar, Alireza; Kim, Hadong; Cirignano, Leonard; Shah, Kanai

2014-09-01

Four thallium bromide planar detectors were fabricated from materials grown at RMD Inc. The TlBr samples were prepared to investigate the effect of guard ring on device gamma-ray spectroscopy performance, and to investigate the leakage current through surface and bulk. The devices' active area in planar configuration were 4.4 × 4.4 × 1.0 mm3. In this report, the detector fabrication process is described and the resulting energy spectra are discussed. It is shown that the guard ring improves device spectroscopic performance by shielding the sensing electrode from the surface leakage current, and by making the electric filed more uniform in the active region of the device.

Highly ordered mesoporous cobalt oxide nanostructures: synthesis, characterisation, magnetic properties, and applications for electrochemical energy devices.

PubMed

Wang, Guoxiu; Liu, Hao; Horvat, Josip; Wang, Bei; Qiao, Shizhang; Park, Jinsoo; Ahn, Hyojun

2010-09-24

Highly ordered mesoporous Co(3)O(4) nanostructures were prepared using KIT-6 and SBA-15 silica as hard templates. The structures were confirmed by small angle X-ray diffraction, high resolution transmission electron microscopy, and N(2) adsorption-desorption isotherm analysis. Both KIT-6 cubic and SBA-15 hexagonal mesoporous Co(3)O(4) samples exhibited a low Néel temperature and bulk antiferromagnetic coupling due to geometric confinement of antiferromagnetic order within the nanoparticles. Mesoporous Co(3)O(4) electrode materials have demonstrated the high lithium storage capacity of more than 1200 mAh g(-1) with an excellent cycle life. They also exhibited a high specific capacitance of 370 F g(-1) as electrodes in supercapacitors.

Bulk superconducting phase with a full energy gap in the doped topological insulator Cu(x)Bi₂Se₃.

PubMed

Kriener, M; Segawa, Kouji; Ren, Zhi; Sasaki, Satoshi; Ando, Yoichi

2011-03-25

The superconductivity recently found in the doped topological insulator Cu(x)Bi₂Se₃ offers a great opportunity to search for a topological superconductor. We have successfully prepared a single-crystal sample with a large shielding fraction and measured the specific-heat anomaly associated with the superconductivity. The temperature dependence of the specific heat suggests a fully gapped, strong-coupling superconducting state, but the BCS theory is not in full agreement with the data, which hints at a possible unconventional pairing in Cu(x)Bi₂Se₃. Also, the evaluated effective mass of 2.6m(e) (m(e) is the free electron mass) points to a large mass enhancement in this material.

Synthesis and photocatalytic performance of g-C{sub 3}N{sub 4} nanosheets via liquid phase stripping

DOE Office of Scientific and Technical Information (OSTI.GOV)

Miao, Jilin; Xu, Guangqing; Key Laboratory of Advanced Functional Materials and Devices of Anhui Province, Hefei University of Technology, Hefei 230009

Well dispersed g-C{sub 3}N{sub 4} nanosheets were prepared by exfoliating the bulk g-C{sub 3}N{sub 4} in concentrated sulfuric acid. Phase structures, morphologies and elemental compositions were characterized by X-ray diffractometer, scanning electron microscope, transmission electron microscope and X-ray photoelectron spectrometer, respectively. Optical absorption and photoluminescence were also used to explain the optical performances of samples. NaI, BQ and IPA were used as the sacrificial agents for studying the surface reactions in the photocatalytic process. By the precipitation of g-C{sub 3}N{sub 4} nanosheets in ethanol with different ratios between concentrated sulfuric acid and ethyl alcohol, well dispersed g-C{sub 3}N{sub 4} nanosheetsmore » with high specific surface area can be obtained. The optimized g-C{sub 3}N{sub 4} (1:10) nanosheets achieve the highest photocatalytic activities under UV light illumination, which can degrade 10 mg/L RhB about 98% in 60 min, which is 6 times that of bulk g-C{sub 3}N{sub 4} under UV light. - Graphical Abstract: The schematic diagram of photocatalysis and excellent photocatalytic performance of g-C{sub 3}N{sub 4} nanosheets. - Highlights: • Well dispersed g-C{sub 3}N{sub 4} were prepared via Liquid Phase Stripping. • The g-C{sub 3}N{sub 4} is in a sheet like structure after being exfoliated. • The g-C{sub 3}N{sub 4} nanosheets possess high photocatalytic performances.« less

Scanning electron microscopy of high-pressure-frozen sea urchin embryos.

PubMed

Walther, P; Chen, Y; Malecki, M; Zoran, S L; Schatten, G P; Pawley, J B

1993-12-01

High-pressure-freezing permits direct cryo-fixation of sea urchin embryos having a defined developmental state without the formation of large ice crystals. We have investigated preparation protocols for observing high-pressure-frozen and freeze-fractured samples in the scanning electron microscope. High-pressure-freezing was superior to other freezing protocols, because the whole bulk sample was reasonably well frozen and the overall three-dimensional shape of the embryos was well preserved. The samples were either dehydrated by freeze-substitution and critical-point-drying, or imaged in the partially hydrated state, using a cold stage in the SEM. During freeze-substitution the samples were stabilized by fixatives. The disadvantage of this method was that shrinking and extraction effects, caused by the removal of the water, could not be avoided. These disadvantages were avoided when the sample was imaged in the frozen-hydrated state using a cold-stage in the SEM. This would be the method of choice for morphometric studies. Frozen-hydrated samples, however, were very beam sensitive and many structures remained covered by the ice and were not visible. Frozen-hydrated samples were partially freeze-dried to make visible additional structures that had been covered by ice. However, this method also caused drying artifacts when too much water was removed.

Damage coefficients in low resistivity silicon. [solar cells

NASA Technical Reports Server (NTRS)

Srour, J. R.; Othmer, S.; Chiu, K. Y.; Curtis, O. L., Jr.

1975-01-01

Electron and proton damage coefficients are determined for low resistivity silicon based on minority-carrier lifetime measurements on bulk material and diffusion length measurements on solar cells. Irradiations were performed on bulk samples and cells fabricated from four types of boron-doped 0.1 ohm-cm silicon ingots, including the four possible combinations of high and low oxygen content and high and low dislocation density. Measurements were also made on higher resistivity boron-doped bulk samples and solar cells. Major observations and conclusions from the investigation are discussed.

Disentangling the surface and bulk electronic structures of LaOFeAs

DOE PAGES

Zhang, P.; Ma, J.; Qian, T.; ...

2016-09-20

We performed a comprehensive angle-resolved photoemission spectroscopy study of the electronic band structure of LaOFeAs single crystals. We found that samples cleaved at low temperature show an unstable and very complicated band structure, whereas samples cleaved at high temperature exhibit a stable and clearer electronic structure. Using in situ surface doping with K and supported by first-principles calculations, we identify both surface and bulk bands. Our assignments are confirmed by the difference in the temperature dependence of the bulk and surface states.

Bulk Genotyping of Biopsies Can Create Spurious Evidence for Hetereogeneity in Mutation Content.

PubMed

Kostadinov, Rumen; Maley, Carlo C; Kuhner, Mary K

2016-04-01

When multiple samples are taken from the neoplastic tissues of a single patient, it is natural to compare their mutation content. This is often done by bulk genotyping of whole biopsies, but the chance that a mutation will be detected in bulk genotyping depends on its local frequency in the sample. When the underlying mutation count per cell is equal, homogenous biopsies will have more high-frequency mutations, and thus more detectable mutations, than heterogeneous ones. Using simulations, we show that bulk genotyping of data simulated under a neutral model of somatic evolution generates strong spurious evidence for non-neutrality, because the pattern of tissue growth systematically generates differences in biopsy heterogeneity. Any experiment which compares mutation content across bulk-genotyped biopsies may therefore suggest mutation rate or selection intensity variation even when these forces are absent. We discuss computational and experimental approaches for resolving this problem.

40 CFR 761.283 - Determination of the number of samples to collect and sample collection locations.

Code of Federal Regulations, 2013 CFR

2013-07-01

... ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) TOXIC SUBSTANCES CONTROL ACT POLYCHLORINATED BIPHENYLS (PCBs...-Implementing Cleanup and On-Site Disposal of Bulk PCB Remediation Waste and Porous Surfaces in Accordance With... locations for bulk PCB remediation waste and porous surfaces destined to remain at a cleanup site after...

40 CFR 761.283 - Determination of the number of samples to collect and sample collection locations.

Code of Federal Regulations, 2014 CFR

2014-07-01

... ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) TOXIC SUBSTANCES CONTROL ACT POLYCHLORINATED BIPHENYLS (PCBs...-Implementing Cleanup and On-Site Disposal of Bulk PCB Remediation Waste and Porous Surfaces in Accordance With... locations for bulk PCB remediation waste and porous surfaces destined to remain at a cleanup site after...

