Sample records for solid sampling graphite

  1. An Electron Microscopy Study of Graphite Growth in Nodular Cast Irons

    NASA Astrophysics Data System (ADS)

    Laffont, L.; Jday, R.; Lacaze, J.

    2018-04-01

    Growth of graphite during solidification and high-temperature solid-state transformation has been investigated in samples cut out from a thin-wall casting which solidified partly in the stable (iron-graphite) and partly in the metastable (iron-cementite) systems. Transmission electron microscopy has been used to characterize graphite nodules in as-cast state and in samples having been fully graphitized at various temperatures in the austenite field. Nodules in the as-cast material show a twofold structure characterized by an inner zone where graphite is disoriented and an outer zone where it is well crystallized. In heat-treated samples, graphite nodules consist of well-crystallized sectors radiating from the nucleus. These observations suggest that the disoriented zone appears because of mechanical deformation when the liquid contracts during its solidification in the metastable system. During heat-treatment, the graphite in this zone recrystallizes. In turn, it can be concluded that nodular graphite growth mechanism is the same during solidification and solid-state transformation.

  2. Liquid-phase and solid-phase microwave irradiations for reduction of graphite oxide

    NASA Astrophysics Data System (ADS)

    Zhao, Na; Wen, Chen-Yu; Zhang, David Wei; Wu, Dong-Ping; Zhang, Zhi-Bin; Zhang, Shi-Li

    2014-12-01

    In this paper, two microwave irradiation methods: (i) liquid-phase microwave irradiation (MWI) reduction of graphite oxide suspension dissolved in de-ionized water and N, N-dimethylformamide, respectively, and (ii) solid-phase MWI reduction of graphite oxide powder have been successfully carried out to reduce graphite oxide. The reduced graphene oxide products are thoroughly characterized by scanning electron microscopy, atomic force microscopy, X-ray photoelectron spectroscopy, Fourier transform infrared spectral analysis, Raman spectroscopy, UV-Vis absorption spectral analysis, and four-point probe conductivity measurements. The results show that both methods can efficiently remove the oxygen-containing functional groups attached to the graphite layers, though the solid-phase MWI reduction method can obtain far more efficiently a higher quality-reduced graphene oxide with fewer defects. The I(D)/I(G) ratio of the solid-phase MWI sample is as low as 0.46, which is only half of that of the liquid-phase MWI samples. The electrical conductivity of the reduced graphene oxide by the solid method reaches 747.9 S/m, which is about 25 times higher than that made by the liquid-phase method.

  3. Determination of lead in flour samples directly by solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Tinas, Hande; Ozbek, Nil; Akman, Suleyman

    2018-02-01

    In this study, lead concentrations in various flour samples were determined by high-resolution continuum source graphite furnace atomic absorption spectrometry with solid sampling. Since samples were analyzed directly, the risks and disadvantages of sample digestion were eliminated. Solid flour samples were dried, weighed on the platforms, Pd was added as a modifier and introduced directly into a graphite tube using a manual solid sampler. Platforms and tubes were coated with Zr. The optimized pyrolysis and atomization temperatures were 800 °C and 2200 °C, respectively. The sensitivities of lead in various flour certified reference materials (CRMs) and aqueous standards were not significantly different. Therefore, aqueous standards were safely used for calibration. The absolute limit of detection and characteristic mass were 7.2 pg and 9.0 pg of lead, respectively. The lead concentrations in different types of flour samples were found in the range of 25-52 μg kg- 1. Finally, homogeneity factors representing the heterogeneity of analyte distribution for lead in flour samples were determined.

  4. Solid sampling determination of magnesium in lithium niobate crystals by graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Dravecz, Gabriella; Laczai, Nikoletta; Hajdara, Ivett; Bencs, László

    2016-12-01

    The vaporization/atomization processes of Mg in high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS-GFAAS) were investigated by evaporating solid (powder) samples of lithium niobate (LiNbO3) optical single crystals doped with various amounts of Mg in a transversally heated graphite atomizer (THGA). Optimal analytical conditions were attained by using the Mg I 215.4353 nm secondary spectral line. An optimal pyrolysis temperature of 1500 °C was found for Mg, while the compromise atomization temperature in THGAs (2400 °C) was applied for analyte vaporization. The calibration was performed against solid (powered) lithium niobate crystal standards. The standards were prepared with exactly known Mg content via solid state fusion of the oxide components of the matrix and analyte. The correlation coefficient (R value) of the linear calibration was not worse than 0.9992. The calibration curves were linear in the dopant concentration range of interest (0.74-7.25 mg/g Mg), when dosing 3-10 mg of the powder samples into the graphite sample insertion boats. The Mg content of the studied 19 samples was in the range of 1.69-4.13 mg/g. The precision of the method was better than 6.3%. The accuracy of the results was verified by means of flame atomic absorption spectrometry with solution sample introduction after digestion of several crystal samples.

  5. Lithium loss in the solid electrolyte interphase: Lithium quantification of aged lithium ion battery graphite electrodes by means of laser ablation inductively coupled plasma mass spectrometry and inductively coupled plasma optical emission spectroscopy

    NASA Astrophysics Data System (ADS)

    Schwieters, Timo; Evertz, Marco; Mense, Maximilian; Winter, Martin; Nowak, Sascha

    2017-07-01

    In this work we present a new method using LA-ICP-MS to quantitatively determine the lithium content in aged graphite electrodes of a lithium ion battery (LIB) by performing total depth profiling. Matrix matched solid external standards are prepared using a solid doping approach to avoid elemental fractionation effects during the measurement. The results are compared and matched to the established ICP-OES technique for bulk quantification after performing a microwave assisted acid digestion. The method is applied to aged graphite electrodes in order to determine the lithium immobilization (= "Li loss") in the solid electrolyte interphase after the first cycle of formation. For this, different samples including a reference sample are created to obtain varying thicknesses of the SEI covering the electrode particles. By applying defined charging voltages, an initial lithiation process is performed to obtain specific graphite intercalation compounds (GICs, with target stoichiometries of LiC30, LiC18, LiC12 and LiC6). Afterwards, the graphite electrode is completely discharged to obtain samples without mobile, thus active lithium in its lattice. Taking the amount of lithium into account which originates from the residues of the LiPF6 (dissolved in the carbon components containing electrolyte), it is possible to subtract the amount of lithium in the SEI.

  6. Solid sampling determination of total fluorine in baby food samples by high-resolution continuum source graphite furnace molecular absorption spectrometry.

    PubMed

    Ozbek, Nil; Akman, Suleyman

    2016-11-15

    This study describes the applicability of solid sampling technique for the determination of fluorine in various baby foods via molecular absorption of calcium monofluoride generated in a graphite furnace of high-resolution continuum source atomic absorption spectrometry. Fluorine was determined at CaF wavelength, 606.440nm in a graphite tube applying a pyrolysis temperature of 1000°C and a molecule forming temperature of 2200°C. The limit of detection and characteristic mass of the method were 0.20ng and 0.17ng of fluorine, respectively. The fluorine concentrations determined in standard reference sample (bush branches and leaves) were in good agreement with the certified values. By applying the optimized parameters, the concentration of fluorine in various baby foods were determined. The fluorine concentrations were ranged from

  7. Solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry for gold determination in geological samples after preconcentration onto carbon nanotubes

    NASA Astrophysics Data System (ADS)

    Dobrowolski, Ryszard; Mróz, Agnieszka; Dąbrowska, Marzena; Olszański, Piotr

    2017-06-01

    A novelty method for the determination of gold in geological samples by solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry (SS HR CS GF AAS) after solid-phase extraction onto modified carbon nanotubes (CNT) was described. The methodology developed is based on solid phase extraction of Au(III) ions from digested samples to eliminate strong interference caused by iron compounds and problems related to inhomogeneities of the samples. The use of aqueous or solid standard for calibration was studied and the slope of calibration curve was the same for both of these modes. This statement indicates the possibility to perform the calibration of the method using aqueous standard solutions. Under optimum conditions the absolute detection limit for gold was equal to 2.24 · 10- 6 μg g- 1 while the adsorption capacity of modified carbon nanotubes was 264 mg g- 1. The proposed procedure was validated by the application of certified reference materials (CRMs) with different content of gold and different matrix, the results were in good agreement with certified values. The method was successfully applied for separation and determination of gold ions in complex geological samples, with precision generally better than 8%.

  8. Determination of trace and minor elements in alloys by atomic-absorption spectroscopy using an induction-heated graphite-well furnace as atom source-II.

    PubMed

    Ashy, M A; Headridge, J B; Sowerbutts, A

    1974-06-01

    Results are presented for the atomic-absorption spectrophotometric determination of zinc in aluminium and aluminium-silicon alloys, and aluminium, antimony and tin in steels, by means of solid samples dropped into an induction-heated graphite-well furnace to produce the atomic vapour.

  9. Determination of ruthenium in pharmaceutical compounds by graphite furnace atomic absorption spectroscopy.

    PubMed

    Jia, Xiujuan; Wang, Tiebang; Bu, Xiaodong; Tu, Qiang; Spencer, Sandra

    2006-04-11

    A graphite furnace atomic absorption (GFAA) spectrometric method for the determination of ruthenium (Rh) in solid and liquid pharmaceutical compounds has been developed. Samples are dissolved or diluted in dimethyl sulfoxide (DMSO) without any other treatment before they were analyzed by GFAA with a carefully designed heating program to avoid pre-atomization signal loss and to achieve suitable sensitivity. Various inorganic and organic solvents were tested and compared and DMSO was found to be the most suitable. In addition, ruthenium was found to be stable in DMSO for at least 5 days. Spike recoveries ranged from 81 to 100% and the limit of quantitation (LOQ) was determined to be 0.5 microg g(-1) for solid samples or 0.005 microg ml(-1) for liquid samples based a 100-fold dilution. The same set of samples was also analyzed by ICP-MS with a different sample preparation method, and excellent agreement was achieved.

  10. New Occurrence of Shocked Graphite Aggregates at Barringer Crater

    NASA Astrophysics Data System (ADS)

    Miura, Y.; Noma, Y.; Iancu, O. G.

    1993-07-01

    High-pressure carbon minera]s are considered to be formed by solid-solid transformation under static or impact high-pressure condition, but shocked quartz aggregates of impact craters are considered to be formed by quenched accretion of various aggregates by dynamic impact process [1-3]. The main purpose of this study is to elucidate new findings and occurrences of shocked graphite (SG) aggregates [2,3] at the Barringer meteorite crater. The graphite nodule block of Barringer Crater used in this study is collected near the rim. The sample is compared with standard graphite samples of Korea, Madagascar, and artificial impact graphites. There are four different mineral aggregates of the Barringer graphite nodule sample: (1) shocked graphite-1, (2) shocked graphite-2 and hexagonal diamond in the vein, (3) shocked quartz-1 (with kamacite) in the rim, and (4) calcite in the rim (Table 1). X-ray diffraction peaks of shocked graphite reveal low X-ray intensity, high Bragg-angle shift of X-ray diffraction peak, and multiple splitting of X-ray diffraction peaks. X-ray calculated density (rho) has been determined by X-ray diffractometer by the equation of density deviation Delta rho (%) = 100 x {(rho-rho(sub)0)/rho(sub)0}, where standard density rho(sub)0 is 2.255 g/cm^3 in Korean graphite [2,3]. The high-density value of shocked graphite grain obtained in Barringer is Delta rho = +0.6 +/- 0.1%. Shocked hexagonal diamonds (chaoite) show a high value of Delta rho = +0.6 +/- 0.9%. Analytical electron microscopy data reveal three different aggregates in the graphite nodule samples (Table 1): (1) shocked graphite-1 in the matrix, which contains uniformly Fe and Ca elements formed under gas state; (2) shocked graphite-2 in the vein, where crystallized shocked graphites and hexagonal diamonds are surrounded by kamacite-rich metals formed under gas-melt states of mixed compositions from iron meteorite and target rocks; and (3) shocked quartz-1 and kamacite in the rim, where coexisted elements are supplied from kamacite, sandstone, and limestone. The shocked quartz-1 grains with high density contain Fe and Ca elements that are different from the shocked quartz-2 of pure silica [1] formed at the final stage from the Coconino sandstone. (4) Limestone in the rim is attached from Kaibab limestone. The present shocked graphites with high density are the same as artificial fine-grained shocked graphites (Delta rho = +0.7%). Table 1, which appears here in the hard copy, shows formation stages with two shocked graphites in the Barringer Crater. Formation of shocked aggregates with chemical contamination indicate dynamic accretion processes of quenching and depression at impact. The existence of two shocked graphites indicates the two formation stages of the first gas-state and the second gas-melt states with quenching processes. The origin of carbon in the shocked graphites is considered in this study to be from Kaibab limestone. References: [1] Miura Y. (1991) Shock Waves, 1, 35-41. [2] Miura Y. (1992) Proc. Shock Waves (Japan), 2, 54-57. [3] Miura Y. et al. (1993) Symp. NIPR Antarctic Meteorite (Tokyo), in press. [4] Foote A. E. (1891) Am. J. Sci., 42, 413-417. [5] Hannemann R. E. et al. (1967) Science, 155, 995-997.

  11. Halloysite nanotubes as a solid sorbent in ultrasound-assisted dispersive micro solid-phase extraction for the determination of bismuth in water samples using high-resolution continuum source graphite-furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Krawczyk-Coda, Magdalena

    2017-03-01

    In this research, a simple, accurate, and inexpensive preconcentration procedure was developed for the determination of bismuth in water samples, using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS GFAAS). During the preconcentration step, halloysite nanotubes (HNTs) were used as a solid sorbent in ultrasound-assisted dispersive micro solid-phase extraction (USA DMSPE). The influence of the pH of the sample solution, amount of HNTs, and extraction time, as well as of the main parameters of HR CS GFAAS, on absorbance was investigated. The limit of detection was 0.005 μg L- 1. The preconcentration factor achieved for bismuth was 32. The relative standard deviation (RSD) was 4%. The accuracy of this method was validated by analyses of NIST SRM 1643e (Trace elements in water) and TMDA-54.5 (A high level fortified sample for trace elements) certified reference materials. The measured bismuth contents in these certified reference materials were in satisfactory agreement with the certified values according to the t-test for a 95% confidence level. The proposed method has been successfully applied to the determination of bismuth in five different real water samples (seawater, lake water, river water, stream water and rain water).

  12. Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of pesticides in water by Carbopak-B solid-phase extraction and high-preformance liquid chromatography

    USGS Publications Warehouse

    Werner, Stephen L.; Burkhardt, Mark R.; DeRusseau, Sabrina N.

    1996-01-01

    In accordance with the needs of the National Water-Quality Assessment Program (NAWQA), the U.S. Geological Survey has developed and implemented a graphitized carbon-based solid-phase extraction and high-performance liquid chromatographic analytical method. The method is used to determine 41 pesticides and pesticide metabolites that are not readily amenable to gas chromatography or other high-temperature analytical techniques. Pesticides are extracted from filtered environmental water samples using a 0.5-gram graphitized carbon-based solid-phase cartridge, eluted from the cartridge into two analytical fractions, and analyzed using high-performance liquid chromatography with photodiode-array detection. The upper concentration limit is 1.6 micrograms per liter (=B5g/L) for most compounds. Single-operator method detection limits in organic-free water samples ranged from 0.006 to 0.032 =B5g/L= Recoveries in organic-free water samples ranged from 37 to 88 percent. Recoveries in ground- and surface-water samples ranged from 29 to 94 percent. An optional on-site extraction procedure allows for samples to be collected and processed at remote sites where it is difficult to ship samples to the laboratory within the recommended pre-extraction holding time of 7 days.

  13. Global analysis of the temperature and flow fields in samples heated in multizone resistance furnaces

    NASA Astrophysics Data System (ADS)

    Pérez-Grande, I.; Rivas, D.; de Pablo, V.

    The temperature field in samples heated in multizone resistance furnaces will be analyzed, using a global model where the temperature fields in the sample, the furnace and the insulation are coupled; the input thermal data is the electric power supplied to the heaters. The radiation heat exchange between the sample and the furnace is formulated analytically, taking into account specular reflections at the sample; for the solid sample the reflectance is both diffuse and specular, and for the melt it is mostly specular. This behavior is modeled through the exchange view factors, which depend on whether the sample is solid or liquid, and, therefore, they are not known a priori. The effect of this specular behavior in the temperature field will be analyzed, by comparing with the case of diffuse samples. A parameter of great importance is the thermal conductivity of the insulation material; it will be shown that the temperature field depends strongly on it. A careful characterization of the insulation is therefore necessary, here it will be done with the aid of experimental results, which will also serve to validate the model. The heating process in the floating-zone technique in microgravity conditions will be simulated; parameters like the Marangoni number or the temperature gradient at the melt-crystal interface will be estimated. Application to the case of compound samples (graphite-silicon-graphite) will be made; the temperature distribution in the silicon part will be studied, especially the temperature difference between the two graphite rods that hold the silicon, since it drives the thermocapillary flow in the melt. This flow will be studied, after coupling the previous model with the convective effects. The possibility of suppresing this flow by the controlled vibration of the graphite rods will be also analyzed. Numerical results show that the thermocapillary flow can indeed be counterbalanced quite effectively.

  14. Simultaneous determination of Cd and Fe in beans and soil of different regions of Brazil using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sampling.

    PubMed

    dos Santos, Lisia M G; Welz, Bernhard; Araujo, Rennan G O; Jacob, Silvana do C; Vale, Maria Goreti R; Martens, Andreas; Gonzaga Martens, Irland B; Becker-Ross, Helmut

    2009-11-11

    A fast routine screening method for the simultaneous determination of cadmium and iron in bean and soil samples is proposed, using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sampling. The primary absorption line at 228.802 nm has been used for the determination of cadmium, and an adjacent secondary line, at 228.726 nm, for iron. Fourteen bean samples and 10 soil samples from nine states all over Brazil have been analyzed. The limits of detection (3 sigma, n = 10) were 2.0 microg kg(-1) for Cd and 4.5 mg kg(-1) for Fe. The relative standard deviation ranged from 4 to 7% for Cd and from 5 to 28% for Fe, which is usually acceptable for a screening method. The accuracy of the method has been confirmed by the analysis of two certified reference materials; the results were in agreement with the certified values at a 95% confidence interval.

  15. Sensitive Voltammetric Determination of Natural Flavonoid Quercetin on a Disposable Graphite Lead

    PubMed Central

    Vu, Dai Long; Žabčíková, Simona; Ertek, Bensu; Dilgin, Yusuf

    2015-01-01

    Summary In this paper, a pencil graphite electrode was pretreated using chronoamperometry technique in phosphate buffer solution (pH=7.0) for sensitive determination of quercetin. Oxidation of quercetin was investigated using pretreated pencil graphite electrode and anodic stripping differential pulse voltammetry. Under optimal conditions, the anodic current of quercetin exhibited linear response to its concentration in the range from 0.001 to 1.5 µmol/L with the limit of detection of 0.3·10–3 µmol/L. The proposed method was successfully applied for the determination of quercetin in cranberry and blackcurrant juices with recovery rate from 93.2 to 94.7%. Solid-phase extraction was found to be necessary prior to voltammetric determination of quercetin in fruit juice samples using pretreated pencil graphite electrode. PMID:27904372

  16. Charge and discharge characteristics of lithium-ion graphite electrodes in solid-state cells

    NASA Astrophysics Data System (ADS)

    Lemont, S.; Billaud, D.

    Lithium ions have been electrochemically intercalated into graphite in solid-state cells operating with solid polymer electrolytes based on poly(ethylene oxide) (PEO) complexed with lithium perchlorate (LiClO 4). The working composite electrode is composed of active-divided natural graphite associated with P(EO) 8-LiClO 4 acting as a binder and a Li + ionic conductor. Intercalation and de-intercalation of Li + were performed using galvanostatic or voltammetry techniques. The curves obtained in our solid-state cells were compared with those performed in liquid ethylene carbonate-LiClO 4 electrolyte. It is shown that in solid-state cells, side reactions occur both in the reduction and in the oxidation processes which leads to some uncertainty in the determination of the maximum reversible capacity of the graphite material.

  17. Tribological and Mechanical Behaviors of Polyamide 6/Glass Fiber Composite Filled with Various Solid Lubricants

    PubMed Central

    Li, Duxin; Xie, Ying; Li, Wenjuan; You, Yilan; Deng, Xin

    2013-01-01

    The effects of polytetrafluoroethylene (PTFE), graphite, ultrahigh molecular weight polyethylene (UHMWPE), and their compounds on mechanical and tribological properties of glass-fiber-reinforced polyamide 6 (PA6/GF) were studied. The polymeric materials were blended using twin-screw extruder and subsequently injection molded for test samples. Mechanical properties were investigated in terms of hardness, tensile strength, and impact strength. Friction and wear experiments were run under ambient conditions at a rotating speed of 200 rpm and load of 100 N. The morphologies of the worn surfaces were also observed with scanning electron microscope. The results showed that graphite could increase the tensile strength of PA6/GF-15 composite, but the material became soft. Graphite/UHMWPE complex solid lubricants were effective in increasing the already high impact strength of PA6/GF-15 composite. 5% PTFE gave the maximum reduction in the coefficient of friction. However, PTFE/UHMWPE complex solid lubricants were the best choice for improving both friction and wear behaviors due to the lower friction coefficient and mass wear rate. Moreover, the worn surface of PA6 composites revealed that adhesive wear, abrasive wear, and fatigue wear occurred in this study. PMID:23766687

  18. Solid hydrogen coated graphite particles in the interstellar medium. I.

    NASA Technical Reports Server (NTRS)

    Swamy, K. S. K.; Wickramasinghe, N. C.

    1969-01-01

    Solid para hydrogen coated graphite particles expulsion into interstellar medium from star formation regions, considering mantles stability and particles extinction efficiency, albedo and phase function

  19. Lead screening in DBS by solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry: application to newborns and pregnant women.

    PubMed

    Rello, Luis; Aramendía, Maite; Belarra, Miguel A; Resano, Martín

    2015-01-01

    DBS have become a clinical specimen especially adequate for establishing home-based collection protocols. In this work, high-resolution continuum source graphite furnace atomic absorption spectrometry is evaluated for the direct monitoring of Pb in DBS, both as a quantitative tool and a screening method. The development of the screening model is based on the establishment of the unreliability region around the threshold limits, 100 or 50 μg l(-1). More than 500 samples were analyzed to validate the model. The screening method demonstrated high sensitivity (the rate of true positives detected was always higher than 95%), an excellent LOD (1 µg l(-1)) and high throughput (10 min per sample).

  20. Solid lubricant materials for high temperatures: A review

    NASA Technical Reports Server (NTRS)

    Sliney, Harold E.

    1985-01-01

    Solid lubricants that can be used above 300 C in air are discussed, including coatings and self-lubricating composite bearing materials. The lubricants considered are representative dichalcogenides, graphite, graphite fluoride, polyimides, soft oxides, oxidatively stable fluorides, and hard coating materials. A few general design considerations revelant to solid lubrication are interspersed.

  1. CH4 Hydrate Formation between Silica and Graphite Surfaces: Insights from Microsecond Molecular Dynamics Simulations.

    PubMed

    He, Zhongjin; Linga, Praveen; Jiang, Jianwen

    2017-10-31

    Microsecond simulations have been performed to investigate CH 4 hydrate formation from gas/water two-phase systems between silica and graphite surfaces, respectively. The hydrophilic silica and hydrophobic graphite surfaces exhibit substantially different effects on CH 4 hydrate formation. The graphite surface adsorbs CH 4 molecules to form a nanobubble with a flat or negative curvature, resulting in a low aqueous CH 4 concentration, and hydrate nucleation does not occur during 2.5 μs simulation. Moreover, an ordered interfacial water bilayer forms between the nanobubble and graphite surface thus preventing their direct contact. In contrast, the hydroxylated-silica surface prefers to be hydrated by water, with a cylindrical nanobubble formed in the solution, leading to a high aqueous CH 4 concentration and hydrate nucleation in the bulk region; during hydrate growth, the nanobubble is gradually covered by hydrate solid and separated from the water phase, hence slowing growth. The silanol groups on the silica surface can form strong hydrogen bonds with water, and hydrate cages need to match the arrangements of silanols to form more hydrogen bonds. At the end of the simulation, the hydrate solid is separated from the silica surface by liquid water, with only several cages forming hydrogen bonds with the silica surface, mainly due to the low CH 4 aqueous concentrations near the surface. To further explore hydrate formation between graphite surfaces, CH 4 /water homogeneous solution systems are also simulated. CH 4 molecules in the solution are adsorbed onto graphite and hydrate nucleation occurs in the bulk region. During hydrate growth, the adsorbed CH 4 molecules are gradually converted into hydrate solid. It is found that the hydrate-like ordering of interfacial water induced by graphite promotes the contact between hydrate solid and graphite. We reveal that the ability of silanol groups on silica to form strong hydrogen bonds to stabilize incipient hydrate solid, as well as the ability of graphite to adsorb CH 4 molecules and induce hydrate-like ordering of the interfacial water, are the key factors to affect CH 4 hydrate formation between silica and graphite surfaces.

  2. Modifications of Graphite and Multiwall Carbon Nanotubes in the Presence of Urea

    NASA Astrophysics Data System (ADS)

    Duraia, El-Shazly M.; Fahami, Abbas; Beall, Gary W.

    2018-02-01

    The effect of high-energy ball milling on two carbon allotropes, graphite and multiwall carbon nanotubes (MWCNT) in the presence of urea has been studied. Samples were investigated using Raman spectroscopy, x-ray diffraction, scanning electron microscope (SEM) and x-ray photoelectron spectroscopy (XPS). Nitrogen-doped graphene has been successfully synthesized via a simple scalable mechanochemistry method using urea and graphite powder precursors. XPS results revealed the existence of the different nitrogen atoms configurations including pyridine, pyrrodic and graphitic N. SEM observations showed that the graphene nanosheets morphology become more wrinkles folded and crumbled as the milling time increased. The ID/IG ratio also increased as the milling time rose. The presence of both D' and G + D bands at 1621 cm-1 and 2940 cm-1, respectively, demonstrated the nitrogen incorporation in the graphene lattice Two factors contribute to the used urea: first it helps to exfoliate graphite into graphene, and second it preserves the graphitic structure from damage during the milling process as well as acting as a solid-state nitrogen source. Based on the phase analysis, the d-spacing of MWCNT samples in the presence of urea decreased due to the mechanical force in the milling process as the milling time increased. On the other hand, in the graphite case, due to its open flat surface, the graphite (002) peak shifts toward lower two theta as the milling time increase. Such findings are important and could be used for large-scale production of N-doped graphene, diminishing the use of either dangerous chemicals or sophisticated equipment.

  3. Simultaneous determination of V, Ni and Fe in fuel fly ash using solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry.

    PubMed

    Cárdenas Valdivia, A; Vereda Alonso, E; López Guerrero, M M; Gonzalez-Rodriguez, J; Cano Pavón, J M; García de Torres, A

    2018-03-01

    A green and simple method has been proposed in this work for the simultaneous determination of V, Ni and Fe in fuel ash samples by solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry (SS HR CS GFAAS). The application of fast programs in combination with direct solid sampling allows eliminating pretreatment steps, involving minimal manipulation of sample. Iridium treated platforms were applied throughout the present study, enabling the use of aqueous standards for calibration. Correlation coefficients for the calibration curves were typically better than 0.9931. The concentrations found in the fuel ash samples analysed ranged from 0.66% to 4.2% for V, 0.23-0.7% for Ni and 0.10-0.60% for Fe. Precision (%RSD) were 5.2%, 10.0% and 9.8% for V, Ni and Fe, respectively, obtained as the average of the %RSD of six replicates of each fuel ash sample. The optimum conditions established were applied to the determination of the target analytes in fuel ash samples. In order to test the accuracy and applicability of the proposed method in the analysis of samples, five ash samples from the combustion of fuel in power stations, were analysed. The method accuracy was evaluated by comparing the results obtained using the proposed method with the results obtained by ICP OES previous acid digestion. The results showed good agreement between them. The goal of this work has been to develop a fast and simple methodology that permits the use of aqueous standards for straightforward calibration and the simultaneous determination of V, Ni and Fe in fuel ash samples by direct SS HR CS GFAAS. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. 14C sample preparation for AMS microdosing studies at Lund University using online combustion and septa-sealed vials

    NASA Astrophysics Data System (ADS)

    Sydoff, Marie; Stenström, Kristina

    2010-04-01

    The Department of Physics at Lund University is participating in a European Union project called EUMAPP (European Union Microdose AMS Partnership Programme), in which sample preparation and accelerator mass spectrometry (AMS) measurements of biological samples from microdosing studies have been made. This paper describes a simplified method of converting biological samples to solid graphite for 14C analysis with AMS. The method is based on online combustion of the samples, and reduction of CO 2 in septa-sealed vials. The septa-sealed vials and disposable materials are used to eliminate sample cross-contamination. Measurements of ANU and Ox I standards show deviations of 2% and 3%, respectively, relative to reference values. This level of accuracy is sufficient for biological samples from microdosing studies. Since the method has very few handling steps from sample to graphite, the risk of failure during the sample preparation process is minimized, making the method easy to use in routine preparation of samples.

  5. Label-free potentiometric biosensor based on solid-contact for determination of total phenols in honey and propolis.

    PubMed

    Draghi, Patrícia Ferrante; Fernandes, Julio Cesar Bastos

    2017-03-01

    We developed a label-free potentiometric biosensor using tyrosinase extracted from Musa acuminata and immobilized by covalent bond on a surface of a solid-contact transducer. The transducer was manufactured containing two layers. The first layer contained a blend of poly(vinyl) chloride carboxylated (PVC-COOH), graphite and potassium permanganate. On this layer, we deposited a second layer containing just a mixture of poly(vinyl chloride) carboxylated and graphite. On the last layer of the transducer, we immobilized the tyrosinase enzyme by reaction with N-(3-dimethylaminopropyl)-N'-ethylcarbodiimide hydrochloride. The solid-contact potentiometric biosensor presented at low detection limit of 7.3×10 -7 M and a linear range to catechol concentration between 9.3×10 -7 M and 8.3×10 -2 M. This biosensor was applied to determine the amount of total phenols in different samples of honey and propolis. The results agreed with the Folin-Ciocalteu method. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Solid Fuel Burning in Steady, Strained, Premixed Flow Fields: The Graphite/Air/Methane System

    NASA Technical Reports Server (NTRS)

    Egolfopoulos, Fokion N.; Wu, Ming-Shin (Technical Monitor)

    2000-01-01

    A detailed numerical investigation was conducted on the simultaneous burning of laminar premixed CH4/air flames and solid graphite in a stagnation flow configuration. The graphite and methane were chosen for this model, given that they are practical fuels and their chemical kinetics are considered as the most reliable ones among solid and hydrocarbon fuels, respectively. The simulation was performed by solving the quasi-one-dimensional equations of mass, momentum, energy, and species. The GRI 2.1 scheme was used for the gas-phase kinetics, while the heterogeneous kinetics were described by a six-step mechanism including stable and radical species. The effects of the graphite surface temperature, the gas-phase equivalence ratio, and the aerodynamic strain rate on the graphite burning rate and NO, production and destruction mechanisms were assessed. Results indicate that as the graphite temperature increases, its burning rate as well as the NO, concentration increase. Furthermore, it was found that by increasing the strain rate, the graphite burning rate increases as a result of the augmented supply of the gas-phase reactants towards the surface, while the NO, concentration decreases as a result of the reduced residence time. The effect of the equivalence ratio on both the graphite burning rate and NO, concentration was found to be non-monotonic and strongly dependent on the graphite temperature. Comparisons between results obtained for a graphite and a chemically inert surface revealed that the chemical activity of the graphite surface can result to the reduction of NO through reactions of the CH3, CH2, CH, and N radicals with NO.