Effect of fluxing treatment on the properties of Fe66Co15Mo1P7.5C5.5B2Si3 bulk metallic glass by water quenching

NASA Astrophysics Data System (ADS)

Li, Jin-Feng; Wang, Xin; Liu, Xue; Zhao, Shao-Fan; Yao, Ke-Fu

2018-01-01

The effect of fluxing treatment on the properties of Fe66Co15Mo1P7.5C5.5B2Si3bulk amorphous alloy (BAA) has been investigated. Prepared by a combination method of flux treatment and water quenching, the Fe66Co15Mo1P7.5C5.5B2Si3 BAA exhibits better glass-forming ability, thermal stability, soft magnetic properties and ductility than those of the one prepared by direct water quenching. This indicates that fluxing treatment can play a potential role in improving the properties of Fe-based BAA due to the effective elimination of the impurities within the alloy.

Temporal soil bulk density following tillage

USDA-ARS?s Scientific Manuscript database

Soil is the medium for air, energy, water, and chemical transport between the atmosphere and the solid earth. Soil bulk density is a key variable impacting the rate at which this transport occurs. Typically, soil bulk density is measured by the gravimetric method, where a sample of known volume is t...

Measurements in Vacuum of the Complex Permittivity of Planetary Regolith Analog Materials in Support of the OSIRIS-REx Mission

NASA Astrophysics Data System (ADS)

Boivin, A.; Hickson, D. C.; Cunje, A.; Tsai, C. A.; Ghent, R. R.; Daly, M. G.

2017-12-01

In preparation for the OSIRIS-REx sample return mission, ground based radar data have been used to help characterize the carbonaceous asteroid (101955) Bennu as well as to produce a 3-D shape model. Radar data have also been used to derive the near-surface bulk density of the asteroid, a key engineering factor for sample acquisition and return. The relationship between radar albedo and bulk density of the nearsurface depends on the relative permittivity of the material, in this case regolith. The relative permittivity is complex such that ɛ r = ɛ r' + i ɛ r'', where ɛ r' is the dielectric constant and ɛ r'' is the loss factor. Laboratory permittivity measurements have been made in the past on a myriad of samples including Earth materials, lunar Apollo and analog samples, Mars soil analog samples, some meteorites, and cometary analog samples in support of the Rosetta mission. These measurements have been made in different frequency bands and in various conditions; however, no measurements to date have systematically explored the effect of changes in mineralogy on the complex permittivity, and particularly the loss tangent (tanδ , the ratio of ɛ r'' to ɛ r'). The loss tangent controls the absorption of the signal by the material. Continuing our investigation of the effects of mineralogy on these properties, we will present for the first time results of complex permittivity measurements of the UCF/DSI-CI-2 CI asteroid regolith simulant produced by Deep Space Industries Inc. The simulant is mineralogically similar to the CI meteorite Orgueil. CI meteorites are the most spectrally similar meteorites to (101955) Bennu. Since the simulant has been provided to us un-mixed, several sub-samples will be created containing different amounts of carbon, thus allowing us to systematically investigate the effects of carbon content on the permittivity. In order to remove moisture from our samples, powders are baked at 250°C for 48hrs prior to being loaded into a coaxial transmission line and measured under vacuum. Measurements are made using a sweep of frequencies from 300 KHz to 8.5 GHz.

Determination of level of antibodies to bovine virus diarrhoea virus (BVDV) in bulk tank milk as a tool in the diagnosis and prophylaxis of BVDV infections in dairy herds.

PubMed

Niskanen, R; Alenius, S; Larsson, B; Jacobsson, S O

1991-01-01

An indirect ELISA has been evaluated for determination of the level of antibodies to BVDV in individual milk samples and recently in bulk tank milk from dairy herds. As part of an epidemiological study, bulk milk and individual milk samples from all cows in 15 dairy herds were analysed for antibodies to BVDV two times one year apart. There was an excellent correlation between the level of antibodies in the bulk tank milk and the prevalence of BVDV antibody positive cows. The mean prevalence of BVDV antibody positive cows in the 15 dairy herds was 45.5% (188/413) at the first sampling and 46.2% (191/413) one year later. Seven of the herds had no, or only a low number of antibody positive cows. In contrast, between 52 to 100% of the cows in seven other herds were antibody positive to BVDV. In the 15th herd all cows without antibodies at the first sampling were antibody positive to BVDV one year later, indicating a recently introduced BVDV infection in this herd. Analysis of bulk milk samples for BVDV antibodies is now routinely used in Sweden as a tool in diagnosis and prophylaxis of BVDV infections in dairy herds. The importance and advantages of this diagnostic technique, that has made it possible to establish BVDV-free dairy herds, is discussed.

Thermal hysteresis and electrocaloric effect in Ba1-xZrxTiO3

NASA Astrophysics Data System (ADS)

Zhang, Yingtang

2018-04-01

Samples of lead-free Ba(ZrxTi1-x)O3 bulk and thick film were fabricated using solid state reaction and tape - casting technique, respectively. A comprehensive investigation of dielectric, ferroelectric, and electrocaloric properties of these samples has been carried out. The results show that there is a dielectric relaxation behavior in the thick film Meantime, the "re-entrant relaxor behavior" and thermal hysteresis are observed in the bulk. Moreover, the electrocaloric effects are observed in the thick film and the bulk. The peak values of ΔTEC of the bulk and the thick film are 2.78 K and 0.37 K, respectively. This work is beneficial for realizing high efficiency and environmentally friendly cooling technology.

Molecularly imprinted polymer microspheres prepared by Pickering emulsion polymerization for selective solid-phase extraction of eight bisphenols from human urine samples.

PubMed

Yang, Jiajia; Li, Yun; Wang, Jincheng; Sun, Xiaoli; Cao, Rong; Sun, Hao; Huang, Chaonan; Chen, Jiping

2015-05-04

The bisphenol A (BPA) imprinted polymer microspheres were prepared by simple Pickering emulsion polymerization. Compared to traditional bulk polymerization, both high yields of polymer and good control of particle sizes were achieved. The characterization results of scanning electron microscopy and nitrogen adsorption-desorption measurements showed that the obtained molecularly imprinted polymer microsphere (MIPMS) particles possessed regular spherical shape, narrow diameter distribution (30-60 μm), a specific surface area (S(BET)) of 281.26 m(2) g(-1) and a total pore volume (V(t)) of 0.459 cm(3) g(-1). Good specific adsorption capacity for BPA was obtained in the sorption experiment and good class selectivity for BPA and its seven structural analogs (bisphenol F, bisphenol B, bisphenol E, bisphenol AF, bisphenol S, bisphenol AP and bisphenol Z) was demonstrated by the chromatographic evaluation experiment. The MIPMS as solid-phase extraction (SPE) packing material was then evaluated for extraction and clean-up of these bisphenols (BPs) from human urine samples. An accurate and sensitive analytical method based on the MIPMS-SPE coupled with HPLC-DAD has been successfully established for simultaneous determination of eight BPs from human urine samples with detection limits of 1.2-2.2 ng mL(-1). The recoveries of BPs for urine samples at two spiking levels (100 and 500 ng mL(-1) for each BP) were in the range of 81.3-106.7% with RSD values below 8.3%. Copyright © 2015 Elsevier B.V. All rights reserved.

Curing kinetics and thermomechanical properties of latent epoxy/carbon fiber composites

NASA Astrophysics Data System (ADS)

Dalle Vacche, S.; Michaud, V.; Demierre, M.; Bourban, P.-E.; Månson, J.-A. E.

2016-07-01

In this work, resins based on diglycidyl ether of bisphenol A (DGEBA) epoxy and a latent hardener, dicyandiamide (DICY), as well as carbon fiber (CF) composites based on them, were prepared with three commercial accelerators: a methylene bis (phenyl dimethyl urea), a cycloaliphatic substituted urea, and a modified polyamine. The curing kinetics of the three DGEBA/DICY/accelerator systems were investigated by chemorheology and differential scanning calorimetry (DSC), in isothermal and over temperature change conditions. Differences in the reaction onset temperature, and in the glass transition temperature (Tg) were highlighted. For curing of thick resin samples, a slow curing cycle at the lowest possible temperature was used, followed by high temperature (160 - 180 °C) post-curing. Indeed, fast curing at higher temperatures caused the formation of hot spots and led to local burning of the samples. The obtained thermomechanical properties, assessed by ultimate tensile testing and dynamic mechanical analysis (DMA) in single cantilever configuration, were all in the expected range for epoxy resins, with tensile moduli close to 3 GPa and Tg > 140 °C. The longterm stability of these resins at room temperature was verified by DSC. Composite samples were prepared by hand lay-up by manually impregnating four layers of 5-harness satin CF textile, and curing in vacuum bag. Impregnation quality and void content were assessed by optical microscopy. The flexural properties of the post-cured composites were assessed by three-point bending test at room temperature and showed no relevant differences, all composites having bending moduli of 45 - 50 GPa. Finally, composites cured with a faster high temperature curing cycle (20 min at 140 °C) were prepared with the DGEBA/DICY/ methylene bis (phenyl dimethyl urea) system, obtaining similar properties as with the slower curing cycle, showing that the prepreg system allowed more flexibility in terms of curing cycle than the bulk resin samples.