  7. [Determination of lead in edible salt with solid-phase extraction and GFAAS].

    PubMed

    Zhao, Xin; Zhou, Shuang; Ma, Lan; Yang, Dajin

    2013-01-01

    Establishing a method for determination of lead in salt with solid-phase extraction and GFAAS. Salt sample was diluted to a certain volume directly with ammonium acetate, then the sample solution was filtered through the solid phase extraction column which has been pre-activated. Lead ions were retained, and the sodium chloride matrix was removed. After elution, the collected lead ions was determined by graphite furnace atomic absorption spectrometry in 257.4 nm. This method can be used effectively to wipe off the sodium chloride in matrix. The limit of detection was 0.7 microg/kg and the limit of quantification was 2 microg/kg. Solid phase extraction technique can be used effectively to reduce the interference in matrix and improves the accuracy and reproducibility of detection.

  8. Graphite fluoride as a solid lubricant in a polyimide binder

    NASA Technical Reports Server (NTRS)

    Fusaro, R. L.; Sliney, H. E.

    1972-01-01

    Polyimide resin (PI) was shown to be a suitable binder material for the solid lubricant graphite fluoride, (CF(1.1))n. Comparisons were made to similar tests using PI-bonded MOS2 films, graphite fluoride rubbed films, and MOS2 rubbed films. The results showed that, at any one specific temperature between 25 and 400 C, the wear life of PI-bonded graphite fluoride films exceeded those of the other three films by at least a factor of 2 and by as much as a factor of 60. Minimum friction coefficients for the PI-bonded films were 0.08 for graphite fluoride and 0.04 for MOS2. The rider wear rates for the two PI-bonded films at 25 C were nearly equal.

  9. Trace analysis of high-purity graphite by LA-ICP-MS.

    PubMed

    Pickhardt, C; Becker, J S

    2001-07-01

    Laser-ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) has been established as a very efficient and sensitive technique for the direct analysis of solids. In this work the capability of LA-ICP-MS was investigated for determination of trace elements in high-purity graphite. Synthetic laboratory standards with a graphite matrix were prepared for the purpose of quantifying the analytical results. Doped trace elements, concentration 0.5 microg g(-1), in a laboratory standard were determined with an accuracy of 1% to +/- 7% and a relative standard deviation (RSD) of 2-13%. Solution-based calibration was also used for quantitative analysis of high-purity graphite. It was found that such calibration led to analytical results for trace-element determination in graphite with accuracy similar to that obtained by use of synthetic laboratory standards for quantification of analytical results. Results from quantitative determination of trace impurities in a real reactor-graphite sample, using both quantification approaches, were in good agreement. Detection limits for all elements of interest were determined in the low ng g(-1) concentration range. Improvement of detection limits by a factor of 10 was achieved for analyses of high-purity graphite with LA-ICP-MS under wet plasma conditions, because the lower background signal and increased element sensitivity.

  10. Ionic liquids at the surface of graphite: Wettability and structure

    NASA Astrophysics Data System (ADS)

    Bordes, Emilie; Douce, Laurent; Quitevis, Edward L.; Pádua, Agílio A. H.; Costa Gomes, Margarida

    2018-05-01

    The aim of this work is to provide a better understanding of the interface between graphite and different molecular and ionic liquids. Experimental measurements of the liquid surface tension and of the graphite-liquid contact angle for sixteen ionic liquids and three molecular liquids are reported. These experimental values allowed the calculation of the solid/liquid interfacial energy that varies, for the ionic liquids studied, between 14.5 mN m-1 for 1-ethyl-3-methylimidazolium dicyanamide and 37.8 mN m-1 for 3-dodecyl-1-(naphthalen-1-yl)-1H-imidazol-3-ium tetrafluoroborate. Imidazolium-based ionic liquids with large alkyl side-chains or functionalized with benzyl groups seem to interact more favourably with freshly peeled graphite surfaces. Even if the interfacial energy seems a good descriptor to assess the affinity of a liquid for a carbon-based solid material, we conclude that both the surface tension of the liquid and the contact angle between the liquid and the solid can be significant. Molecular dynamics simulations were used to investigate the ordering of the ions near the graphite surface. We conclude that the presence of large alkyl side-chains in the cations increases the ordering of ions at the graphite surface. Benzyl functional groups in the cations lead to a large affinity towards the graphite surface.

  11. 24-HOUR DIFFUSIVE SAMPLING OF 1,3-BUTADIENE IN AIR ONTO CARBONPAK X SOLID ADSORBENT WITH THEMAL DESORPTION/GC/MS ANALYSIS - FEASIBILITY STUDIES

    EPA Science Inventory

    Diffusive sampling of 1,3-butadiene for 24 hours onto the graphitic adsorbent Carbopack X contained in a stainless steel tube badge (6.3 mm OD, 5 mm ID, and 90 mm in length) with analysis by thermal desorption/GC/MS has been evaluated in controlled tests. A test matrix of 42 tr...

  12. 24-HOUR DIFFUSIVE SAMPLING OF 1,3-BUTADIENE IN AIR ONTO CARBOPACK X SOLID ADSORBENT FOLLOWED BY THERMAL DESORPTION/GC/MS ANALYSIS - FEASIBILITY STUDY

    EPA Science Inventory

    Diffusive sampling of 1,3-butadiene for 24 hr onto the graphitic adsorbent Carbopack X packed in a stainless steel tube badge (6.3 mm o.d., 5 mm i.d., and 90 mm in length) with analysis by thermal desorption/gas chromatography (GC)/mass spectrometry (MS) has been evaluated in con...

  13. Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of pesticides in water by graphitized carbon-based solid-phase extraction and high-performance liquid chromatography/mass spectrometry

    USGS Publications Warehouse

    Furlong, Edward T.; Anderson, Bruce D.; Werner, Stephen L.; Soliven, Paul P.; Coffey, Laura J.; Burkhardt, Mark R.

    2001-01-01

    In 1996, the U.S. Geological Survey National Water Quality Laboratory (NWQL) developed and implemented a graphitized carbon-based solid-phase extraction and high-performance liquid chromatographic analytical method to determine polar pesticide concentrations in surface- and ground-water samples. Subsequently, the NWQL developed a complementary analysis that uses high-performance liquid chromatography/mass spectrometry to detect, identify, and quantify polar pesticides and pesticide metabolites in filtered water at concentrations as low as 10 nanograms per liter. This new method was designed to improve sensitivity and selectivity over the prior method, and to reduce known interferences from natural organic matter.In this new method, pesticides are extracted from filtered water samples by useing a 0.5-gram graphitized carbon-based solid-phase extraction cartridge, eluted from the cartridge, and concentrations determined by using high-performance liquid chromatography with electrospray ionization-mass spectrometry. The upper concentration limit is 1.000 microgram per liter (μg/L) for most compounds. Single-operator method detection limits in organic-free water samples fortified with pesticides at a concentration of 0.025 μg/L ranged from 0.0019 to 0.022 μg/L for all compounds in the method. The grand mean (mean of mean recoveries for individual compounds) recoveries in organic-free water samples ranged from 72 to 89 percent, fortified with pesticides at three concentrations between 0.025 and 0.5 μg/L. Grand mean recoveries in ground- and surface-water samples ranged from 46 to 119 percent, also fortified with pesticides at three concentrations between 0.025 and 0.5 μg/L. Long-term recoveries from reagent water spikes were used to demonstrate that 38 of 65 compounds can be reported without qualification of the quantitative result across the analytical range of the method. The remaining 27 are reported with qualified estimates of concentration because of greater variability of recovery.

  14. Calculations of stopping powers of 100 eV-30 keV electrons in 31 elemental solids

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

    Tanuma, S.; Powell, C. J.; Penn, D. R.

    We present calculated electron stopping powers (SPs) for 31 elemental solids (Li, Be, glassy C, graphite, diamond, Na, Mg, K, Sc, Ti, V, Fe, Y, Zr, Nb, Mo, Ru, Rh, In, Sn, Cs, Gd, Tb, Dy, Hf, Ta, W, Re, Os, Ir, and Bi). These SPs were determined with an algorithm previously used for the calculation of electron inelastic mean free paths and from energy-loss functions (ELFs) derived from experimental optical data. The SP calculations were made for electron energies between 100 eV and 30 keV and supplement our earlier SP calculations for ten additional solids (Al, Si, Cr, Ni,more » Cu, Ge, Pd, Ag, Pt, and Au). Plots of SP versus atomic number for the group of 41 solids show clear trends. Multiple peaks and shoulders are seen that result from the contributions of valence-electron and various inner-shell excitations. Satisfactory agreement was found between the calculated SPs and values from the relativistic Bethe SP equation with recommended values of the mean excitation energy (MEE) for energies above 10 keV. We determined effective MEEs versus maximum excitation energy from the ELFs for each solid. Plots of effective MEE versus atomic number showed the relative contributions of valence-electron and different core-electron excitations to the MEE. For a maximum excitation energy of 30 keV, our effective MEEs agreed well for Be, graphite, Na, Al, and Si with recommended MEEs; a difference for Li was attributed to sample oxidation in the SP measurements for the recommended MEE. Substantially different effective MEEs were found for the three carbon allotropes (graphite, diamond, and glassy C)« less

  15. High density-high purity graphite prepared by hot isostatic pressing in refractory metal containers

    DOEpatents

    Hoenig, Clarence L.

    1994-01-01

    Porous graphite in solid form is hot isostatically pressed in a refractory metal container to produce a solid graphite monolith with a bulk density greater than or equal to 2.10 g/cc. The refractory metal container is formed of tantalum, niobium, tungsten, molybdenum or alloys thereof in the form of a canister or alternatively plasma sprayed, chemically vapor deposited, or coated by some other suitable means onto graphite. Hot isostatic pressing at 2200.degree. C. and 30 KSI (206.8 MPa) argon pressure for two hours produces a bulk density of 2.10 g/cc. Complex shapes can be made.

  16. High density-high purity graphite prepared by hot isostatic pressing in refractory metal containers

    DOEpatents

    Hoenig, C.L.

    1994-08-09

    Porous graphite in solid form is hot isostatically pressed in a refractory metal container to produce a solid graphite monolith with a bulk density greater than or equal to 2.10 g/cc. The refractory metal container is formed of tantalum, niobium, tungsten, molybdenum or alloys thereof in the form of a canister or alternatively plasma sprayed, chemically vapor deposited, or coated by some other suitable means onto graphite. Hot isostatic pressing at 2,200 C and 30 KSI (206.8 MPa) argon pressure for two hours produces a bulk density of 2.10 g/cc. Complex shapes can be made. 1 fig.

  17. Determination of copper and mercury in phosphate fertilizers employing direct solid sampling analysis and high resolution continuum source graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    de Oliveira Souza, Sidnei; François, Luciane Luiza; Borges, Aline Rocha; Vale, Maria Goreti Rodrigues; Araujo, Rennan Geovanny Oliveira

    2015-12-01

    The present study proposes the determination of copper and mercury in phosphate fertilizers by direct solid sampling analysis (SS) employing high resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS). For Cu determination, two analytical lines were used: 327.3960 nm and 249.2146 nm. Hg determination was carried out on the line 253.6521 nm and 100 μg KMnO4 was used as chemical modifier. The optimal pyrolysis temperature for Cu determination was 1300 °C. Atomization temperatures for Cu and Hg were 2400 and 1100 °C, respectively. External calibration with aqueous standard solutions was adopted for both elements. The limits of quantification (LoQs) and characteristic mass (m0) obtained for Cu determination were 0.4 μg g- 1 and 1.12 ng, respectively, on line 249.2146 nm, and 64 μg g- 1 and 25 pg on 327.3960 nm. For mercury, LoQ and m0 were 4.8 ng g- 1 and 39 pg, respectively. The accuracy of the proposed methods was confirmed by the analysis of standard reference material (SRM) of Trace Elements in Multi-Nutrient Fertilizer (SRM NIST 695). The precision expressed as relative standard deviation (RSD), was better than 8.2% for Hg and 7.7% for the Cu (n = 5), considered satisfactory for microanalysis in solid sample. Four fertilizer samples acquired in commercial establishments in the city of Salvador, Bahia, Brazil, were analyzed. The optimized analytical methods were simple, fast, accurate, precise and free of spectral interferences for the determination of Cu and Hg in phosphate fertilizer samples by SS-HR-CS GF AAS, avoiding the dissolution of the sample, the use of harmful reagents and the generation of residues.

  18. Artificially-built solid electrolyte interphase via surface-bonded vinylene carbonate derivative on graphite by molecular layer deposition

    NASA Astrophysics Data System (ADS)

    Chae, Seulki; Lee, Jeong Beom; Lee, Jae Gil; Lee, Tae-jin; Soon, Jiyong; Ryu, Ji Heon; Lee, Jin Seok; Oh, Seung M.

    2017-12-01

    Vinylene carbonate (VC) is attached in a ring-opened form on a graphite surface by molecular layer deposition (MLD) method, and its role as a solid electrolyte interphase (SEI) former is studied. When VC is added into the electrolyte solution of a graphite/LiNi0.5Mn1.5O4 (LNMO) full-cell, it is reductively decomposed to form an effective SEI on the graphite electrode. However, VC in the electrolyte solution has serious adverse effects due to its poor stability against electrochemical oxidation on the LNMO positive electrode. A excessive acid generation as a result of VC oxidation is observed, causing metal dissolution from the LNMO electrode. The dissolved metal ions are plated on the graphite electrode to destroy the SEI layer, eventually causing serious capacity fading and poor Coulombic efficiency. The VC derivative on the graphite surface also forms an effective SEI layer on the graphite negative electrode via reductive decomposition. The detrimental effects on the LNMO positive electrode, however, can be avoided because the bonded VC derivative on the graphite surface cannot move to the LNMO electrode. Consequently, the graphite/LNMO full-cell fabricated with the VC-attached graphite outperforms the cells without VC or with VC in the electrolyte, in terms of Coulombic efficiency and capacity retention.

  19. Novel approach to microwave-assisted extraction and micro-solid-phase extraction from soil using graphite fibers as sorbent.

    PubMed

    Xu, Li; Lee, Hian Kee

    2008-05-30

    A single-step extraction-cleanup procedure involving microwave-assisted extraction (MAE) and micro-solid-phase extraction (micro-SPE) has been developed for the analysis of polycyclic aromatic hydrocarbons (PAHs) from soil samples. Micro-SPE is a relatively new extraction procedure that makes use of a sorbent enclosed within a sealed polypropylene membrane envelope. In the present work, for the first time, graphite fiber was used as a sorbent material for extraction. MAE-micro-SPE was used to cleanup sediment samples and to extract and preconcentrate five PAHs in sediment samples prepared as slurries with addition of water. The best extraction conditions comprised of microwave heating at 50 degrees C for a duration of 20 min, and an elution (desorption) time of 5 min using acetonitrile with sonication. Using gas chromatography (GC)-flame ionization detection (FID), the limits of detection (LODs) of the PAHs ranged between 2.2 and 3.6 ng/g. With GC-mass spectrometry (MS), LODs were between 0.0017 and 0.0057 ng/g. The linear ranges were between 0.1 and 50 or 100 microg/g for GC-FID analysis, and 1 and 500 or 1000 ng/g for GC-MS analysis. Granular activated carbon was also used for the micro-SPE device but was found to be not as efficient in the PAH extraction. The MAE-micro-SPE method was successfully used for the extraction of PAHs in river and marine sediments, demonstrating its applicability to real environmental solid matrixes.

  20. Ab initio molecular dynamics simulations of the initial stages of solid-electrolyte interphase formation on lithium ion battery graphitic anodes.

    PubMed

    Leung, Kevin; Budzien, Joanne L

    2010-07-07

    The decomposition of ethylene carbonate (EC) during the initial growth of solid-electrolyte interphase (SEI) films at the solvent-graphitic anode interface is critical to lithium ion battery operations. Ab initio molecular dynamics simulations of explicit liquid EC/graphite interfaces are conducted to study these electrochemical reactions. We show that carbon edge terminations are crucial at this stage, and that achievable experimental conditions can lead to surprisingly fast EC breakdown mechanisms, yielding decomposition products seen in experiments but not previously predicted.

  1. The complex ion structure of warm dense carbon measured by spectrally resolved x-ray scattering

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

    Kraus, D.; Barbrel, B.; Falcone, R. W.

    2015-05-15

    We present measurements of the complex ion structure of warm dense carbon close to the melting line at pressures around 100 GPa. High-pressure samples were created by laser-driven shock compression of graphite and probed by intense laser-generated x-ray sources with photon energies of 4.75 keV and 4.95 keV. High-efficiency crystal spectrometers allow for spectrally resolving the scattered radiation. Comparing the ratio of elastically and inelastically scattered radiation, we find evidence for a complex bonded liquid that is predicted by ab-initio quantum simulations showing the influence of chemical bonds under these conditions. Using graphite samples of different initial densities we demonstrate the capability ofmore » spectrally resolved x-ray scattering to monitor the carbon solid-liquid transition at relatively constant pressure of 150 GPa. Showing first single-pulse scattering spectra from cold graphite of unprecedented quality recorded at the Linac Coherent Light Source, we demonstrate the outstanding possibilities for future high-precision measurements at 4th Generation Light Sources.« less

  2. Determination of submicrogram-per-liter concentrations of caffeine in surface water and groundwater samples by solid-phase extraction and liquid chromatography

    USGS Publications Warehouse

    Burkhardt, M.R.; Soliven, P.P.; Werner, S.L.; Vaught, D.G.

    1999-01-01

    A method for determining submicrogram-per-liter concentrations of caffeine in surface water and groundwater samples has been developed. Caffeine is extracted from a 1 L water sample with a 0.5 g graphitized carbon-based solid-phase cartridge, eluted with methylene chloride-methanol (80 + 20, v/v), and analyzed by liquid chromatography with photodiode-array detection. The single-operator method detection limit for organic-free water samples was 0.02 ??g/L. Mean recoveries and relative standard deviations were 93 ?? 13% for organicfree water samples fortified at 0.04 ??g/L and 84 ?? 4% for laboratory reagent spikes fortified at 0.5 ??g/L. Environmental concentrations of caffeine ranged from 0.003 to 1.44 ??g/L in surface water samples and from 0.01 to 0.08 ??g/L in groundwater samples.

  3. Graphite Carbon-Supported Mo2C Nanocomposites by a Single-Step Solid State Reaction for Electrochemical Oxygen Reduction.

    PubMed

    Huang, K; Bi, K; Liang, C; Lin, S; Wang, W J; Yang, T Z; Liu, J; Zhang, R; Fan, D Y; Wang, Y G; Lei, M

    2015-01-01

    Novel graphite-molybdenum carbide nanocomposites (G-Mo2C) are synthesized by a typical solid state reaction with melamine and MoO3 as precursors under inert atmosphere. The characterization results indicate that G-Mo2C composites are composed of high crystallization and purity of Mo2C and few layers of graphite carbon. Mo2C nanoparticles with sizes ranging from 5 to 50 nm are uniformly supported by surrounding graphite layers. It is believed that Mo atom resulting from the reduction of MoO3 is beneficial to the immobilization of graphite carbon. Moreover, the electrocatalytic performances of G-Mo2C for ORR in alkaline medium are investigated by cyclic voltammetry (CV), rotating disk electrode (RDE) and chronoamperometry test with 3M methanol. The results show that G-Mo2C has a considerable catalytic activity and superior methanol tolerance performance for the oxygen reduction reaction (ORR) benefiting from the chemical interaction between the carbide nanoparticles and graphite carbon.

  4. Preparation by low-temperature nonthermal plasma of graphite fiber and its characteristics for solid-phase microextraction.

    PubMed

    Luo, Fan; Wu, Zucheng; Tao, Ping; Cong, Yanqing

    2009-01-05

    Low-temperature nonthermal plasma has been used to prepare solid-phase microextraction (SPME) fibers with high adsorbability, long-term serviceability, and high reproducibility. Graphite rods serving as fiber precursors were treated by an air plasma discharged at 15.2-15.5 kV for a duration of 8 min. Sampling results revealed that the adsorptive capacity of the homemade fiber was 2.5-34.6 times that of a polyacrylate (PA) fiber for alcohols (methanol, ethanol, isopropyl alcohol, n-butyl alcohol), and about 1.4-1.6 times and 2.5-5.1 times that of an activated carbon fiber (ACF) for alcohols and BTEX (benzene, toluene, ethylbenzene, and xylenes), respectively. It is confirmed from FTIR (Fourier transform infrared spectrophotometer) and SEM (scanning electron microscope) analyses that the improvement in the adsorptive performance attributed to increased surface energy and roughness of the graphite fiber. Using gas chromatography (GC)-flame-ionization detector (FID), the limits of detection (LODs) of the alcohols and BTEX ranged between 0.19 and 3.75 microg L(-1), the linear ranges were between 0.6 and 35,619 microg L(-1) with good linearity (R(2)=0.9964-0.9997). It was demonstrated that nonthermal plasma offers a fast and simple method for preparing an efficient graphite SPME fiber, and that SPME using the homemade fiber represents a sensitive and selective extraction method for the analysis of a wide range of organic compounds.

  5. Mechanical Property Allowables Generated for the Solid Rocket Booster Composite Note Cap

    NASA Technical Reports Server (NTRS)

    Hodge, A. J.

    2000-01-01

    Mechanical property characterization was performed on AS4/3501-6 graphite/epoxy and SC350G syntactic foam for the SRB Composite Nose Cap Shuttle Upgrades Project. Lamina level properties for the graphite/epoxy were determined at room temperature, 240 F, 350 F, 480 F, 600 F, and 350 F after a cycle to 600 F. Graphite/epoxy samples were moisture conditioned prior to testing. The syntactic foam material was tested at room temperature, 350 F, and 480 F. A high-temperature test facility was developed at MSFC. Testing was performed with quartz lamp heaters and high resistance heater strips. The thermal history profile of the nose cap was simulated in order to test materials at various times during launch. A correlation study was performed with Southern Research Institute to confirm the test methodology and validity of test results. A-basis allowables were generated from the results of testing on three lots of material.

  6. Ignitability of Diesel Fuel with an Inclusion of Ultrafine Carbon Particles

    NASA Astrophysics Data System (ADS)

    Krivosheev, P. N.; Leshchevich, V. V.; Shimchenko, S. Yu.; Shushkov, S. V.; Penyazkov, O. G.

    2017-11-01

    Nanosize carbon fuel additions were synthesized by the action of an electric discharge on a diesel fuel. Depending on the discharge regime, variously shaped carbon particles, including planar graphitized ones, were formed in the fuel. Ignitability of the produced samples was assessed by the method of initiation of a foamed fuel sample by a lowcurrent electric arc. The modified fuel showed the improvement of the ignition characteristics in the presence of a nanodispersed solid phase.

  7. Flame speed enhancement of solid nitrocellulose monopropellant coupled with graphite at microscales

    NASA Astrophysics Data System (ADS)

    Jain, S.; Yehia, O.; Qiao, L.

    2016-03-01

    The flame-speed-enhancement phenomenon of a solid monopropellant (nitrocellulose) using a highly conductive thermal base (graphite sheet) was demonstrated and studied both experimentally and theoretically. A propellant layer ranging from 20 μm to 170 μm was deposited on the top of a 20-μm thick graphite sheet. Self-propagating oscillatory combustion waves were observed, with average flame speed enhancements up to 14 times the bulk value. The ratio of the fuel-to-graphite layer thickness affects not only the average reaction front velocities but also the period and the amplitude of the combustion wave oscillations. To better understand the flame-speed enhancement and the oscillatory nature of the combustion waves, the coupled nitrocellulose-graphite system was modeled using one-dimensional energy conservation equations along with simple one-step chemistry. The period and the amplitude of the oscillatory combustion waves were predicted as a function of the ratio of the fuel-to-graphite thickness (R), the ratio of the graphite-to-fuel thermal diffusivity (α0), and the non-dimensional inverse adiabatic temperature rise (β). The predicted flame speeds and the characteristics of the oscillations agree well with the experimental data. The new concept of using a highly conductive thermal base such as carbon-based nano- and microstructures to enhance flame propagation speed or burning rate of propellants and fuels could lead to improved performance of solid and liquid rocket motors, as well as of the alternative energy conversion microelectromechanical devices.

  8. Preliminary Results of IS Plasma Focus as a Breeder of Short-Lived Radioisotopes 12C(d,n)13N

    NASA Astrophysics Data System (ADS)

    Sadat Kiai, S. M.; Elahi, M.; Adlparvar, S.; Shahhoseini, E.; Sheibani, S.; Ranjber akivaj, H.; Alhooie, S.; Safarien, A.; Farhangi, S.; Aghaei, N.; Amini, S.; Khalaj, M. M.; Zirak, A. R.; Dabirzadeh, A. A.; Soleimani, J.; Torkzadeh, F.; Mousazadeh, M. M.; Moradi, K.; Abdollahzadeh, M.; Talaei, A.; Zaeem, A. A.; Moslehi, A.; Kashani, A.; Babazadeh, A. R.; Bagiyan, F.; Ardestani, M.; Roozbahani, A.; Pourbeigi, H.; Tajik Ahmadi, H.; Ahmadifaghih, M. A.; Mahlooji, M. S.; Mortazavi, B. N.; Zahedi, F.

    2011-04-01

    Modified IS (Iranian Sun) plasma focus (10 kJ,15 kV, 94 μF, 0.1 Hz) has been used to produce the short-lived radioisotope 13N (half-life of 9.97 min) through 12C(d,n)13N nuclear reaction. The filling gas was 1.5-3 torr of hydrogen (60%) deuterium (40%) mixture. The target was solid nuclear grade graphite with 5 mm thick, 9 cm width and 13 in length. The activations of the exogenous target on average of 20 shots (only one-third acceptable) through 10-13 kV produced the 511 keV gamma rays. Another peak found at the 570 keV gamma of which both was measured by a NaI portable gamma spectrometer calibrated by a 137Cs 0.25 μCi sealed reference source with its single line at 661.65 keV and 22Na 0.1 μCi at 511 keV. To measure the gamma rays, the graphite target converts to three different phases; solid graphite, powder graphite, and powder graphite in water solution. The later phase approximately has a doubled activity with respect to the solid graphite target up to 0.5 μCi of 511 keV and 1.1 μCi of 570 keV gamma lines were produced. This increment in activity was perhaps due to structural transformation of graphite powder to nano-particles characteristic in liquid water.

  9. Organic matter and containment of uranium and fissiogenic isotopes at the Oklo natural reactors

    USGS Publications Warehouse

    Nagy, B.; Gauthier-Lafaye, F.; Holliger, P.; Davis, D.W.; Mossman, D.J.; Leventhal, J.S.; Rigali, M.J.; Parnell, J.

    1991-01-01

    SOME of the Precambrian natural fission reactors at Oklo in Gabon contain abundant organic matter1,2, part of which was liquefied at the time of criticality and subsequently converted to a graphitic solid3,4. The liquid organic matter helps to reduce U(VI) to U(IV) from aqueous solutions, resulting in the precipitation of uraninite5. It is known that in the prevailing reactor environments, precipitated uraninite grains incorporated fission products. We report here observations which show that these uraninite crystals were held immobile within the resolidified, graphitic bitumen. Unlike water-soluble (humic) organic matter, the graphitic bituminous organics at Oklo thus enhanced radionu-clide containment. Uraninite encased in solid graphitic matter in the organic-rich reactor zones lost virtually no fissiogenic lan-thanide isotopes. The first major episode of uranium and lead migration was caused by the intrusion of a swarm of adjacent dolerite dykes about 1,100 Myr after the reactors went critical. Our results from Oklo imply that the use of organic, hydrophobic solids such as graphitic bitumen as a means of immobilizing radionuclides in pretreated nuclear waste warrants further investigation. ?? 1991 Nature Publishing Group.

  10. Mycoestrogen determination in cow milk: Magnetic solid-phase extraction followed by liquid chromatography and tandem mass spectrometry analysis.