Comparison of different models for predicting soil bulk density. Case study - Slovakian agricultural soils

NASA Astrophysics Data System (ADS)

Makovníková, Jarmila; Širáň, Miloš; Houšková, Beata; Pálka, Boris; Jones, Arwyn

2017-10-01

Soil bulk density is one of the main direct indicators of soil health, and is an important aspect of models for determining agroecosystem services potential. By way of applying multi-regression methods, we have created a distributed prediction of soil bulk density used subsequently for topsoil carbon stock estimation. The soil data used for this study were from the Slovakian partial monitoring system-soil database. In our work, two models of soil bulk density in an equilibrium state, with different combinations of input parameters (soil particle size distribution and soil organic carbon content in %), have been created, and subsequently validated using a data set from 15 principal sampling sites of Slovakian partial monitoring system-soil, that were different from those used to generate the bulk density equations. We have made a comparison of measured bulk density data and data calculated by the pedotransfer equations against soil bulk density calculated according to equations recommended by Joint Research Centre Sustainable Resources for Europe. The differences between measured soil bulk density and the model values vary from -0.144 to 0.135 g cm-3 in the verification data set. Furthermore, all models based on pedotransfer functions give moderately lower values. The soil bulk density model was then applied to generate a first approximation of soil bulk density map for Slovakia using texture information from 17 523 sampling sites, and was subsequently utilised for topsoil organic carbon estimation.

Advanced Microwave Ferrite Research (AMFeR): Phase Two

DTIC Science & Technology

2006-12-31

motion for the single crystal LPE films were a qualitative success, but a complete set of parameters for these films has not yet been achieved. Key...biasing field. In order to address these issues, we investigated and optimized a new LPE flux system to grow high quality thick films and bulk single...self-biased circulators. III. Methodology: BaM thick film and bulk single crystal growth by LPE process BaFe 120 19 flux melt was prepared from a

Spherical nitroguanidine process

DOEpatents

Sanchez, John A.; Roemer, Edward L.; Stretz, Lawrence A.

1990-01-01

A process of preparing spherical high bulk density nitroguanidine by dissing low bulk density nitroguanidine in N-methyl pyrrolidone at elevated temperatures and then cooling the solution to lower temperatures as a liquid characterized as a nonsolvent for the nitroguanidine is provided. The process is enhanced by inclusion in the solution of from about 1 ppm up to about 250 ppm of a metal salt such as nickel nitrate, zinc nitrate or chromium nitrate, preferably from about 20 to about 50 ppm.

Texture analysis at neutron diffractometer STRESS-SPEC

NASA Astrophysics Data System (ADS)

Brokmeier, H.-G.; Gan, W. M.; Randau, C.; Völler, M.; Rebelo-Kornmeier, J.; Hofmann, M.

2011-06-01

In response to the development of new materials and the application of materials and components in advanced technologies, non-destructive measurement methods of textures and residual stresses have gained worldwide significance in recent years. The materials science neutron diffractometer STRESS-SPEC at FRM II (Garching, Germany) is designed to be applied equally to texture and residual stress analyses by virtue of its very flexible configuration. Due to the high penetration capabilities of neutrons and the high neutron flux of STRESS-SPEC it allows a combined analysis of global texture, local texture, strain pole figure and FWHM pole figure in a wide variety of materials including metals, alloys, composites, ceramics and geological materials. Especially, the analysis of texture gradients in bulk materials using neutron diffraction has advantages over laboratory X-rays and EBSD for many scientific cases. Moreover, neutron diffraction is favourable for coarse-grained materials, where bulk information averaged over texture inhomogeneities is needed, and also stands out due to easy sample preparation. In future, the newly developed robot system for STRESS-SPEC will allow much more flexibility than an Eulerian cradle as on standard instruments. Five recent measurements are shown to demonstrate the wide range of possible texture applications at STRESS-SPEC diffractometer.

Bulk synthesis of monodisperse magnetic FeNi3 nanopowders by flow levitation method.

PubMed

Chen, Shanjun; Chen, Yan; Kang, Xiaoli; Li, Song; Tian, Yonghong; Wu, Weidong; Tang, Yongjian

2013-10-01

In this work, a novel bulk synthesis method for monodisperse FeNi3 nanoparticles was developed by flow levitation method (FL). The Fe and Ni vapours ascending from the high temperature levitated droplet was condensed by cryogenic Ar gas under atmospheric pressure. X-ray diffraction was used to identify and characterize the crystal phase of prepared powders exhibiting a FeNi3 phase. The morphology and size of nanopowders were observed by transmission electron microscopy (TEM). The chemical composition of the nanoparticles was determined with energy dispersive spectrometer (EDS). The results indicated that the FeNi3 permalloy powders are nearly spherical-shaped with diameter about 50-200 nm. Measurement of the magnetic property of nanopowders by a superconducting quantum interference device (SQUID, Quantum Design MPMS-7) showed a symmetric hysteresis loop of ferromagnetic behavior with coercivity of 220 Oe and saturation magnetization of 107.17 emu/g, at 293 K. At 5 K, the obtained saturation magnetization of the sample was 102.16 emu/g. The production rate of FeNi3 nanoparticles was estimated to be about 6 g/h. This method has great potential in mass production of FeNi3 nannoparticles.

The Role of Concentration and Solvent Character in the Molecular Organization of Humic Acids.

PubMed

Klučáková, Martina; Věžníková, Kateřina

2016-10-27

The molecular organization of humic acids in different aqueous solutions was studied over a wide concentration range (0.01-10 g·dm -3 ). Solutions of humic acids were prepared in three different media: NaOH, NaCl, and NaOH neutralized by HCl after dissolution of the humic sample. Potentiometry, conductometry, densitometry, and high resolution ultrasound spectrometry were used in order to investigate conformational changes in the humic systems. The molecular organization of humic acids in the studied systems could be divided into three concentration ranges. The rearrangements were observed at concentrations of ~0.02 g·dm -3 and ~1 g·dm -3 . The first "switch-over point" was connected with changes in the hydration shells of humic particles resulting in changes in their elasticity. The compressibility of water in the hydration shells is less than the compressibility of bulk water. The transfer of hydration water into bulk water increased the total compressibility of the solution, reducing the ultrasonic velocity. The aggregation of humic particles and the formation of rigid structures in systems with concentrations higher than 1 g·dm -3 was detected.

Characterization of Inorganic Filler Content, Mechanical Properties, and Light Transmission of Bulk-fill Resin Composites.

PubMed

Fronza, B M; Ayres, Apa; Pacheco, R R; Rueggeberg, F A; Dias, Cts; Giannini, M

The aims of this study were to characterize inorganic content (IC), light transmission (LT), biaxial flexural strength (BFS), and flexural modulus (FM) of one conventional (layered) and four bulk-fill composites at different depths. Bulk-fill composites tested were Surefil SDR flow (SDR), Filtek Bulk Fill (FBF), Tetric EvoCeram Bulk Fill (TEC), and EverX Posterior (EXP). Herculite Classic (HER) was used as a control. Energy dispersive x-ray analysis and scanning electron microscopy were used to characterize filler particle composition and morphology. The LT through different composite thicknesses (1, 2, 3, and 4 mm) was measured using a laboratory-grade spectral radiometer system (n=5). For the BFS and FM tests, sets of eight stacked composite discs (0.5-mm thick) were prepared simulating bulk filling of a 4-mm-thick increment (n=8). SDR demonstrated larger, irregular particles than those observed in TEC or HER. Filler particles in FBF were spherical, while those in EXP were composed of fiberglass strands. The LT decreased with increased composite thickness for all materials. Bulk-fill composites allowed higher LT than the HER. Furthermore, HER proved to be the unique material, having lower BFS values at deeper regions. SDR, FBF, and TEC bulk-fill composites presented reduced FM with increasing composite depth. The bulk-fill composites investigated exhibited higher LT, independent of different filler content and characteristics. Although an increase in composite thickness reduced LT, the BFS of bulk-fill composites at deeper layers was not compromised.

Differences in photoluminescence properties and thermal degradation between nanoparticle and bulk particle BaMgAl10O17:Eu2+ phosphors under UV?VUV irradiation.

PubMed

Liu, Bitao; Xin, Shuangyu; Li, Fenghua; Zhang, Jiachi; Wang, Yuhua

2014-05-01

BaMgAl10O17:Eu2+ (BAM) phosphors used for plasma display panels and three-band fluorescence lamps are exposed to an oxidizing environment at about 500 degrees C, which is currently unavoidable in actual applications. We investigated the mechanism of the luminance degradation of BAM caused by annealing at 500 degrees C based on the difference in luminance degradation of bulk particle and nanoparticle samples under various excitation source irradiations. When the samples were excited by the different light sources, more than 30% degradation of luminance occurred under 147 nm while less than 10% degradation occurred under 254 nm both for nanoparticle and bulk particle samples. In addition, the luminescence degradation of nanophosphors shows a different tendency compared to the bulk phosphors. With a model based on the particle size and excitation light penetration depth, we demonstrate that the degradation is still mainly ascribed to the oxidized of divalent Eu. The differences in luminescence properties between nanophosphors and bulk phosphors are also illustrated by this model. As a result, the potential industrial applications of nanophosphors are evaluated.