    PubMed

    Capriotti, Anna Laura; Cavaliere, Chiara; Foglia, Patrizia; La Barbera, Giorgia; Samperi, Roberto; Ventura, Salvatore; Laganà, Aldo

    2016-12-01

    Recently, magnetic solid-phase extraction has gained interest because it presents various operational advantages over classical solid-phase extraction. Furthermore, magnetic nanoparticles are easy to prepare, and various materials can be used in their synthesis. In the literature, there are only few studies on the determination of mycoestrogens in milk, although their carryover in milk has occurred. In this work, we wanted to develop the first (to the best of our knowledge) magnetic solid-phase extraction protocol for six mycoestrogens from milk, followed by liquid chromatography and tandem mass spectrometry analysis. Magnetic graphitized carbon black was chosen as the adsorbent, as this carbonaceous material, which is very different from the most diffuse graphene and carbon nanotubes, had already shown selectivity towards estrogenic compounds in milk. The graphitized carbon black was decorated with Fe 3 O 4 , which was confirmed by the characterization analyses. A milk deproteinization step was avoided, using only a suitable dilution in phosphate buffer as sample pretreatment. The overall process efficiency ranged between 52 and 102%, whereas the matrix effect considered as signal suppression was below 33% for all the analytes even at the lowest spiking level. The obtained method limits of quantification were below those of other published methods that employ classical solid-phase extraction protocols. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. 3-Dimensional atomic scale structure of the ionic liquid-graphite interface elucidated by AM-AFM and quantum chemical simulations

    NASA Astrophysics Data System (ADS)

    Page, Alister J.; Elbourne, Aaron; Stefanovic, Ryan; Addicoat, Matthew A.; Warr, Gregory G.; Voïtchovsky, Kislon; Atkin, Rob

    2014-06-01

    In situ amplitude modulated atomic force microscopy (AM-AFM) and quantum chemical simulations are used to resolve the structure of the highly ordered pyrolytic graphite (HOPG)-bulk propylammonium nitrate (PAN) interface with resolution comparable with that achieved for frozen ionic liquid (IL) monolayers using STM. This is the first time that (a) molecular resolution images of bulk IL-solid interfaces have been achieved, (b) the lateral structure of the IL graphite interface has been imaged for any IL, (c) AM-AFM has elucidated molecular level structure immersed in a viscous liquid and (d) it has been demonstrated that the IL structure at solid surfaces is a consequence of both thermodynamic and kinetic effects. The lateral structure of the PAN-graphite interface is highly ordered and consists of remarkably well-defined domains of a rhomboidal superstructure composed of propylammonium cations preferentially aligned along two of the three directions in the underlying graphite lattice. The nanostructure is primarily determined by the cation. Van der Waals interactions between the propylammonium chains and the surface mean that the cation is enriched in the surface layer, and is much less mobile than the anion. The presence of a heterogeneous lateral structure at an ionic liquid-solid interface has wide ranging ramifications for ionic liquid applications, including lubrication, capacitive charge storage and electrodeposition.In situ amplitude modulated atomic force microscopy (AM-AFM) and quantum chemical simulations are used to resolve the structure of the highly ordered pyrolytic graphite (HOPG)-bulk propylammonium nitrate (PAN) interface with resolution comparable with that achieved for frozen ionic liquid (IL) monolayers using STM. This is the first time that (a) molecular resolution images of bulk IL-solid interfaces have been achieved, (b) the lateral structure of the IL graphite interface has been imaged for any IL, (c) AM-AFM has elucidated molecular level structure immersed in a viscous liquid and (d) it has been demonstrated that the IL structure at solid surfaces is a consequence of both thermodynamic and kinetic effects. The lateral structure of the PAN-graphite interface is highly ordered and consists of remarkably well-defined domains of a rhomboidal superstructure composed of propylammonium cations preferentially aligned along two of the three directions in the underlying graphite lattice. The nanostructure is primarily determined by the cation. Van der Waals interactions between the propylammonium chains and the surface mean that the cation is enriched in the surface layer, and is much less mobile than the anion. The presence of a heterogeneous lateral structure at an ionic liquid-solid interface has wide ranging ramifications for ionic liquid applications, including lubrication, capacitive charge storage and electrodeposition. Electronic supplementary information (ESI) available. See DOI: 10.1039/c4nr01219d

  12. Novel ion imprinted magnetic mesoporous silica for selective magnetic solid phase extraction of trace Cd followed by graphite furnace atomic absorption spectrometry detection

    NASA Astrophysics Data System (ADS)

    Zhao, Bingshan; He, Man; Chen, Beibei; Hu, Bin

    2015-05-01

    Determination of trace Cd in environmental, biological and food samples is of great significance to toxicological research and environmental pollution monitoring. While the direct determination of Cd in real-world samples is difficult due to its low concentration and the complex matrix. Herein, a novel Cd(II)-ion imprinted magnetic mesoporous silica (Cd(II)-II-MMS) was prepared and was employed as a selective magnetic solid-phase extraction (MSPE) material for extraction of trace Cd in real-world samples followed by graphite furnace atomic absorption spectrometry (GFAAS) detection. Under the optimized conditions, the detection limit of the proposed method was 6.1 ng L- 1 for Cd with the relative standard deviation (RSD) of 4.0% (c = 50 ng L- 1, n = 7), and the enrichment factor was 50-fold. To validate the proposed method, Certified Reference Materials of GSBZ 50009-88 environmental water, ZK018-1 lyophilized human urine and NIES10-b rice flour were analyzed and the determined values were in a good agreement with the certified values. The proposed method exhibited a robust anti-interference ability due to the good selectivity of Cd(II)-II-MMS toward Cd(II). It was successfully employed for the determination of trace Cd(II) in environmental water, human urine and rice samples with recoveries of 89.3-116%, demonstrating that the proposed method has good application potential in real world samples with complex matrix.

  13. Developments in Hollow Graphite Fiber Technology

    NASA Technical Reports Server (NTRS)

    Stallcup, Michael; Brantley, Lott W., Jr. (Technical Monitor)

    2002-01-01

    Hollow graphite fibers will be lighter than standard solid graphite fibers and, thus, will save weight in optical components. This program will optimize the processing and properties of hollow carbon fibers developed by MER and to scale-up the processing to produce sufficient fiber for fabricating a large ultra-lightweight mirror for delivery to NASA.

  14. Multistage Mechanism of Lithium Intercalation into Graphite Anodes in the Presence of the Solid Electrolyte Interface.

    PubMed

    Dinkelacker, Franz; Marzak, Philipp; Yun, Jeongsik; Liang, Yunchang; Bandarenka, Aliaksandr S

    2018-04-25

    A so-called solid electrolyte interface (SEI) in a lithium-ion battery largely determines the performance of the whole system. However, it is one of the least understood objects in these types of batteries. SEIs are formed during the initial charge-discharge cycles, prevent the organic electrolytes from further decomposition, and at the same time govern lithium intercalation into the graphite anodes. In this work, we use electrochemical impedance spectroscopy and atomic force microscopy to investigate the properties of a SEI film and an electrified "graphite/SEI/electrolyte interface". We reveal a multistage mechanism of lithium intercalation and de-intercalation in the case of graphite anodes covered by SEI. On the basis of this mechanism, we propose a relatively simple model, which perfectly explains the impedance response of the "graphite/SEI/electrolyte" interface at different temperatures and states of charge. From the whole data obtained in this work, it is suggested that not only Li + but also negatively charged species, such as anions from the electrolyte or functional groups of the SEI, likely interact with the surface of the graphite anode.

  15. Evidence for Bulk Ripplocations in Layered Solids

    NASA Astrophysics Data System (ADS)

    Gruber, Jacob; Lang, Andrew C.; Griggs, Justin; Taheri, Mitra L.; Tucker, Garritt J.; Barsoum, Michel W.

    2016-09-01

    Plastically anisotropic/layered solids are ubiquitous in nature and understanding how they deform is crucial in geology, nuclear engineering, microelectronics, among other fields. Recently, a new defect termed a ripplocation-best described as an atomic scale ripple-was proposed to explain deformation in two-dimensional solids. Herein, we leverage atomistic simulations of graphite to extend the ripplocation idea to bulk layered solids, and confirm that it is essentially a buckling phenomenon. In contrast to dislocations, bulk ripplocations have no Burgers vector and no polarity. In graphite, ripplocations are attracted to other ripplocations, both within the same, and on adjacent layers, the latter resulting in kink boundaries. Furthermore, we present transmission electron microscopy evidence consistent with the existence of bulk ripplocations in Ti3SiC2. Ripplocations are a topological imperative, as they allow atomic layers to glide relative to each other without breaking the in-plane bonds. A more complete understanding of their mechanics and behavior is critically important, and could profoundly influence our current understanding of how graphite, layered silicates, the MAX phases, and many other plastically anisotropic/layered solids, deform and accommodate strain.

  16. Conductivities of the ionic complexes of two cyclic polyethers

    NASA Technical Reports Server (NTRS)

    Fielder, W. L.; Odonnell, P. M.

    1975-01-01

    The conductivities of the solid potassium thiocyanate complex of both dicyclohexyl-18-crown-6 and dibenzo-18-crown-6 were measured at 300K (27 C). Saturated aqueous potassium thiocyanate and graphite were used as ion-transporting and ion-blocking electrodes, respectively. The ionic conductivity predominated for both samples, but it was many orders of magnitude smaller than the value previously reported. The ionic conductivity of the dicyclohexyl complex (the better conductor) was 0.000003 ohm/cm. Crown complexes, in general, do not appear promising as potassium ion solid electrolytes contrary to claims in the patent literature.

  17. Micro-sampling method based on high-resolution continuum source graphite furnace atomic absorption spectrometry for calcium determination in blood and mitochondrial suspensions.

    PubMed

    Gómez-Nieto, Beatriz; Gismera, Mª Jesús; Sevilla, Mª Teresa; Satrústegui, Jorgina; Procopio, Jesús R

    2017-08-01

    A micro-sampling and straightforward method based on high resolution continuum source atomic absorption spectrometry (HR-CS AAS) was developed to determine extracellular and intracellular Ca in samples of interest in clinical and biomedical analysis. Solid sampling platforms were used to introduce the micro-samples into the graphite furnace atomizer. The secondary absorption line for Ca, located at 239.856nm, was selected to carry out the measurements. Experimental parameters such as pyrolysis and atomization temperatures and the amount of sample introduced for the measurements were optimized. Calibration was performed using aqueous standards and the approach to measure at the wings of the absorption lines was employed for the expansion of the linear response range. The limit of detection was of 0.02mgL -1 Ca (0.39ng Ca) and the upper limit of linear range was increased up to 8.0mgL -1 Ca (160ng Ca). The proposed method was used to determine Ca in mitochondrial suspensions and whole blood samples with successful results. Adequate recoveries (within 91-107%) were obtained in the tests performed for validation purposes. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Application of sunflower stalk-carbon nitride nanosheets as a green sorbent in the solid-phase extraction of polycyclic aromatic hydrocarbons followed by high-performance liquid chromatography.

    PubMed

    Marzi Khosrowshahi, Elnaz; Razmi, Habib

    2018-02-08

    A green biocomposite of sunflower stalks and graphitic carbon nitride nanosheets has been applied as a solid-phase extraction adsorbent for sample preparation of five polycyclic aromatic hydrocarbons in different solutions using high-performance liquid chromatography with ultraviolet detection. Before the modification, sunflower stalks exhibited relatively low adsorption to the polycyclic aromatic hydrocarbons extraction. The modified sunflower stalks showed increased adsorption to the analytes extraction due to the increase in surface and existence of a π-π interaction between the analytes and graphitic carbon nitride nanosheets on the surface. Under the optimal conditions, the limits of detection and quantification for five polycyclic aromatic hydrocarbons compounds could reach 0.4-32 and 1.2-95 ng/L, respectively. The method accuracy was evaluated using recovery measurements in spiked real samples and good recoveries from 71 to 115% with relative standard deviations of <10% have been achieved. The developed method was successfully applied for polycyclic aromatic hydrocarbons determination in various samples-well water, tap water, soil, vegetable, and barbequed meat (kebab)-with analytes contents ranging from 0.065 to 13.3 μg/L. The prepared green composite as a new sorbent has some advantages including ease of preparation, low cost, and good reusability. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Nitrogen-doped graphene by all-solid-state ball-milling graphite with urea as a high-power lithium ion battery anode

    NASA Astrophysics Data System (ADS)

    Liu, Chao; Liu, Xingang; Tan, Jiang; Wang, Qingfu; Wen, Hao; Zhang, Chuhong

    2017-02-01

    Nitrogen-doped graphene nanosheets (NGNS) are prepared by a novel mechanochemical method via all-solid-state ball-milling graphite with urea. The ball-milling process does not only successfully exfoliate the graphite into multi-layer (<10 layers) graphene nanosheets, but at the same time, enables the N element to be doped onto the graphene. Urea, acting as a new solid doping and assist-grinding agents, has the advantages of low cost and good water solubility that can simplify the fabrication process. The as-prepared NGNS are investigated in detail by XRD, SEM, HRTEM, TGA, XPS and Raman spectroscopy. The doping nitrogens are around 3.15% and dominated (>94%) by pyrindic-N and pyrrolic-N which facilitates the NGNS with enhanced electronic conductivity and Li-ion storage capability. For the first time, we demonstrate that the all-solid-state prepared NGNS exhibits, especially at high currents, enhanced cycling stability and rate capability as Lithium ion battery (LIB) anode active material when compared to pristine graphite and undoped graphene in half-cell configuration. The method presented in this article may provide a simple, clean, economical and scalable strategy for preparation of NGNS as a feasible and promising anode material for LIBs.

  20. REFRACTORY COATING FOR GRAPHITE MOLDS

    DOEpatents

    Stoddard, S.D.

    1958-06-24

    Refractory coating for graphite molds used in the casting of uranium is described. The coating is an alumino-silicate refractory composition which may be used as a mold surface in solid form or as a coating applied to the graphite mold. The composition consists of a mixture of ball clay, kaolin, alumina cement, alumina, water, sodium silicate, and sodium carbonate.

  1. Fast arsenic speciation in water by on-site solid phase extraction and high-resolution continuum source graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Mihucz, Victor G.; Bencs, László; Koncz, Kornél; Tatár, Enikő; Weiszburg, Tamás; Záray, Gyula

    2017-02-01

    A method of high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS-GFAAS), combined with on-site separation/solid phase extraction (SPE) has been developed for the speciation of inorganic As (iAs) in geothermal and drinking water samples. The HR-CS-GFAAS calibration curves were linear up to 200 μg/L As, but using second order polynomial fitting, accurate calibration could be performed up to 500 μg/L. It has been demonstrated that sample pH should not be higher than 8 for an accurate speciation of As(V) with a recovery of ≈ 95%. Geothermal water had fairly high salt content (≈ 2200 mg/L) due to the presence of chlorides and sulfates at mg/L levels. Therefore, a two-fold dilution of these types of samples before SPE is recommended, especially, for total As determinations, when the As concentration is as high as 400 μg/L. For drinking water, sampled from public wells with records of As concentrations higher than the 10 μg/L in the past, the reduction of As contamination below the WHO's health limit value could be observed. However, the electrical conductivity was close to 2500 μS/cm, i.e., the guideline limit for drinking water, which was due to their higher chloride content. The proposed fit-for-purpose SPE-HR-CS-GFAAS method could be a candidate for screening drinking water quality.

  2. Electrochemical Control of Peptide Self-Organization on Atomically Flat Solid Surfaces: A Case Study with Graphite.

    PubMed

    Seki, Takakazu; So, Christopher R; Page, Tamon R; Starkebaum, David; Hayamizu, Yuhei; Sarikaya, Mehmet

    2018-02-06

    The nanoscale self-organization of biomolecules, such as proteins and peptides, on solid surfaces under controlled conditions is an important issue in establishing functional bio/solid soft interfaces for bioassays, biosensors, and biofuel cells. Electrostatic interaction between proteins and surfaces is one of the most essential parameters in the adsorption and self-assembly of proteins on solid surfaces. Although the adsorption of proteins has been studied with respect to the electrochemical surface potential, the self-assembly of proteins or peptides forming well-organized nanostructures templated by lattice structure of the solid surfaces has not been studied in the relation to the surface potential. In this work, we utilize graphite-binding peptides (GrBPs) selected by the phage display method to investigate the relationship between the electrochemical potential of the highly ordered pyrolytic graphite (HOPG) and peptide self-organization forming long-range-ordered structures. Under modulated electrical bias, graphite-binding peptides form various ordered structures, such as well-ordered nanowires, dendritic structures, wavy wires, amorphous (disordered) structures, and islands. A systematic investigation of the correlation between peptide sequence and self-organizational characteristics reveals that the presence of the bias-sensitive amino acid modules in the peptide sequence has a significant effect on not only surface coverage but also on the morphological features of self-assembled structures. Our results show a new method to control peptide self-assembly by means of applied electrochemical bias as well as peptide design-rules for the construction of functional soft bio/solid interfaces that could be integrated in a wide range of practical implementations.

  3. Macrosegregation of GeSi Alloys Grown in a Static Magnetic Field

    NASA Technical Reports Server (NTRS)

    Ritter, T. M.; Volz, M. P.; Cobb, S. D.; Szofran, F. R.

    1999-01-01

    Axial and radial macrosegregation profiles have been determined for GeSi alloy crystals grown by the vertical Bridgman technique. An axial 5 Tesla magnetic field was applied to several samples during growth to decrease the melt velocities by means of the Lorentz force. Compositions were measured with either energy dispersive X-ray spectroscopy (EDS) on a scanning electron microscope (SEM) or by wavelength dispersive X-ray spectroscopy (WDS) on a microprobe. The crystals were processed in graphite, hot-pressed boron nitride (BN), and pyrolytic boron nitride (PBN) ampoules, which produced various solid-liquid interface shapes during solidification. Those samples grown in a graphite ampoule exhibited radial profiles consistent with a highly concave interface and axial profiles indicative of complete mixing in the melt. The samples grown in BN and PBN ampoules had less radial variation. Axial macrosegregation profiles of these samples fell between the predictions for a completely mixed melt and one where solute transport is dominated by diffusion. Possible explanations for the apparent insufficiency of the magnetic field to achieve diffusion controlled growth conditions are discussed.

  4. Pencil Graphite Electrodes: A Versatile Tool in Electroanalysis

    PubMed Central

    2017-01-01

    Due to their electrochemical and economical characteristics, pencil graphite electrodes (PGEs) gained in recent years a large applicability to the analysis of various types of inorganic and organic compounds from very different matrices. The electrode material of this type of working electrodes is constituted by the well-known and easy commercially available graphite pencil leads. Thus, PGEs are cheap and user-friendly and can be employed as disposable electrodes avoiding the time-consuming step of solid electrodes surface cleaning between measurements. When compared to other working electrodes PGEs present lower background currents, higher sensitivity, good reproducibility, and an adjustable electroactive surface area, permitting the analysis of low concentrations and small sample volumes without any deposition/preconcentration step. Therefore, this paper presents a detailed overview of the PGEs characteristics, designs and applications of bare, and electrochemically pretreated and chemically modified PGEs along with the corresponding performance characteristics like linear range and detection limit. Techniques used for bare or modified PGEs surface characterization are also reviewed. PMID:28255500

  5. The solid film lubrication by carbon ion implantation into α-Al 2O 3

    NASA Astrophysics Data System (ADS)

    Jun, Tian; Qizu, Wang; Qunji, Xue

    1998-10-01

    Improvement in tribological performance by C +110 keV implantation can be achieved by having a more graphite-like carbon structure on Al 2O 3. It was shown that fracture toughness and critical peeling load increased for a fluence of 5 × 10 17C +/cm 2 because of residual compression stress and amorphism of surface. The testing in a different implantation dose indicated that the friction and wear mechanism in Optimol fretting wear machine (SRV) was a combination of surface structure and its abrasive wear. Raman shift shows that the amorphous graphite with 5 × 10 17-1 × 10 18 C +/cm 2 implantation dose was formed on Al 2O 3 surface, so that it reduced friction coefficient and wear of Al 2O 3, also it is noticed that the failure of lubrication due to graphite-like film wear is much earlier in the implantation sample with 1 × 10 17C +/cm 2 dose.

  6. Determination of arsenic and cadmium in crude oil by direct sampling graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    de Jesus, Alexandre; Zmozinski, Ariane Vanessa; Damin, Isabel Cristina Ferreira; Silva, Márcia Messias; Vale, Maria Goreti Rodrigues

    2012-05-01

    In this work, a direct sampling graphite furnace atomic absorption spectrometry method has been developed for the determination of arsenic and cadmium in crude oil samples. The samples were weighed directly on the solid sampling platforms and introduced into the graphite tube for analysis. The chemical modifier used for both analytes was a mixture of 0.1% Pd + 0.06% Mg + 0.06% Triton X-100. Pyrolysis and atomization curves were obtained for both analytes using standards and samples. Calibration curves with aqueous standards could be used for both analytes. The limits of detection obtained were 5.1 μg kg- 1 for arsenic and 0.2 μg kg- 1 for cadmium, calculated for the maximum amount of sample that can be analyzed (8 mg and 10 mg) for arsenic and cadmium, respectively. Relative standard deviations lower than 20% were obtained. For validation purposes, a calibration curve was constructed with the SRM 1634c and aqueous standards for arsenic and the results obtained for several crude oil samples were in agreement according to paired t-test. The result obtained for the determination of arsenic in the SRM against aqueous standards was also in agreement with the certificate value. As there is no crude oil or similar reference material available with a certified value for cadmium, a digestion in an open vessel under reflux using a "cold finger" was adopted for validation purposes. The use of paired t-test showed that the results obtained by direct sampling and digestion were in agreement at a 95% confidence level. Recovery tests were carried out with inorganic and organic standards and the results were between 88% and 109%. The proposed method is simple, fast and reliable, being appropriated for routine analysis.

  7. Auger Electrons as Probes for Composite Micro- and Nano- structured Materials: Application to Solid Electrolyte Interphases in Graphite and Silicon-Graphite Electrodes

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

    Kalaga, Kaushik; Shkrob, Ilya A.; Haasch, Richard T.

    In this study, Auger electron spectroscopy (AES) combined with ion sputtering profilometry, Xray photoelectron spectroscopy (XPS), and scanning electron microscopy (SEM) have been used in a complementary fashion to examine chemical and microstructural changes in graphite (Gr) and silicon/graphite (Si/Gr) blends contained in the negative electrodes of lithium-ion cells. We demonstrate how AES can be used to characterize morphology of the solid-electrolyte interphase (SEI) deposits in such heterogeneous media, complementing well-established methods, such as XPS and SEM. In this way we demonstrate that the SEI does not consist of uniformly thick layers on the graphite and silicon; the thickness ofmore » the SEI layers in cycle-life aged electrodes follows an exponential distribution with a mean of ca. 13 nm for the graphite and ca. 20-25 nm for the silicon nanoparticles (with a crystalline core of 50-70 nm in diameter). Furthermore, a “sticky-sphere” model, in which Si nanoparticles are covered with a layer of polymer binder (that is replaced by the SEI during cycling) of variable thickness is introduced to account for the features observed.« less

  8. Auger Electrons as Probes for Composite Micro- and Nano- structured Materials: Application to Solid Electrolyte Interphases in Graphite and Silicon-Graphite Electrodes

    DOE PAGES

    Kalaga, Kaushik; Shkrob, Ilya A.; Haasch, Richard T.; ...

    2017-10-05

    In this study, Auger electron spectroscopy (AES) combined with ion sputtering profilometry, Xray photoelectron spectroscopy (XPS), and scanning electron microscopy (SEM) have been used in a complementary fashion to examine chemical and microstructural changes in graphite (Gr) and silicon/graphite (Si/Gr) blends contained in the negative electrodes of lithium-ion cells. We demonstrate how AES can be used to characterize morphology of the solid-electrolyte interphase (SEI) deposits in such heterogeneous media, complementing well-established methods, such as XPS and SEM. In this way we demonstrate that the SEI does not consist of uniformly thick layers on the graphite and silicon; the thickness ofmore » the SEI layers in cycle-life aged electrodes follows an exponential distribution with a mean of ca. 13 nm for the graphite and ca. 20-25 nm for the silicon nanoparticles (with a crystalline core of 50-70 nm in diameter). Furthermore, a “sticky-sphere” model, in which Si nanoparticles are covered with a layer of polymer binder (that is replaced by the SEI during cycling) of variable thickness is introduced to account for the features observed.« less

  9. Determination of sulphur in various vegetables by solid sampling high-resolution electrothermal molecular absorption spectrometry.

    PubMed

    Gunduz, Sema; Akman, Suleyman

    2015-04-01

    Sulphur was determined in various vegetables via molecular absorption of carbon monosulphide (CS) at 258.056 nm using a solid sampling high resolution continuum source electrothermal atomic absorption spectrometer (SS HR-CS ETAAS). Samples were dried, ground and directly introduced into the ruthenium coated graphite furnace as 0.05 to 0.50mg. All determinations were performed using palladium+citric acid modifier and applying a pyrolysis temperature of 1000 °C and a volatilisation temperature of 2400 °C. The results were in good agreement with certified sulphur concentrations of various vegetal CRM samples applying linear calibration technique prepared from thioacetamide. The limit of detection and characteristic mass of the method were 7.5 and 8.7 ng of S, respectively. The concentrations of S in various spinach, leek, lettuce, radish, Brussels sprouts, zucchini and chard samples were determined. It was showed that distribution of sulphur in CRM and grinded food samples were homogeneous even in micro-scale. Copyright © 2014 Elsevier Ltd. All rights reserved.

  10. Self-Passivating Lithium/Solid Electrolyte/Iodine Cells

    NASA Technical Reports Server (NTRS)

    Bugga, Ratnakumar; Whitcare, Jay; Narayanan, Sekharipuram; West, William

    2006-01-01

    Robust lithium/solid electrolyte/iodine electrochemical cells that offer significant advantages over commercial lithium/ iodine cells have been developed. At room temperature, these cells can be discharged at current densities 10 to 30 times those of commercial lithium/iodine cells. Moreover, from room temperature up to 80 C, the maximum discharge-current densities of these cells exceed those of all other solid-electrolyte-based cells. A cell of this type includes a metallic lithium anode in contact with a commercial flexible solid electrolyte film that, in turn, is in contact with an iodine/ graphite cathode. The solid electrolyte (the chemical composition of which has not been reported) offers the high ionic conductivity needed for high cell performance. However, the solid electrolyte exhibits an undesirable chemical reactivity to lithium that, if not mitigated, would render the solid electrolyte unsuitable for use in a lithium cell. In this cell, such mitigation is affected by the formation of a thin passivating layer of lithium iodide at the anode/electrolyte interface. Test cells of this type were fabricated from iodine/graphite cathode pellets, free-standing solid-electrolyte films, and lithium-foil anodes. The cathode mixtures were made by grinding together blends of nominally 10 weight percent graphite and 90 weight percent iodine. The cathode mixtures were then pressed into pellets at 36 kpsi (248 MPa) and inserted into coin-shaped stainless-steel cell cases that were coated with graphite paste to minimize corrosion. The solid-electrolyte film material was stamped to form circular pieces to fit in the coin cell cases, inserted in the cases, and pressed against the cathode pellets with polyethylene gaskets. Lithium-foil anodes were placed directly onto the electrolyte films. The layers described thus far were pressed and held together by stainless- steel shims, wave springs, and coin cell caps. The assembled cells were then crimped to form hermetic seals. It was found that the solid electrolyte films became discolored within seconds after they were placed in contact with the cathodes - a result of facile diffusion of iodine through the solid electrolyte material (see figure).

  11. Thermodynamic approach to the paradox of diamond formation with simultaneous graphite etching in the low pressure synthesis of diamond

    NASA Astrophysics Data System (ADS)

    Hwang, Nong M.; Yoon, Duk Y.

    1996-03-01

    In spite of the critical handicap from the thermodynamic point of view, the atomic hydrogen hypothesis is strongly supported by experimental observations of diamond deposition with simultaneous graphite etching. Thermodynamic analysis of the CH system showed that at ˜ 1500 K, carbon solubility in the gas phase is minimal and thus, the equilibrium fraction of solid carbon is maximal. Depending on whether gas phase nucleation takes place or not, the driving force is for deposition or for etching of solid carbon below ˜ 1500 K for the input gas of the typical mixture of 1% CH 499% H 2. The previous observation of etching of the graphite substrate is not expected unless solid carbon precipitated in the gas phase. By rigorous thermodynamic analysis of the previous experimental observations of diamond deposition with simultaneous graphite etching, we suggested that the previous implicit assumption that diamond deposits by an atomic unit should be the weakest point leading to the thermodynamic paradox. The experimental observations could be successfully explained without violating thermodynamics by assuming that the diamond phase had nucleated in the gas phase as fine clusters.

  12. High-temperature solid electrolyte interphases (SEI) in graphite electrodes

    NASA Astrophysics Data System (ADS)

    Rodrigues, Marco-Tulio F.; Sayed, Farheen N.; Gullapalli, Hemtej; Ajayan, Pulickel M.

    2018-03-01

    Thermal fragility of the solid electrolyte interphase (SEI) is a major source of performance decay in graphite anodes, and efforts to overcome the issues offered by extreme environments to Li-ion batteries have had limited success. Here, we demonstrate that the SEI can be extensively reinforced by carrying the formation cycles at elevated temperatures. Under these conditions, decomposition of the ionic liquid present in the electrolyte favored the formation of a thicker and more protective layer. Cells in which the solid electrolyte interphase was cast at 90 °C were significantly less prone to self-discharge when exposed to high temperature, with no obvious damages to the formed SEI. This additional resilience was accomplished at the expense of rate capability, as charge transfer became growingly inefficient in these systems. At slower rates, however, cells that underwent SEI formation at 90 °C presented superior performances, as a result of improved Li+ transport through the SEI, and optimal wetting of graphite by the electrolyte. This work analyzes different graphite hosts and ionic liquids, showing that this effect is more pervasive than anticipated, and offering the unique perspective that, for certain systems, temperature can actually be an asset for passivation.

  13. Determination of palladium, platinum and rhodium in used automobile catalysts and active pharmaceutical ingredients using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sample analysis

    NASA Astrophysics Data System (ADS)

    Resano, Martín; Flórez, María del Rosario; Queralt, Ignasi; Marguí, Eva

    2015-03-01

    This work investigates the potential of high-resolution continuum source graphite furnace atomic absorption spectrometry for the direct determination of Pd, Pt and Rh in two samples of very different nature. While analysis of active pharmaceutical ingredients is straightforward and it is feasible to minimize matrix effects, to the point that calibration can be carried out against aqueous standard solutions, the analysis of used automobile catalysts is more challenging requiring the addition of a chemical modifier (NH4F·HF) to help in releasing the analytes, a more vigorous temperature program and the use of a solid standard (CRM ERM®-EB504) for calibration. However, in both cases it was possible to obtain accurate results and precision values typically better than 10% RSD in a fast and simple way, while only two determinations are needed for the three analytes, since Pt and Rh can be simultaneously monitored in both types of samples. Overall, the methods proposed seem suited for the determination of these analytes in such types of samples, offering a greener and faster alternative that circumvents the traditional problems associated with sample digestion, requiring a small amount of sample only (0.05 mg per replicate for catalysts, and a few milligrams for the pharmaceuticals) and providing sufficient sensitivity to easily comply with regulations. The LODs achieved were 6.5 μg g- 1 (Pd), 8.3 μg g- 1 (Pt) and 9.3 μg g- 1 (Rh) for catalysts, which decreased to 0.08 μg g- 1 (Pd), 0.15 μg g- 1 (Pt) and 0.10 μg g- 1 (Rh) for pharmaceuticals.