Direct and indirect measurement of the magnetocaloric effect in bulk and nanostructured Ni-Mn-In Heusler alloy

NASA Astrophysics Data System (ADS)

Ghahremani, Mohammadreza; Aslani, Amir; Hosseinnia, Marjan; Bennett, Lawrence H.; Della Torre, Edward

2018-05-01

A systematic study of the magnetocaloric effect of a Ni51Mn33.4In15.6 Heusler alloy converted to nanoparticles via high energy ball-milling technique in the temperature range of 270 to 310 K has been performed. The properties of the particles were characterized by x-ray diffraction, electron microscopy, and magnetometer techniques. Isothermal magnetic field variation of magnetization exhibits field hysteresis in bulk Ni51Mn33.4In15.6 alloy across the martensitic transition which significantly lessened in the nanoparticles. The magnetocaloric effects of the bulk and nanoparticle samples were measured both with direct method, through our state of the art direct test bed apparatus with controllability over the applied fields and temperatures, as well as an indirect method through Maxwell and thermodynamic equations. In direct measurements, nanoparticle sample's critical temperature decreased by 6 K, but its magnetocaloric effect enhanced by 17% over the bulk counterpart. Additionally, when comparing the direct and indirect magnetocaloric curves, the direct method showed 14% less adiabatic temperature change in the bulk and 5% less adiabatic temperature change in the nanostructured sample.

Method of forming crystalline silicon devices on glass

DOEpatents

McCarthy, Anthony M.

1995-01-01

A method for fabricating single-crystal silicon microelectronic components on a silicon substrate and transferring same to a glass substrate. This is achieved by utilizing conventional silicon processing techniques for fabricating components of electronic circuits and devices on bulk silicon, wherein a bulk silicon surface is prepared with epitaxial layers prior to the conventional processing. The silicon substrate is bonded to a glass substrate and the bulk silicon is removed leaving the components intact on the glass substrate surface. Subsequent standard processing completes the device and circuit manufacturing. This invention is useful in applications requiring a transparent or insulating substrate, particularly for display manufacturing. Other applications include sensors, actuators, optoelectronics, radiation hard electronics, and high temperature electronics.

Core vs. Bulk Samples in Soil-Moisture Tension Analyses

Treesearch

Walter M. Broadfoot

1954-01-01

The usual laboratory procedure in determining soil-moisture tension values is to use "undisturbed" soil cores for tensions up to 60 cm. of water and bulk soil samples for higher tensions. Low tensions are usually obtained with a tension table and the higher tensions by use of pressure plate apparatus. In tension analysis at the Vicksburg Infiltration Project...

40 CFR 761.295 - Reporting and recordkeeping of the PCB concentrations in samples.

Code of Federal Regulations, 2013 CFR

2013-07-01

... concentrations in samples. 761.295 Section 761.295 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY... On-Site Disposal of Bulk PCB Remediation Waste and Porous Surfaces in Accordance With § 761.61(a)(6... concentrations for bulk PCB remediation waste and porous surfaces on a dry weight basis and as micrograms of PCBs...

40 CFR 761.295 - Reporting and recordkeeping of the PCB concentrations in samples.

Code of Federal Regulations, 2014 CFR

2014-07-01

... concentrations in samples. 761.295 Section 761.295 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY... On-Site Disposal of Bulk PCB Remediation Waste and Porous Surfaces in Accordance With § 761.61(a)(6... concentrations for bulk PCB remediation waste and porous surfaces on a dry weight basis and as micrograms of PCBs...

40 CFR 761.295 - Reporting and recordkeeping of the PCB concentrations in samples.

Code of Federal Regulations, 2011 CFR

2011-07-01

... concentrations in samples. 761.295 Section 761.295 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY... On-Site Disposal of Bulk PCB Remediation Waste and Porous Surfaces in Accordance With § 761.61(a)(6... concentrations for bulk PCB remediation waste and porous surfaces on a dry weight basis and as micrograms of PCBs...

40 CFR 761.295 - Reporting and recordkeeping of the PCB concentrations in samples.

Code of Federal Regulations, 2012 CFR

2012-07-01

... concentrations in samples. 761.295 Section 761.295 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY... On-Site Disposal of Bulk PCB Remediation Waste and Porous Surfaces in Accordance With § 761.61(a)(6... concentrations for bulk PCB remediation waste and porous surfaces on a dry weight basis and as micrograms of PCBs...

40 CFR 761.347 - First level sampling-waste from existing piles.

Code of Federal Regulations, 2010 CFR

2010-07-01

... Purposes of Characterization for PCB Disposal in Accordance With § 761.62, and Sampling PCB Remediation... a cone; that is, having a circular base with PCB bulk product waste or PCB remediation waste... one pile. If the PCB bulk product waste or PCB remediation waste consists of more than one pile or...

Rapid Assessment of the Ce-Co-Fe-Cu System for Permanent Magnetic Applications

DOE PAGES

Meng, F.; Chaudhary, R. P.; Gandha, K.; ...

2018-04-23

Here, this work focuses on the rapid synthesis and characterization of quaternary Ce(CoFeCu) 5 alloy libraries to assess their potential viability as permanent magnets. Arrays of bulk specimens with controlled compositions were synthesized via laser engineered net shaping (LENS) by feeding different ratios of alloy powders into a melt pool created by a laser. Based on the assessment of the magnetic properties of the LENS printed samples, arc-melted and cast ingots were prepared with varying Fe (5–20 at.%) and Co (60–45 at.%) compositions while maintaining constant Ce (16 at.%) and Cu (19 at.%) content. The evolution of the microstructure andmore » phases with varying chemical compositions and their dependence on magnetic properties are analyzed in as-cast and heat-treated samples. In both the LENS printed and cast samples, we find the best magnetic properties correspond to a predominantly single-phase Ce(CoFeCu) 5 microstructure in which high coercivity ( H c > 10 kOe) can be achieved without any microstructural refinement.« less

Rapid Assessment of the Ce-Co-Fe-Cu System for Permanent Magnetic Applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Meng, F.; Chaudhary, R. P.; Gandha, K.

Here, this work focuses on the rapid synthesis and characterization of quaternary Ce(CoFeCu) 5 alloy libraries to assess their potential viability as permanent magnets. Arrays of bulk specimens with controlled compositions were synthesized via laser engineered net shaping (LENS) by feeding different ratios of alloy powders into a melt pool created by a laser. Based on the assessment of the magnetic properties of the LENS printed samples, arc-melted and cast ingots were prepared with varying Fe (5–20 at.%) and Co (60–45 at.%) compositions while maintaining constant Ce (16 at.%) and Cu (19 at.%) content. The evolution of the microstructure andmore » phases with varying chemical compositions and their dependence on magnetic properties are analyzed in as-cast and heat-treated samples. In both the LENS printed and cast samples, we find the best magnetic properties correspond to a predominantly single-phase Ce(CoFeCu) 5 microstructure in which high coercivity ( H c > 10 kOe) can be achieved without any microstructural refinement.« less

Pharmacokinetics Evaluation of Carbon Nanotubes Using FTIR Analysis and Histological Analysis.

PubMed

Gherman, Claudia; Tudor, Matea Cristian; Constantin, Bele; Flaviu, Tabaran; Stefan, Razvan; Maria, Bindea; Chira, Sergiu; Braicu, Cornelia; Pop, Laura; Petric, Roxana Cojocneanu; Berindan-Neagoe, Ioana

2015-04-01

Carbon nanotubes (CNTs) are biologically non-toxic and long-circulating nanostructures that have special physical properties. This study was focused on developing alternative methods that track carbon nanotubes, like FR-IR to classical tissue histological procedure. FT-IR absorption spectra were used to confirm the carboxylation of carbon nanotubes and to evaluate the presence of carbon nanotubes from bulk spleen samples and histologically prepared samples (control spleen and spleen with SWCNT-COOH). FT-IR spectrum of spleen sample from animals injected with CNTs shows major spectral differences consisting in infrared bands located at ~1173 cm(-1), ~ 1410 cm(-1); ~1658 cm(-1), ~1737 cm(-1) and around 1720 cm(-1) respectively. In terms of localization of carbon nanotubes, selective accumulation of marginal zone macrophages and splenic red pulp is observed for all treated groups, indicating the presence of carbon nanotubes even at 3, 4 and 7 days after treatment. In summary, we believe that histological evaluation and FT-IR can provide more characteristic information about the pharmacokinetcis and the clearance of carbon nanotubes.

Variations in the Infrared Spectra of Wüstite with Defects and Disorder

NASA Astrophysics Data System (ADS)

Koike, C.; Matsuno, J.; Chihara, H.

2017-08-01

The presence of FeO particles in circumstellar space has been suggested based on the observation of a mysterious 21 μm emission band. However, the complete infrared spectra of FeO have not been obtained so far; hence, data of the infrared (IR) spectra of FeO need to be investigated. We prepared synthetic and commercial samples of FeO, which were obtained by crushing bulk samples, annealing iron oxalate dihydrate ({{FeC}}2{{{O}}}4\\cdot 2{{{H}}}2{{O}}), and mechanical milling of a powder mixture comprising (Fe and {{Fe}}2{{{O}}}3) particles with different milling times. We present a new study on the IR spectra of these samples, and show that these spectra changed according to defects and disorders. Furthermore, FeO particles are very sensitive to oxygen fugacity and temperature. The spectra of FeO particles were compared with the unidentified observed feature. It may be difficult for FeO particles to exist alone in the ISM and circumstellar space. This may be connected to the problem of missing iron in the ISM.

X-ray diffraction, Raman, and photoacoustic studies of ZnTe nanocrystals

NASA Astrophysics Data System (ADS)

Ersching, K.; Campos, C. E. M.; de Lima, J. C.; Grandi, T. A.; Souza, S. M.; da Silva, D. L.; Pizani, P. S.