  14. Temperature effect of friction and wear characteristics for solid lubricating graphite

    NASA Astrophysics Data System (ADS)

    Kim, Yeonwook; Kim, Jaehoon

    2015-03-01

    Graphite is one of the effective lubricant additives due to its excellent high-temperature endurance and self-lubricating properties. In this study, wear behavior of graphite used as sealing materials to cut off hot gas is evaluated at room and elevated temperature. Wear occurs on graphite seal due to the friction of driving shaft and graphite. Thus, a reciprocating wear test to evaluate the wear generated for the graphite by means of the relative motion between a shaft material and a graphite seal was carried out. The friction coefficient and specific wear rate for the changes of applied load and sliding speed were compared under different temperature conditions considering the actual operating environment. Through SEM observation of the worn surface, the lubricating film was observed and compared with test conditions.

  15. A comparison of laser ablation-inductively coupled plasma-mass spectrometry and high-resolution continuum source graphite furnace molecular absorption spectrometry for the direct determination of bromine in polymers

    NASA Astrophysics Data System (ADS)

    de Gois, Jefferson S.; Van Malderen, Stijn J. M.; Cadorim, Heloisa R.; Welz, Bernhard; Vanhaecke, Frank

    2017-06-01

    This work describes the development and comparison of two methods for the direct determination of Br in polymer samples via solid sampling, one using laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) and the other using high-resolution continuum source graphite furnace molecular absorption spectrometry with direct solid sample analysis (HR-CS SS-GF MAS). The methods were optimized and their accuracy was evaluated by comparing the results obtained for 6 polymeric certified reference materials (CRMs) with the corresponding certified values. For Br determination with LA-ICP-MS, the 79Br+ signal could be monitored interference-free. For Br determination via HR-CS SS-GF MAS, the CaBr molecule was monitored at 625.315 nm with integration of the central pixel ± 1. Bromine quantification by LA-ICP-MS was performed via external calibration against a single CRM while using the 12C+ signal as an internal standard. With HR-CS SS-GF MAS, Br quantification could be accomplished using external calibration against aqueous standard solutions. Except for one LA-ICP-MS result, the concentrations obtained with both techniques were in agreement with the certified values within the experimental uncertainty as evidenced using a t-test (95% confidence level). The limit of quantification was determined to be 100 μg g- 1 Br for LA-ICP-MS and 10 μg g- 1 Br for HR-CS SS-GF MAS.

  16. Evaluation of exposure to polycyclic aromatic hydrocarbons in a coke production and a graphite electrode manufacturing plant: assessment of urinary excretion of 1-hydroxypyrene as a biological indicator of exposure.

    PubMed Central

    Buchet, J P; Gennart, J P; Mercado-Calderon, F; Delavignette, J P; Cupers, L; Lauwerys, R

    1992-01-01

    OBJECTIVES--Characterisation of the airborne concentration of 13 polycyclic aromatic hydrocarbons (PAHs) at various workplaces in a graphite electrode and a coke production plant. Validation of the urinary excretion of 1-hydroxypyrene (hydroxypyrene) as a biological marker of exposure to PAH. DESIGN--Cross sectional study of workers exposed to PAHs (106 in the graphite electrode producing plant and 16 in the coke works). METHODS--Personal air sampling during at least six hours per workshift using a glass fibre filter and a Chromosorb 102 solid sorbent tube and analysis of PAHs by high performance liquid chromatography (HPLC) and spectrofluorometric detection (SFD). Collection of spot urine samples before and after the shift and analysis of 1-hydroxypyrene by HPLC and SFD. RESULTS--The workers most exposed to PAHs were those occupied at the topside area of the coke oven plant and those working in the blending and impregnation areas of the graphite electrode producing plant (mean airborne concentration of total PAHs: 199 and 223 micrograms/m3 respectively). Except for naphthalene and perylene, the relative proportion of the different PAHs did not differ between the plants. Pyrene concentration in air was highly correlated with the total airborne PAH concentration (r = 0.83, p < 0.0001) and the correlation coefficients between hydroxypyrene concentration in postshift urine samples and pyrene or total PAHs in air were 0.67 (p < 0.0001) and 0.72 (p < 0.0001) respectively. Excretion of hydroxypyrene doubled when the exposure to pyrene in air increased 10-fold. The half life for the urinary excretion of hydroxypyrene was around 18 hours (95% confidence interval 16.1-19.8). Smoking habits only explained 2.3% of the variance in hydroxypyrene excretion compared with 45% for the pyrene concentration in air. CONCLUSION--The determination of the urinary excretion of hydroxypyrene in postshift urine samples can be used as a suitable biomarker to assess individual exposure to PAHs in coke ovens and in graphite electrode manufacturing plants. PMID:1463676

  17. Effect of fluroine content, atmosphere, and burnishing technique on the lubricating properties of graphite fluoride

    NASA Technical Reports Server (NTRS)

    Fusaro, R. L.

    1974-01-01

    Eight different graphite fluoride compounds with fluorine to carbon ratios varying from x = 0.25 to 1.1 were evaluated as burnished films in order to determine the effect of fluorine content on the solid lubricant properties of graphite fluoride. For comparison, similar experiments were conducted on graphite burnished films. It was found that even a small amount of fluorine in graphite fluoride (CF0.25)n improved the lubricating properties of graphite. However, such factors as burnishing atmosphere, burnishing technique, test atmosphere, and specimen temperature affected the results as much as varying the fluorine to carbon ratio of the compound. Best life was found for films that were machined burnished in moist air and tested in moist air.

  18. Graphite fluoride lubrication: The effect of fluorine content, atmosphere, and burnishing technique

    NASA Technical Reports Server (NTRS)

    Fusaro, R. L.

    1975-01-01

    Eight different graphite fluoride compounds with fluorine to carbon ratios varying from x = 0.25 to 1.1 were evaluated as burnished films in order to determine the effect of fluorine content on the solid lubricant properties of graphite fluoride. For comparison, similar experiments were conducted on graphite burnished films. It was found that even a small amount of fluorine in graphite fluoride (CF sub 0.25) sub n improved the lubricating properties of graphite. Such factors as burnishing atmosphere, burnishing technique, test atmosphere, and specimen temperature affected the results as much as varying the fluorine to carbon ratio of the compound. Best life was found for films that were machine-burnished in moist air and tested in moist air.

  19. Bias-induced conformational switching of supramolecular networks of trimesic acid at the solid-liquid interface

    NASA Astrophysics Data System (ADS)

    Ubink, J.; Enache, M.; Stöhr, M.

    2018-05-01

    Using the tip of a scanning tunneling microscope, an electric field-induced reversible phase transition between two planar porous structures ("chickenwire" and "flower") of trimesic acid was accomplished at the nonanoic acid/highly oriented pyrolytic graphite interface. The chickenwire structure was exclusively observed for negative sample bias, while for positive sample bias only the more densely packed flower structure was found. We suggest that the slightly negatively charged carboxyl groups of the trimesic acid molecule are the determining factor for this observation: their adsorption behavior varies with the sample bias and is thus responsible for the switching behavior.

  20. Magnetic separation of general solid particles realised by a permanent magnet

    PubMed Central

    Hisayoshi, K.; Uyeda, C.; Terada, K.

    2016-01-01

    Most existing solids are categorised as diamagnetic or weak paramagnetic materials. The possibility of magnetic motion has not been intensively considered for these materials. Here, we demonstrate for the first time that ensembles of heterogeneous particles (diamagnetic bismuth, diamond and graphite particles, as well as two paramagnetic olivines) can be dynamically separated into five fractions by the low field produced by neodymium (NdFeB) magnets during short-duration microgravity (μg). This result is in contrast to the generally accepted notion that ordinary solid materials are magnetically inert. The materials of the separated particles are identified by their magnetic susceptibility (χ), which is determined from the translating velocity. The potential of this approach as an analytical technique is comparable to that of chromatography separation because the extraction of new solid phases from a heterogeneous grain ensemble will lead to important discoveries about inorganic materials. The method is applicable for the separation of the precious samples such as lunar soils and/or the Hayabusa particles recovered from the asteroids, because even micron-order grains can be thoroughly separated without sample-loss. PMID:27929081

  1. Magnetic separation of general solid particles realised by a permanent magnet

    NASA Astrophysics Data System (ADS)

    Hisayoshi, K.; Uyeda, C.; Terada, K.

    2016-12-01

    Most existing solids are categorised as diamagnetic or weak paramagnetic materials. The possibility of magnetic motion has not been intensively considered for these materials. Here, we demonstrate for the first time that ensembles of heterogeneous particles (diamagnetic bismuth, diamond and graphite particles, as well as two paramagnetic olivines) can be dynamically separated into five fractions by the low field produced by neodymium (NdFeB) magnets during short-duration microgravity (μg). This result is in contrast to the generally accepted notion that ordinary solid materials are magnetically inert. The materials of the separated particles are identified by their magnetic susceptibility (χ), which is determined from the translating velocity. The potential of this approach as an analytical technique is comparable to that of chromatography separation because the extraction of new solid phases from a heterogeneous grain ensemble will lead to important discoveries about inorganic materials. The method is applicable for the separation of the precious samples such as lunar soils and/or the Hayabusa particles recovered from the asteroids, because even micron-order grains can be thoroughly separated without sample-loss.

  2. Magnetic separation of general solid particles realised by a permanent magnet.

    PubMed

    Hisayoshi, K; Uyeda, C; Terada, K

    2016-12-08

    Most existing solids are categorised as diamagnetic or weak paramagnetic materials. The possibility of magnetic motion has not been intensively considered for these materials. Here, we demonstrate for the first time that ensembles of heterogeneous particles (diamagnetic bismuth, diamond and graphite particles, as well as two paramagnetic olivines) can be dynamically separated into five fractions by the low field produced by neodymium (NdFeB) magnets during short-duration microgravity (μg). This result is in contrast to the generally accepted notion that ordinary solid materials are magnetically inert. The materials of the separated particles are identified by their magnetic susceptibility (χ), which is determined from the translating velocity. The potential of this approach as an analytical technique is comparable to that of chromatography separation because the extraction of new solid phases from a heterogeneous grain ensemble will lead to important discoveries about inorganic materials. The method is applicable for the separation of the precious samples such as lunar soils and/or the Hayabusa particles recovered from the asteroids, because even micron-order grains can be thoroughly separated without sample-loss.

  3. Electrolyte volume effects on electrochemical performance and solid electrolyte interphase in Si-graphite/NMC lithium-ion pouch cells

    DOE PAGES

    An, Seong Jin; Li, Jianlin; Daniel, Claus; ...

    2017-05-15

    This study aims to explore the correlations between electrolyte volume, electrochemical performance, and properties of the solid electrolyte interphase in pouch cells with Si-graphite composite anodes. The electrolyte is 1.2 M LiPF 6 in ethylene carbonate:ethylmethyl carbonate with 10 wt.% fluoroethylene carbonate. Single layer pouch cells (100 mAh) were constructed with 15 wt.% Si-graphite/LiNi 0.5Mn 0.3CO 0.2O 2 electrodes. It is found that a minimum electrolyte volume factor of 3.1 times the total pore volume of cell components (cathode, anode, and separator) is needed for better cycling stability. Less electrolyte causes increases in ohmic and charge transfer resistances. Lithium dendritesmore » are observed when the electrolyte volume factor is low. The resistances from the anodes become significant as the cells are discharged. As a result, solid electrolyte interphase thickness grows as the electrolyte volume factor increases and is non-uniform after cycling.« less

  4. Thermophysical properties of graphite HOPG and HAPG in the solid state and under melting (from 2000 K up to 5000 K)

    NASA Astrophysics Data System (ADS)

    Savvatimskiy, A. I.; Onufriev, S. V.; Konyukhov, S. A.

    2017-11-01

    Experiments with HOPG graphite grade showed that the melting temperature of graphite equals 4800-4900 K and that the melting of graphite is possible only at elevated pressures. The data were obtained for resistivity, specific heat and input (Joule) energy up to 5000 K. HAPG (Highly Annealing Pyrolytic Graphite) is a form of highly oriented pyrolytic graphite. HAPG specimens in the form of strips (thickness 30 microns) were placed in a cell (between two plates of glass-sapphire). The specimen temperature was measured by a high speed pyrometer. The heat of fusion for both graphite grades (heated in a confined volume) was less (and specific heat - higher) than for the case with nearly free expansion. A possible reason for the observed effects is discussed in the report.

  5. High purity polyimide analysis by solid sampling graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Santos, Rafael F.; Carvalho, Gabriel S.; Duarte, Fabio A.; Bolzan, Rodrigo C.; Flores, Erico M. M.

    2017-03-01

    In this work, Cr, Cu, Mn, Na and Ni were determined in high purity polyimides (99.5%) by solid sampling graphite furnace atomic absorption spectrometry (SS-GFAAS) using Zeeman effect background correction system with variable magnetic field, making possible the simultaneous measurement at high or low sensitivity. The following analytical parameters were evaluated: pyrolysis and atomization temperatures, feasibility of calibration with aqueous solution, linear calibration range, sample mass range and the use of chemical modifier. Calibration with aqueous standard solutions was feasible for all analytes. No under or overestimated results were observed and up to 10 mg sample could be introduced on the platform for the determination of Cr, Cu, Mn, Na and Ni. The relative standard deviation ranged from 3 to 20%. The limits of detection (LODs) achieved using the high sensitivity mode were as low as 7.0, 2.5, 1.7, 17 and 0.12 ng g- 1 for Cr, Cu, Mn, Na and Ni, respectively. No addition of chemical modifier was necessary, except for Mn determination where Pd was required. The accuracy was evaluated by analyte spike and by comparison of the results with those obtained by inductively coupled plasma optical emission spectrometry and inductively coupled plasma mass spectrometry after microwave-assisted digestion in a single reaction chamber system and also by neutron activation analysis. No difference among the results obtained by SS-GFAAS and those obtained by alternative analytical methods using independent techniques. SS-GFAAS method showed some advantages, such as the determination of metallic contaminants in high purity polyimides with practically no sample preparation, very low LODs, calibration with aqueous standards and determination in a wide range of concentration.

  6. Determination of cadmium in coal using solid sampling graphite furnace high-resolution continuum source atomic absorption spectrometry.

    PubMed

    da Silva, Alessandra Furtado; Borges, Daniel L G; Lepri, Fábio Grandis; Welz, Bernhard; Curtius, Adilson J; Heitmann, Uwe

    2005-08-01

    This work describes the development of a method to determine cadmium in coal, in which iridium is used as a permanent chemical modifier and calibration is performed against aqueous standards by high-resolution continuum source atomic absorption spectrometry (HR-CS AAS). This new instrumental concept makes the whole spectral environment in the vicinity of the analytical line accessible, providing a lot more data than just the change in absorbance over time available from conventional instruments. The application of Ir (400 microg) as a permanent chemical modifier, thermally deposited on the pyrolytic graphite platform surface, allowed pyrolysis temperatures of 700 degrees C to be used, which was sufficiently high to significantly reduce the continuous background that occurred before the analyte signal at pyrolysis temperatures <700 degrees C. Structured background absorption also occurred after the analyte signal when atomization temperatures of >1600 degrees C were used, which arose from the electron-excitation spectrum (with rotational fine structure) of a diatomic molecule. Under optimized conditions (pyrolysis at 700 degrees C and atomization at 1500 degrees C), interference-free determination of cadmium in seven certified coal reference materials and two real samples was achieved by direct solid sampling and calibrating against aqueous standards, resulting in good agreement with the certified values (where available) at the 95% confidence level. A characteristic mass of 0.4 pg and a detection limit of 2 ng g(-1), calculated for a sample mass of 1.0 mg coal, was obtained. A precision (expressed as the relative standard deviation, RSD) of <10% was typically obtained when coal samples in the mass range 0.6-1.2 mg were analyzed.