2009-06-01

Nanocrystalline ZnTe was prepared by mechanical alloying. X-ray diffraction (XRD), energy dispersive spectroscopy, Raman spectroscopy, and photoacoustic absorption spectroscopy techniques were used to study the structural, chemical, optical, and thermal properties of the as-milled powder. An annealing of the mechanical alloyed sample at 590 °C for 6 h was done to investigate the optical properties in a defect-free sample (close to bulk form). The main crystalline phase formed was the zinc-blende ZnTe, but residual trigonal tellurium and hexagonal ZnO phases were also observed for both as-milled and annealed samples. The structural parameters, phase fractions, average crystallite sizes, and microstrains of all crystalline phases were obtained from Rietveld analyses of the X-ray patterns. Raman results corroborate the XRD results, showing the longitudinal optical phonons of ZnTe (even at third order) and those modes of trigonal Te. Nonradiative surface recombination and thermal bending heat transfer mechanisms were proposed from photoacoustic analysis. An increase in effective thermal diffusivity coefficient was observed after annealing and the carrier diffusion coefficient, the surface recombination velocity, and the recombination time parameters remained the same.

The effect of storage temperature and duration on the microbial quality of bulk tank milk.

PubMed

O'Connell, A; Ruegg, P L; Jordan, K; O'Brien, B; Gleeson, D

2016-05-01

The dairy industry in Ireland is currently undergoing a period of expansion and, as a result, it is anticipated that milk may be stored in bulk tanks on-farm for periods greater than 48 h. The objective of this study was to investigate the effects of storage temperature and duration on microbial quality of bulk tank milk when fresh milk is added to the bulk tank twice daily. Bulk tank milk stored at 3 temperatures was sampled at 24-h intervals during storage periods of 0 to 96 h. Bulk tank milk samples were analyzed for total bacterial count (TBC), psychrotrophic bacterial count (PBC), laboratory pasteurization count (LPC), psychrotrophic-thermoduric bacterial count (PBC-LPC), proteolytic bacterial count, lipolytic bacterial count, presumptive Bacillus cereus, sulfite-reducing Clostridia (SRC), and SCC. The bulk tank milk temperature was set at each of 3 temperatures (2°C, 4°C, and 6°C) in each of 3 tanks on 2 occasions during two 6-wk periods. Period 1 was undertaken in August and September, when all cows were in mid lactation, and period 2 was undertaken in October and November, when all cows were in late lactation. None of the bulk tank bacterial counts except the proteolytic count were affected by lactation period. The proteolytic bacterial count was greater in period 2 than in period 1. The TBC and PBC of milk stored at 6°C increased as storage duration increased. The TBC did not increase with increasing storage duration when milk was stored at 2°C or 4°C but the PBC of milk stored at 4°C increased significantly between 0 and 96 h. The numbers of proteolytic and lipolytic bacteria, LPC, or PBC-LPC in bulk tank milk were not affected by temperature or duration of storage. Presumptive B. cereus were detected in 10% of all bulk tank milk samples taken over the two 6-wk periods, with similar proportions observed in both. In bulk tank milk samples, a greater incidence of SRC was observed in period 2 (20%) compared with period 1 (3%). Milk produced on-farm with minimal bacterial contamination can be successfully stored at 2°C and 4°C for up to 96h with little effect on its microbial quality. Copyright © 2016 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Recent developments on field gas extraction and sample preparation methods for radiokrypton dating of groundwater

NASA Astrophysics Data System (ADS)

Yokochi, Reika

2016-09-01

Current and foreseen population growths will lead to an increased demand in freshwater, large quantities of which is stored as groundwater. The ventilation age is crucial to the assessment of groundwater resources, complementing the hydrological model approach based on hydrogeological parameters. Ultra-trace radioactive isotopes of Kr (81 Kr and 85 Kr) possess the ideal physical and chemical properties for groundwater dating. The recent advent of atom trap trace analyses (ATTA) has enabled determination of ultra-trace noble gas radioisotope abundances using 5-10 μ L of pure Kr. Anticipated developments will enable ATTA to analyze radiokrypton isotope abundances at high sample throughput, which necessitates simple and efficient sample preparation techniques that are adaptable to various sample chemistries. Recent developments of field gas extraction devices and simple and rapid Kr separation method at the University of Chicago are presented herein. Two field gas extraction devices optimized for different sampling conditions were recently designed and constructed, aiming at operational simplicity and portability. A newly developed Kr purification system enriches Kr by flowing a sample gas through a moderately cooled (138 K) activated charcoal column, followed by a gentle fractionating desorption. This simple process uses a single adsorbent and separates 99% of the bulk atmospheric gases from Kr without significant loss. The subsequent two stages of gas chromatographic separation and a hot Ti sponge getter further purify the Kr-enriched gas. Abundant CH4 necessitates multiple passages through one of the gas chromatographic separation columns. The presented Kr separation system has a demonstrated capability of extracting Kr with > 90% yield and 99% purity within 75 min from 1.2 to 26.8 L STP of atmospheric air with various concentrations of CH4. The apparatuses have successfully been deployed for sampling in the field and purification of groundwater samples.

Monitoring the bulk milk antibody response to bovine viral diarrhea in dairy herds vaccinated with inactivated vaccines.

PubMed

Gonzalez, A M; Arnaiz, I; Eiras, C; Camino, F; Sanjuán, M L; Yus, E; Diéguez, F J

2014-01-01

This study was designed to determine long-term responses in dairy herds after vaccination with 1 of 3 inactivated bovine viral diarrhea virus (BVDV) vaccines with regard to antibodies against p80 protein in bulk tank milk samples, as detected by ELISA. In the present study, 29 dairy herds were vaccinated with Bovilis BVD (MSD Animal Health, Milton Keynes, UK), 11 with Hiprabovis Balance (Laboratorios Hipra, Amer, Spain), and 9 with Pregsure BVD (Zoetis, Florham Park, NJ). In these herds, bulk tank milk samples were collected and examined at the time of the first vaccination and every 6 mo during a 3-yr period. Samples were analyzed with a commercial ELISA test for the p80 protein of BVDV. The results demonstrated that vaccination affected the level of antibodies against p80. Hence, vaccination status should be taken into consideration when interpreting bulk tank milk antibody tests. Copyright © 2014 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Total and non-seasalt sulfate and chloride measured in bulk precipitation samples from the Kilauea Volcano area, Hawaii

USGS Publications Warehouse

Scholl, M.A.; Ingebritsen, S.E.

1995-01-01

Six-month cumulative precipitation samples provide estimates of bulk deposition of sulfate and chloride for the southeast part of the Island of Hawaii during four time periods: August 1991 to February 1992, February 1992 to September 1992, March 1993 to September 1993, and September 1993 to February 1994. Total estimated bulk deposition rates for sulfate ranged from 0.12 to 24 grams per square meter per 180 days, and non-seasalt sulfate deposition ranged from 0.06 to 24 grams per square meter per 180 days. Patterns of non-seasalt sulfate deposition were generally related to prevailing wind directions and the proximity of the collection site to large sources of sulfur gases, namely Kilauea Volcano's summit and East Rift Zone eruption. Total chloride deposition from bulk precipitation samples ranged from 0.01 to 17 grams per square meter per 180 days. Chloride appeared to be predominantly from oceanic sources, as non- seasalt chloride deposition was near zero for most sites.

Disorder-induced transition from grain boundary to bulk dominated ionic diffusion in pyrochlores

DOE PAGES

Perriot, Romain; Dholabhai, Pratik P.; Uberuaga, Blas P.

2017-05-04

In this paper, we use molecular dynamics simulations to investigate the role of grain boundaries (GBs) on ionic diffusion in pyrochlores, as a function of the GB type, chemistry of the compound, and level of cation disorder. We observe that the presence of GBs promotes oxygen transport in ordered and low-disordered systems, as the GBs are found to have a higher concentration of mobile carriers with higher mobilities than in the bulk. Thus, in ordered samples, the ionic diffusion is 2D, localized along the grain boundary. When cation disorder is introduced, bulk carriers begin to contribute to the overall diffusion,more » while the GB contribution is only slightly enhanced. In highly disordered samples, the diffusive behavior at the GBs is bulk-like, and the two contributions (bulk vs. GB) can no longer be distinguished. There is thus a transition from 2D/GB dominated oxygen diffusivity to 3D/bulk dominated diffusivity versus disorder in pyrochlores. Finally, these results provide new insights into the possibility of using internal interfaces to enhance ionic conductivity in nanostructured complex oxides.« less

The thermoelectric properties of bulk crystalline n- and p-type Mg2Si prepared by the vertical Bridgman method

NASA Astrophysics Data System (ADS)

Akasaka, Masayasu; Iida, Tsutomu; Matsumoto, Atsunobu; Yamanaka, Kohei; Takanashi, Yoshifumi; Imai, Tomohiro; Hamada, Noriaki

2008-07-01

Bulk Mg2Si crystals were grown using the vertical Bridgman melt growth method. The n-type and p-type dopants, bismuth (Bi) and silver (Ag), respectively, were incorporated during the growth. X-ray powder diffraction analysis revealed clear peaks of Mg2Si with no peaks associated with the metallic Mg and Si phases. Residual impurities and process induced contaminants were investigated by using glow discharge mass spectrometry (GDMS). A comparison between the results of GDMS and Hall effect measurements indicated that electrical activation of the Bi doping in the Mg2Si was sufficient, while activation of the Ag doping was relatively smaller. It was shown that an undoped n-type specimen contained a certain amount of aluminum (Al), which was due either to residual impurities in the Mg source or the incorporation of process-induced impurities. Thermoelectric properties such as the Seebeck coefficient and the electrical and thermal conductivities were measured as a function of temperature up to 850 K. The dimensionless figures of merit for Bi-doped and Ag-doped samples were 0.65 at 840 K and 0.1 at 566 K, respectively. Temperature dependence of the observed Seebeck coefficient was fitted well by the two-carrier model. The first-principles calculations were carried out by using the all-electron band-structure calculation package (ABCAP) in which the full-potential linearized augmented-plane-wave method was employed. The ABCAP calculation adequately presents characteristics of the Seebeck coefficients for the undoped and heavily Bi-doped samples over the whole measured temperature range from room temperature to 850 K. The agreement between the theory and the experiment is poorer for the Ag-doped p-type samples.

A protected annealing strategy to enhanced light emission and photostability of YAG:Ce nanoparticle-based films

NASA Astrophysics Data System (ADS)

Revaux, Amelie; Dantelle, Geraldine; George, Nathan; Seshadri, Ram; Gacoin, Thierry; Boilot, Jean-Pierre

2011-05-01

A significant obstacle in the development of YAG:Ce nanoparticles as light converters in white LEDs and as biological labels is associated with the difficulty of finding preparative conditions that allow simultaneous control of structure, particle size and size distribution, while maintaining the optical properties of bulk samples. Preparation conditions frequently involve high-temperature treatments of precursors (up to 1400 °C), which result in increased particle size and aggregation, and lead to oxidation of Ce(iii) to Ce(iv). We report here a process that we term protected annealing, that allows the thermal treatment of preformed precursor particles at temperatures up to 1000 °C while preserving their small size and state of dispersion. In a first step, pristine nanoparticles are prepared by a glycothermal reaction, leading to a mixture of YAG and boehmite crystalline phases. The preformed nanoparticles are then dispersed in a porous silica. Annealing of the composite material at 1000 °C is followed by dissolution of the amorphous silica by hydrofluoric acid to recover the annealed particles as a colloidal dispersion. This simple process allows completion of YAG crystallization while preserving their small size. The redox state of Ce ions can be controlled through the annealing atmosphere. The obtained particles of YAG:Ce (60 +/- 10 nm in size) can be dispersed as nearly transparent aqueous suspensions, with a luminescence quantum yield of 60%. Transparent YAG:Ce nanoparticle-based films of micron thickness can be deposited on glass substrates using aerosol spraying. Films formed from particles prepared by the protected annealing strategy display significantly improved photostability over particles that have not been subject to such annealing.A significant obstacle in the development of YAG:Ce nanoparticles as light converters in white LEDs and as biological labels is associated with the difficulty of finding preparative conditions that allow simultaneous control of structure, particle size and size distribution, while maintaining the optical properties of bulk samples. Preparation conditions frequently involve high-temperature treatments of precursors (up to 1400 °C), which result in increased particle size and aggregation, and lead to oxidation of Ce(iii) to Ce(iv). We report here a process that we term protected annealing, that allows the thermal treatment of preformed precursor particles at temperatures up to 1000 °C while preserving their small size and state of dispersion. In a first step, pristine nanoparticles are prepared by a glycothermal reaction, leading to a mixture of YAG and boehmite crystalline phases. The preformed nanoparticles are then dispersed in a porous silica. Annealing of the composite material at 1000 °C is followed by dissolution of the amorphous silica by hydrofluoric acid to recover the annealed particles as a colloidal dispersion. This simple process allows completion of YAG crystallization while preserving their small size. The redox state of Ce ions can be controlled through the annealing atmosphere. The obtained particles of YAG:Ce (60 +/- 10 nm in size) can be dispersed as nearly transparent aqueous suspensions, with a luminescence quantum yield of 60%. Transparent YAG:Ce nanoparticle-based films of micron thickness can be deposited on glass substrates using aerosol spraying. Films formed from particles prepared by the protected annealing strategy display significantly improved photostability over particles that have not been subject to such annealing. Electronic supplementary information (ESI) available: Thermogravimetric analysis curve, picture of a YAG:Ce3+ thin film. See DOI: 10.1039/c0nr01000f

Quantitative analysis of thoria phase in Th-U alloys using diffraction studies

NASA Astrophysics Data System (ADS)

Thakur, Shital; Krishna, P. S. R.; Shinde, A. B.; Kumar, Raj; Roy, S. B.

2017-05-01

In the present study the quantitative phase analysis of Th-U alloys in bulk form namely Th-52 wt% U and Th-3wt%U has been performed over the data obtained from both X ray diffraction and neutron diffraction technique using Rietveld method of FULLPROF software. Quantifying thoria (ThO2) phase present in bulk of the sample is limited due to surface oxidation and low penetration of x rays in high Z material. Neutron diffraction study probing bulk of the samples has been presented in comparison with x-ray diffraction study.

A Survey on Aflatoxin M1 Content in Sheep and Goat Milk Produced in Sardinia Region, Italy (2005-2013).

PubMed

Virdis, Salvatore; Scarano, Christian; Spanu, Vincenzo; Murittu, Gavino; Spanu, Carlo; Ibba, Ignazio; De Santis, Enrico Pietro Luigi

2014-12-09

In the present work the results of a survey conducted in Sardinia Region on Aflatoxin M 1 (AFM 1 ) contamination in milk of small ruminants from 2005 to 2013 are reported. A total of 517 sheep and 88 goat milk samples from bulk tank, tank trucks and silo tank milk were collected. Analyses were performed by the Regional Farmers Association laboratory using high-performance liquid chromatography following the ISO 14501:1998 standard. None of the sheep milk samples analysed during 2005-2012 showed AFM 1 contamination. In sheep milk samples collected in 2013, 8 out of 172 (4.6%) were contaminated by AFM 1 with a concentration (mean±SD) of 12.59±14.05 ng/L. In one bulk tank milk sample 58.82 ng/L AFM 1 was detected, exceeding the EU limit. In none of goat milk samples analysed from 2010 to 2012 AFM 1 was detected. In 2013, 9 out of 66 goat milk samples (13.6%) showed an AFM 1 concentration of 47.21±19.58 ng/L. Two of these samples exceeded the EU limit, with concentrations of 62.09 and 138.6 ng/L. Higher contamination frequency and concentration rates were detected in bulk tank milk samples collected at farm than in bulk milk truck or silo samples, showing a dilution effect on AFM 1 milk content along small ruminants supply chain. The rate and levels of AFM 1 contamination in sheep and goat milk samples were lower than other countries. However, the small number of milk samples analysed for AFM 1 in Sardinia Region in 2005-2013 give evidence that food business operators check programmes should be improved to ensure an adequate monitoring of AFM 1 contamination in small ruminant dairy chain.

Constipation and catharsis.

PubMed Central

Thompson, W. G.

1976-01-01

Constipation is endemic in the Western world. Stool consistence and associated symptoms are more important than stool frequency. The patient's attitude towards his bowel habit is also important. Exclusion of "organic" disease, reassurance and discussion of normal variations of bowel habit are necessary first steps in treatment. Adquate bulk in the stool must be ensured, either through diet or bulking agnets, and bowel retraining attempted. Laxatives should be reserved for episodes of constipation following enforced bedrest, or as a preparation for diagnostic procedures. Long-term use should be avoided. PMID:1268778

Interaction of Polarized Light with Chalcogenide Glasses

DTIC Science & Technology

2001-06-01

simultaneous measurement of the laser radiation transmitted through the bulk sample and radiation scattered by the sample to various angles up to 230...fixed in the central part of the lens, reflected the transmitted light beam to a second photodiode. He-Ne laser radiation (), = 633 nm) which was sub...band-gap radiation for the studied bulk glass samples (As 2S3 glass) played in this installation, by turns, a role of inducing or probing light. This

Molecularly imprinted solid-phase extraction combined with high performance liquid chromatography for analysis of phenolic compounds from environmental water samples.

PubMed

Feng, Qin-Zhong; Zhao, Li-Xia; Yan, Wei; Lin, Jin-Ming; Zheng, Zhi-Xia

2009-08-15

The molecularly imprinted bulk polymer with 2,4,6-trichlorophenol (2,4,6-TCP) as the template molecule and methylacrylic acid (MAA), ethylene glycol dimethacrylate (EGDMA) as functional monomer and the crosslinker, respectively, has been prepared and applied to the molecularly imprinted solid-phase extraction (MISPE) procedure for selective preconcentration of phenolic compounds from environmental water samples. Various parameters affecting the extraction efficiency of the polymer have been evaluated to optimize the selective preconcentration of the phenolic compounds from aqueous samples. The characteristics of the MISPE method were validated by HPLC. The recoveries ranged between 90% and 98% (RSD: 0.9-2.3%, n=3) for tap water, between 85% and 105% (RSD: 2.6-4.9%, n=3) for river water, between 78% and 98% (RSD: 2.6-5.4%, n=3) for sewage water fortified with 0.4 mg L(-1) of phenol, 4-chlorophenol (4-CP), 2,4-dichlorophenol (2,4-DCP), pentachlorophenol (PCP). It was demonstrated that this MISPE-HPLC method could be applied to direct preconcentration and determination of phenolic compounds in environmental water samples.

The Use of Isotope Dilution Alpha Spectrometry and Liquid Scintillation Counting to Determine Radionuclides in Environmental Samples (abstract)

NASA Astrophysics Data System (ADS)

Bylyku, Elida

2009-04-01

In Albania in recent years it has been of increasing interest to determine various pollutants in the environment and their possible effects on human health. The radiochemical procedure used to identify Pu, Am, U, Th, and Sr radioisotopes in soil, sediment, water, coal, and milk samples is described. The analysis is carried out in the presence of respective tracer solutions and combines the procedure for Pu analysis based on anion exchange, the selective method for Sr isolation based on extraction chromatography using Sr-Spec resin, and the application of the TRU-Spec column for separation of Am fraction. An acid digestion method has been applied for the decomposition of samples. The radiochemical procedure involves the separation of Pu from Th, Am, and Sr by anion exchange, followed by the preconcentration of Am and Sr by coprecipitation with calcium oxalate. Am is separated from Sr by extraction chromatography. Uranium is separated from the bulk elements by liquid-liquid extraction using UTEVA® resin. Thin sources for alpha spectrometric measurements are prepared by microprecipitation with NdF3. Two International Atomic Energy Agency reference materials were analyzed in parallel with the samples.

Phase transitions of amorphous solid acetone in confined geometry investigated by reflection absorption infrared spectroscopy.

PubMed

Shin, Sunghwan; Kang, Hani; Kim, Jun Soo; Kang, Heon

2014-11-26

We investigated the phase transformations of amorphous solid acetone under confined geometry by preparing acetone films trapped in amorphous solid water (ASW) or CCl4. Reflection absorption infrared spectroscopy (RAIRS) and temperature-programmed desorption (TPD) were used to monitor the phase changes of the acetone sample with increasing temperature. An acetone film trapped in ASW shows an abrupt change in the RAIRS features of the acetone vibrational bands during heating from 80 to 100 K, which indicates the transformation of amorphous solid acetone to a molecularly aligned crystalline phase. Further heating of the sample to 140 K produces an isotropic solid phase, and eventually a fluid phase near 157 K, at which the acetone sample is probably trapped in a pressurized, superheated condition inside the ASW matrix. Inside a CCl4 matrix, amorphous solid acetone crystallizes into a different, isotropic structure at ca. 90 K. We propose that the molecularly aligned crystalline phase formed in ASW is created by heterogeneous nucleation at the acetone-water interface, with resultant crystal growth, whereas the isotropic crystalline phase in CCl4 is formed by homogeneous crystal growth starting from the bulk region of the acetone sample.

Novel sampling methods for atmospheric semi-volatile organic compounds (SOCs) in a high altitude alpine environment.

PubMed

Offenthaler, I; Jakobi, G; Kaiser, A; Kirchner, M; Kräuchi, N; Niedermoser, B; Schramm, K-W; Sedivy, I; Staudinger, M; Thanner, G; Weiss, P; Moche, W

2009-12-01

High- and low-volume active air samplers as well as bulk deposition samplers were developed to sample atmospheric SOCs under the adverse conditions of a mountain environment. Active sampling employed separate filters for different European source regions. Filters were switched depending on daily trajectory forecasts, whose accuracy was evaluated post hoc. The sampling continued on three alpine summits over five periods of four months. The prevailing trajectories varied stronger between sampling periods than between stations. The sampling equipment (active and bulk deposition) proved dependable for operation in a mountain environment, with idle times being mainly due to non-routine manipulations and connectivity.

Preparing to Teach Newcomer Students: The Significance of Critical Pedagogy and the Study of Ideology in Teacher Education

ERIC Educational Resources Information Center

Bartolome, Lilia I.

2010-01-01

In recent decades, the number of school-aged linguistic-minority students in the United States has increased dramatically. Society at large and public schools in particular must be prepared to respond to these students' needs. In public education, the bulk of this responsibility falls on teachers, who are called upon to apply educational policies…

Controlling the crystalline three-dimensional order in bulk materials by single-wall carbon nanotubes.

PubMed

López-Andarias, Javier; López, Juan Luis; Atienza, Carmen; Brunetti, Fulvio G; Romero-Nieto, Carlos; Guldi, Dirk M; Martín, Nazario

2014-04-29

The construction of ordered single-wall carbon nanotube soft-materials at the nanoscale is currently an important challenge in science. Here we use single-wall carbon nanotubes as a tool to gain control over the crystalline ordering of three-dimensional bulk materials composed of suitably functionalized molecular building blocks. We prepare p-type nanofibres from tripeptide and pentapeptide-containing small molecules, which are covalently connected to both carboxylic and electron-donating 9,10-di(1,3-dithiol-2-ylidene)-9,10-dihydroanthracene termini. Adding small amounts of single-wall carbon nanotubes to the so-prepared p-nanofibres together with the externally controlled self assembly by charge screening by means of Ca(2+) results in new and stable single-wall carbon nanotube-based supramolecular gels featuring remarkably long-range internal order.

Bulk heterojunction perovskite solar cells based on room temperature deposited hole-blocking layer: Suppressed hysteresis and flexible photovoltaic application

NASA Astrophysics Data System (ADS)

Chen, Zhiliang; Yang, Guang; Zheng, Xiaolu; Lei, Hongwei; Chen, Cong; Ma, Junjie; Wang, Hao; Fang, Guojia

2017-05-01

Perovskite solar cells have developed rapidly in recent years as the third generation solar cells. In spite of the great improvement achieved, there still exist some issues such as undesired hysteresis and indispensable high temperature process. In this work, bulk heterojunction perovskite-phenyl-C61-butyric acid methyl ester solar cells have been prepared to diminish hysteresis using a facile two step spin-coating method. Furthermore, high quality tin oxide films are fabricated using pulse laser deposition technique at room temperature without any annealing procedure. The as fabricated tin oxide film is successfully applied in bulk heterojunction perovskite solar cells as a hole blocking layer. Bulk heterojunction devices based on room temperature tin oxide exhibit almost hysteresis-free characteristics with power conversion efficiency of 17.29% and 14.0% on rigid and flexible substrates, respectively.

The force required to fracture endodontically roots restored with various materials as intra-orifice barriers.

PubMed

Yasa, E; Arslan, H; Yasa, B; Akcay, M; Alsancak, M; Hatirli, H

2017-10-01

To evaluate the effect of various materials as intra-orifice barriers on the force required fracture roots. One hundred-thirty five mandibular premolars were decoronated and prepared up to size #40. The root canals were filled and randomly divided into two control and seven experimental groups (n = 15), as follows: Positive control group (the intra-orifice barrier cavity was not prepared), negative control group (the intra-orifice barrier cavity was prepared, but not filled), filling using glass ionomer cement, nano-hybrid composite resin, short fiber-reinforced composite, bulk-fill flowable composite, MTA Angelus, Micro Mega MTA or Biodentine. A fracture strength test was performed, and the data were analyzed using one-way ANOVA and Tukey's post hoc tests. Nano-hybrid composite, short fiber-reinforced composite, bulk-fill flow able composite, and glass ionomer cement increased the force required fracture the roots compared to the positive and negative control groups (P < 0.05). While MTA groups did not increase the force required fracture the roots compared to the control groups, Biodentine increased significantly. Within the limitations of the present study, the use of nano-hybrid composite, short fiber-reinforced composite, bulk-fill flowable composite, and glass ionomer cement as an intra-orifice barrier may be useful in reinforcing roots. MTA placement (MTA Angelus or Micro Mega MTA) did not significantly increase the fracture resistance of endodontically treated roots compared to the control groups, however Biodentine did.

Using the Opposition Effect in Remotely Sensed Data to Assist in the Retrieval of Bulk Density

NASA Astrophysics Data System (ADS)

Ambeau, Brittany L.

Bulk density is an important geophysical property that impacts the mobility of military vehicles and personnel. Accurate retrieval of bulk density from remotely sensed data is, therefore, needed to estimate the mobility on "off-road" terrain. For a particulate surface, the functional form of the opposition effect can provide valuable information about composition and structure. In this research, we examine the relationship between bulk density and angular width of the opposition effect for a controlled set of laboratory experiments. Given a sample with a known bulk density, we collect reflectance measurements on a spherical grid for various illumination and view geometries -- increasing the amount of reflectance measurements collected at small phase angles near the opposition direction. Bulk densities are varied using a custom-made pluviation device, samples are measured using the Goniometer of the Rochester Institute of Technology-Two (GRIT-T), and observations are fit to the Hapke model using a grid-search method. The method that is selected allows for the direct estimation of five parameters: the single-scattering albedo, the amplitude of the opposition effect, the angular width of the opposition effect, and the two parameters that describe the single-particle phase function. As a test of the Hapke model, the retrieved bulk densities are compared to the known bulk densities. Results show that with an increase in the availability of multi-angular reflectance measurements, the prospects for retrieving the spatial distribution of bulk density from satellite and airborne sensors are imminent.

Enhanced hydrogen generation by hydrolysis of Mg doped with flower-like MoS2 for fuel cell applications

NASA Astrophysics Data System (ADS)

Huang, Minghong; Ouyang, Liuzhang; Liu, Jiangwen; Wang, Hui; Shao, Huaiyu; Zhu, Min

2017-10-01

In this work, flower-like MoS2 spheres are synthesized via a hydrothermal method and the catalytic activity of the as-prepared and bulk MoS2 on hydrolysis of Mg is systematically investigated for the first time. The Mg-MoS2 composites are prepared by ball milling and the hydrogen generation performances of the composites are investigated in 3.5% NaCl solution. The experimental results suggest that the as-prepared MoS2 exhibits better catalytic effect on hydrolysis of Mg compared to bulk MoS2. In particular, Mg-10 wt% MoS2 (as-prepared) composite milled for 1 h shows the best hydrogen generation properties and releases 90.4% of theoretical hydrogen generation capacity within 1 min at room temperature. The excellent catalytic effect of as-prepared MoS2 may be attributed to the following aspects: three-dimensional flower-like MoS2 architectures improve its dispersibility on Mg particles; make the composite more reactive; hamper the generated Mg(OH)2 from adhering to the surface of Mg; and increase the galvanic corrosion of Mg. In addition, a hydrogen generator based on the hydrolysis reaction of Mg-0.2 wt% MoS2 composite is manufactured and it can supply a maximum hydrogen flow rate of 2.5 L/min. The findings here demonstrate the as-prepared flower-like MoS2 can be a promising catalyst for hydrogen generation from Mg.

Effect of bulk-fill base material on fracture strength of root-filled teeth restored with laminate resin composite restorations.

PubMed

Taha, N A; Maghaireh, G A; Ghannam, A S; Palamara, J E

2017-08-01

To evaluate the effect of using a bulk-fill flowable base material on fracture strength and fracture patterns of root-filled maxillary premolars with MOD preparations restored with laminate restorations. Fifty extracted maxillary premolars were selected for the study. Standardized MOD cavities with endodontic treatment were prepared for all teeth, except for intact control. The teeth were divided randomly into five groups (n=10); (Group 1) sound teeth, (Group 2) unrestored teeth; (Group 3) MOD cavities with Vitrebond base and resin-based composite (Ceram. X One Universal); (Group 4) MOD cavities with 2mm GIC base (Fuji IX GP) and resin-based composite (Ceram. X One Universal) open laminate, (Group 5) MOD cavities were restored with 4mm of bulk-fill flowable base material (SDR) and resin-based composite (Ceram. X One Universal). All teeth were thermocycled and subjected to a 45° ramped oblique load in a universal testing machine. Fracture load and fracture patterns were recorded. Data were analyzed using one-way ANOVA and Dunnett's T3 test. Restoration in general increased the fracture strength compared to unrestored teeth. The fracture strength of group 5 (bulk-fill) was significantly higher than the fracture strength of the GIC laminate groups and not significantly different from the intact teeth (355±112N, P=0.118). The type of failure was unfavorable for most of the groups, with the majority being mixed failures. The use of a bulk-fill flowable base material significantly increased the fracture strength of extracted root-filled teeth with MOD cavities; however it did not improve fracture patterns to more favorable ones. Investigating restorative techniques that may improve the longevity of root-filled premolar teeth restored with direct resin restorations. Copyright © 2017 Elsevier Ltd. All rights reserved.

Facilities Management Guide for Asbestos and Lead

DTIC Science & Technology

2004-11-01

equipment such as HEPA filtered power tools, portable welding exhaust systems, and paint removal equipment when work disturbs lead. Do not dry sweep ...sampling and analysis of [______] paint bulk and wipe samples by atomic absorption spectrophotometry (AA) or anodic stripping voltametry (ASV...analysis. e. All bulk (destructive) collected for lead shall be analyzed by atomic absorption spectrophotometry (AA) or anodic stripping voltametry

Dynamics of lipid saccharide nanoparticles by quasielastic neutron scattering

NASA Astrophysics Data System (ADS)

Di Bari, M. T.; Gerelli, Y.; Sonvico, F.; Deriu, A.; Cavatorta, F.; Albanese, G.; Colombo, P.; Fernandez-Alonso, F.

2008-04-01

Nano- and microparticles composed of saccharide and lipid systems are extensively investigated for applications as highly biocompatible drug carriers. A detailed understanding of particle-solvent interactions is of key importance in order to tailor their characteristics for delivering drugs with specific chemical properties. Here we report results of a quasielastic neutron scattering (QENS) investigation on lecithin/chitosan nanoparticles prepared by autoassembling the two components in an aqueous solution. The measurements were performed at room temperature on lyophilized and H 2O hydrated nanoparticles ( h = 0.47 w H 2O/w hydrated sample). In the latter, hydration water is mostly enclosed inside the nanoparticles; its dynamics is similar to that of bulk water but with a significant decrease in diffusivity. The scattering from the nanoparticles can be described by a simple model of confined diffusion. In the lyophilized state only hydrogens belonging to the polar heads are seen as mobile within the experimental time-window. In the hydrated sample the diffusive dynamics involves also a significant part of the hydrogens in the lipid tails.

Gelatinized wheat starch influences crystallization behaviour and structure of roll-in shortenings in laminated bakery products.

PubMed

Mattice, Kristin D; Marangoni, Alejandro G

2018-03-15

One hydrogenated and one non-hydrogenated shortening were baked with isolated components of a croissant matrix, including crystalline wheat starch, gelatinized wheat starch, gluten, and formed gluten network. The impact of the matrix components on fat crystallization was analyzed for polymorphism using powder X-ray diffraction, solid fat content by pulsed nuclear magnetic resonance and thermal behaviour by differential scanning calorimetry. When compared to results obtained from croissants prepared with the respective shortenings, samples containing gelatinized wheat starch displayed notably similar results: polymorphic conversion, from the β' to β form over storage, and visually broader peaks in the melting endotherms indicating a greater temperature was required to completely melt all of the fat. All other component mixtures behaved similar to the respective fats in bulk. The measured rate of crystallization was greater in samples containing gelatinized wheat starch, indicating that the gelatinized starch could act as a nucleation site to speed crystallization. Copyright © 2017 Elsevier Ltd. All rights reserved.

Design of Inorganic Water Repellent Coatings for Thermal Protection Insulation on an Aerospace Vehicle

NASA Technical Reports Server (NTRS)

Fuerstenau, D. W.; Ravikumar, R.

1997-01-01

In this report, thin film deposition of one of the model candidate materials for use as water repellent coating on the thermal protection systems (TPS) of an aerospace vehicle was investigated. The material tested was boron nitride (BN), the water-repellent properties of which was detailed in our other investigation. Two different methods, chemical vapor deposition (CVD) and pulsed laser deposition (PLD), were used to prepare the BN films on a fused quartz substrate (one of the components of thermal protection systems on aerospace vehicles). The deposited films were characterized by a variety of techniques including X-ray diffraction, X-ray photoelectron spectroscopy, and scanning electron microscopy. The BN films were observed to be amorphous in nature, and a CVD-deposited film yielded a contact angle of 60 degrees with water, similar to the pellet BN samples investigated previously. This demonstrates that it is possible to use the bulk sample wetting properties as a guideline to determine the candidate waterproofing material for the TPS.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Siwei; Chen, Yan; Zhang, Lingling

Ceramic-based proton conductors enable high-temperature hydrogen economy applications such as hydrogen separation membranes, fuel cells, and steam electrolyzers. BaZr 0.8Y 0.2O 3-δ(BZY) proton-conducting oxide possesses the highest level of proton conductivity reported to date, but poor sinterability hinders its widespread utilization. In this paper, we report a two-step reactive aid sintering (TRAS) method involving the introduction of BaCO 3 and B 2O 3-Li 2O for the preparation of dense BZY ceramics sintered at 1500°C. The resulting BZY samples showed a pure perovskite structure with a dramatic increase in the relative density to 91.5%. In addition, the shrinkage during sintering wasmore » improved to 19.3% by a TRAS method as compared to 2.6% by the conventional solid date reaction method. In conclusion, the bulk conductivity was improved due to enhanced densification, while the grain boundary conductivity decreased due to the blocking behavior of the sintering aid resulting in a decrease in the total conductivity of the samples.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Siwei; Chen, Yan; Zhang, Lingling

Ceramic-based proton conductors enable high-temperature hydrogen economy applications such as hydrogen separation membranes, fuel cells, and steam electrolyzers. BaZr 0.8Y 0.2O 3-δ (BZY) proton-conducting oxide possesses the highest level of proton conductivity reported to date, but poor sinterability hinders its widespread utilization. Here, we report a two-step reactive aid sintering (TRAS) method involving the introduction of BaCO 3 and B 2O 3-Li 2O for the preparation of dense BZY ceramics sintered at 1500°C. The resulting BZY samples showed a pure perovskite structure with a dramatic increase in the relative density to 91.5%. In addition, the shrinkage during sintering was improvedmore » to 19.3% by a TRAS method as compared to 2.6% by the conventional solid date reaction method. Moreover, the bulk conductivity was improved due to enhanced densification, while the grain boundary conductivity decreased due to the blocking behavior of the sintering aid resulting in a decrease in the total conductivity of the samples.« less