  7. Cobalt internal standard for Ni to assist the simultaneous determination of Mo and Ni in plant materials by high-resolution continuum source graphite furnace atomic absorption spectrometry employing direct solid sample analysis.

    PubMed

    de Babos, Diego Victor; Bechlin, Marcos André; Barros, Ariane Isis; Ferreira, Edilene Cristina; Gomes Neto, José Anchieta; de Oliveira, Silvana Ruella

    2016-05-15

    A new method is proposed for the simultaneous determination of Mo and Ni in plant materials by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GFAAS), employing direct solid sample analysis (DSS) and internal standardization (IS). Cobalt was used as internal standard to minimize matrix effects during Ni determinations, enabling the use of aqueous standards for calibration. Correlation coefficients for the calibration curves were typically better than 0.9937. The performance of the method was checked by analysis of six plant certified reference materials, and the results for Mo and Ni were in agreement with the certified values (95% confidence level, t-test). Analysis was made of different types of plant materials used as renewable sources of energy, including sugarcane leaves, banana tree fiber, soybean straw, coffee pods, orange bagasse, peanut hulls, and sugarcane bagasse. The concentrations found for Mo and Ni ranged from 0.08 to 0.63 ng mg(-1) and from 0.41 to 6.92 ng mg(-1), respectively. Precision (RSD) varied from 2.1% to 11% for Mo and from 3.7% to 10% for Ni. Limits of quantification of 0.055 and 0.074 ng were obtained for Mo and Ni, respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. Solid-phase extraction of polar pesticides from environmental water samples on graphitized carbon and Empore-activated carbon disks and on-line coupling to octadecyl-bonded silica analytical columns.

    PubMed

    Slobodník, J; Oztezkizan, O; Lingeman, H; Brinkman, U A

    1996-10-25

    The suitability of Empore-activated carbon disks (EACD), Envi-Carb graphitized carbon black (GCB) and CPP-50 graphitized carbon for the trace enrichment of polar pesticides from water samples was studied by means of off-line and on-line solid-phase extraction (SPE). In the off-line procedure, 0.5-2 l samples spiked with a test mixture of oxamyl, methomyl and aldicarb sulfoxide were enriched on EnviCarb SPE cartridges or 47 mm diameter EACD and eluted with dichloromethane-methanol. After evaporation, a sample was injected onto a C18-bonded silica column and analysed by liquid chromatography with ultraviolet (LC-UV) detection. EACD performed better than EnviCarb cartridges in terms of breakthrough volumes (> 2 l for all test analytes), reproducibility (R.S.D. of recoveries, 4-8%, n = 3) and sampling speed (100 ml/min); detection limits in drinking water were 0.05-0.16 microgram/l. In the on-line experiments, 4.6 mm diameter pieces cut from original EACD and stacked onto each other in a 9 mm long precolumn, and EnviCarb and CPP-50 packed in 10 x 2.0 mm I.D. precolumn, were tested, and 50-200 ml spiked water samples were preconcentrated. Because of the peak broadening caused by the strong sorption of the analytes on carbon, the carbon-packed precolumns were eluted by a separate stream of 0.1 ml/min acetonitrile which was mixed with the gradient LC eluent in front of the C18 analytical column. The final on-line procedure was also applied for the less polar propoxur, carbaryl and methiocarb. EnviCarb could not be used due to its poor pressure resistance. CPP-50 provided less peak broadening than EACD: peak widths were 0.1-0.3 min and R.S.D. of peak heights 4-14% (n = 3). In terms of analyte trapping efficiency on-line SPE-LC-UV with a CPP-50 precolumn also showed better performance than when Bondesil C18/OH or polymeric PLRP-S was used, but chromatographic resolution was similar. With the CPP-50-based system, detection limits of the test compounds were 0.05-1 microgram/l in surface water.

  9. Measurements of slip length for flows over graphite surface with gas domains

    NASA Astrophysics Data System (ADS)

    Li, Dayong; Wang, Yuliang; Pan, Yunlu; Zhao, Xuezeng

    2016-10-01

    We present the measurements of slip lengths for the flows of purified water over graphite surface covered with surface nanobubbles or nano/micropancakes, which can be produced after using high temperature water to replace low temperature water. The slip length values measured on bare graphite surface, nano/micropancake or nanobubble covered graphite surfaces are about 8 nm, 27 nm, and 63 nm, respectively. Our results indicate that the gaseous domains formed at the solid-liquid interface, including surface nanobubbles and nano/micropancakes, could act as a lubricant and significantly increase slip length.

  10. Interface structure between tetraglyme and graphite

    NASA Astrophysics Data System (ADS)

    Minato, Taketoshi; Araki, Yuki; Umeda, Kenichi; Yamanaka, Toshiro; Okazaki, Ken-ichi; Onishi, Hiroshi; Abe, Takeshi; Ogumi, Zempachi

    2017-09-01

    Clarification of the details of the interface structure between liquids and solids is crucial for understanding the fundamental processes of physical functions. Herein, we investigate the structure of the interface between tetraglyme and graphite and propose a model for the interface structure based on the observation of frequency-modulation atomic force microscopy in liquids. The ordering and distorted adsorption of tetraglyme on graphite were observed. It is found that tetraglyme stably adsorbs on graphite. Density functional theory calculations supported the adsorption structure. In the liquid phase, there is a layered structure of the molecular distribution with an average distance of 0.60 nm between layers.

  11. Enhanced performance of graphite anode materials by AlF3 coating for lithium-ion batteries

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

    Ding, Fei; Xu, Wu; Choi, Daiwon

    2012-04-27

    In order to form the stable surface film and to further enhance the long-term cycling stability of the graphite anodes of lithium-ion batteries, the surface of graphite powders has been modified by AlF3 coating through chemical precipitation method. The AlF3-coated graphite shows no evident changes in the bulk structure and a thin AlF3-coating layer of about 2 nm thick is found to uniformly cover the graphite particles with 2 wt% AlF3 content. However, it delivers a higher initial discharge capacity and largely improved rate performances compared to the pristine graphite. Remarkably, AlF3 coated graphite demonstrated a much better cycle life.more » After 300 cycles, AlF3 coated graphite and uncoated graphite show capacity retention of 92% and 81%, respectively. XPS measurement shows that a more conductive solid electrode interface (SEI) layer was formed on AlF3 coated graphite as compared to uncoated graphite. SEM monograph also reveals that the AlF3-coated graphite particles have a much more stable surface morphology after long-term cycling. Therefore, the improved electrochemical performance of AlF3 coated graphite can be attributed to a more stable and conductive SEI formed on coated graphite anode during cycling process.« less

  12. The Physics and Chemistry of carbides, Nitrides and Borides. Volume 185

    DTIC Science & Technology

    1990-01-01

    and C-B-C chains [15,17]. Clearly, the use of boron-rich solids as electronic materials will place new demands on the quality of materials. In this...first heated in a pyrolytic boron nitride (PBN) crucible ( Union Carbide Corp.) under high vacuum (< 50 mTorr) to 1900°C. This removed surface...contamination of the sample. The powders were loaded into a graphite die with a high-purity BN die liner ( Union Carbide Grade HBC) with inner diameter of 3/8

  13. Influence of Applied Thermal Gradients and a Static Magnetic Field on Bridgman-Grown GeSi Alloys

    NASA Technical Reports Server (NTRS)

    Volz, M. P.; Szofran, F. R.; Cobb, S. D.; Ritter, T. M.

    1999-01-01

    The effect of applied axial and radial thermal gradients and an axial static magnetic field on the macrosegregation profiles of Bridgman-grown GeSi alloy crystals has been assessed. The axial thermal gradients were adjusted by changing the control setpoints of a seven-zone vertical Bridgman furnace. The radial thermal gradients were affected by growing samples in ampoules with different thermal conductivities, namely graphite, hot-pressed boron nitride (BN), and pyrolytic boron nitride (PBN). Those samples grown in a graphite ampoule exhibited radial profiles consistent with a highly concave interface and axial profiles indicative of complete mixing in the melt. The samples grown in BN and PBN ampoules had less radial variation. Axial macrosegregation profiles of these samples fell between the predictions for a completely mixed melt and one where solute transport is dominated by diffusion. All of the samples were grown on Ge seeds. This resulted in a period of free growth until the Si concentration in the solid was in equilibrium with the Si concentration in the liquid. The length of crystal grown during this period was inversely proportional to the applied axial thermal gradient. Several samples were grown in an axial 5 Tesla magnetic field. Measured macroscopic segregation profiles on these samples indicate that the magnetic field did not, in general, reduce the melt flow velocities to below the growth velocities.

  14. Non-destructive control of graphite electrodes with use of current displacement effect

    NASA Astrophysics Data System (ADS)

    Myatezh, A. V.; Malozyomov, B. V.; Smirnov, M. A.

    2017-10-01

    The work is devoted to methods of nondestructive diagnostics and their use for solving the problem of diagnosing various defects in solid surface of graphite electrodes used in steelmaking furnaces. Various non-destructive control methods of materials are analyzed. In the article, methods of eddy-current defectoscopy of graphite electrodes are considered. Rationalization of the sensitivity increase of the method and localization of damage is described. Imitating modeling of electromagnetic processes was executed; results were made and conclusions were drawn.

  15. Compressive strength of damaged and repaired composite plates

    NASA Technical Reports Server (NTRS)

    Finn, Scott R.; He, Yi-Fei; Springer, George S.; Lee, Hung-Joo

    1992-01-01

    Tests were performed assessing the effectiveness of repair in restoring the mechanical properties of damaged, solid composite plates made either of Fiberite T300/976 graphite-epoxy, Fiberite IM7/977-2 graphite-toughened epoxy, or ICI APC-2 graphite-PEEK. The plate length, the layup and the amount of damage were also varied. Damage was introduced in the plates either by impacting them with a solid projectile or by applying a transverse static load. Some (75 percent) or all (100 percent) of the damaged zone was then cut out, and the plate was repaired by plugging and patching the hole. The effectiveness of the repair was evaluated by measuring the compressive strengths of undamaged plates, damaged plates with no cutout, damaged plates with a cutout, and repaired plates. The data at an intermediate stage of repair provide information on the effect of each repair step on the compressive strength. The results indicated that for the solid plates used in these tests, the repair methods used herein did not improve the compressive strength of already damaged plates.

  16. Oxygen Buffering in High Pressure Solid Media Assemblies: New Approach Enabling Study of fO2 from IW-4 to IW+4.5

    NASA Technical Reports Server (NTRS)

    Righter, K.; Pando, K. M.; Ross, D. K.; Butterworth, A. L.; Gainsforth, Z.; Jilly-Rehak, C. E.; Westphal, A. J.

    2017-01-01

    Oxygen fugacity is an intensive parameter that controls some fundamental chemical and physical properties in planetary materials. In terrestrial magmas high fO2 promotes magnetite stability and low fO2 causes Fe-enrichment due to magnetite suppression. In lunar and asteroidal basalts, low fO2 can allow metal to be stable. Experimental studies will therefore be most useful if they are done at a specific and relevant fO2 for the samples under consideration. Control of fO2 in the solid media apparatus (piston cylinder multi-anvil) has relied on either sliding sensors or graphite capsule buffering, which are of limited application to the wide range of fO2 recorded in planetary or astromaterials. Here we describe a new approach that allows fO2 to be specified across a wide range of values relevant to natural samples.

  17. Tris(trimethylsilyl) Phosphite as an Efficient Electrolyte Additive To Improve the Surface Stability of Graphite Anodes.

    PubMed

    Yim, Taeeun; Han, Young-Kyu

    2017-09-27

    Tris(trimethylsilyl) phosphite (TMSP) has received considerable attention as a functional additive for various cathode materials in lithium-ion batteries, but the effect of TMSP on the surface stability of a graphite anode has not been studied. Herein, we demonstrate that TMSP serves as an effective solid electrolyte interphase (SEI)-forming additive for graphite anodes in lithium-ion batteries (LIBs). TMSP forms SEI layers by chemical reactions between TMSP and a reductively decomposed ethylene carbonate (EC) anion, which is strikingly different from the widely known mechanism of the SEI-forming additives. TMSP is stable under cathodic polarization, but it reacts chemically with radical anion intermediates derived from the electrochemical reduction of the carbonate solvents to generate a stable SEI layer. These TMSP-derived SEI layers improve the interfacial stability of the graphite anode, resulting in a retention of 96.8% and a high Coulombic efficiency of 95.2%. We suggest the use of TMSP as a functional additive that effectively stabilizes solid electrolyte interfaces of both the anode and cathode in lithium-ion batteries.

  18. Speciation of As(III) and As(V) in water samples by graphite furnace atomic absorption spectrometry after solid phase extraction combined with dispersive liquid-liquid microextraction based on the solidification of floating organic drop.

    PubMed

    Shamsipur, Mojtaba; Fattahi, Nazir; Assadi, Yaghoub; Sadeghi, Marzieh; Sharafi, Kiomars

    2014-12-01

    A solid phase extraction (SPE) coupled with dispersive liquid-liquid microextraction based on the solidification of floating organic drop (DLLME-SFO) method, using diethyldithiphosphate (DDTP) as a proper chelating agent, has been developed as an ultra preconcentration technique for the determination of inorganic arsenic in water samples prior to graphite furnace atomic absorption spectrometry (GFAAS). Variables affecting the performance of both steps were thoroughly investigated. Under optimized conditions, 100mL of As(ΙΙΙ) solution was first concentrated using a solid phase sorbent. The extract was collected in 2.0 mL of acetone and 60.0 µL of 1-undecanol was added into the collecting solvent. The mixture was then injected rapidly into 5.0 mL of pure water for further DLLME-SFO. Total inorganic As(III, V) was extracted similarly after reduction of As(V) to As(III) with potassium iodide and sodium thiosulfate and As(V) concentration was calculated by difference. A mixture of Pd(NO3)2 and Mg(NO3)2 was used as a chemical modifier in GFAAS. The analytical characteristics of the method were determined. The calibration graph was linear in the rage of 10-100 ng L(-1) with detection limit of 2.5 ng L(-1). Repeatability (intra-day) and reproducibility (inter-day) of method based on seven replicate measurements of 80 ng L(-1) of As(ΙΙΙ) were 6.8% and 7.5%, respectively. The method was successfully applied to speciation of As(III), As(V) and determination of the total amount of As in water samples and in a certified reference material (NIST RSM 1643e). Copyright © 2014 Elsevier B.V. All rights reserved.

  19. Nucleation and Growth of Graphite in Eutectic Spheroidal Cast Iron: Modeling and Testing

    NASA Astrophysics Data System (ADS)

    Carazo, Fernando D.; Dardati, Patricia M.; Celentano, Diego J.; Godoy, Luis A.

    2016-06-01

    A new model of graphite growth during the continuous cooling of eutectic spheroidal cast iron is presented in this paper. The model considers the nucleation and growth of graphite from pouring to room temperature. The microstructural model of solidification accounts for the eutectic as divorced and graphite growth rate as a function of carbon gradient at the liquid in contact with the graphite. In the solid state, the microstructural model takes into account three stages for graphite growth, namely (1) from the end of solidification to the upper bound of intercritical stable eutectoid, (2) during the intercritical stable eutectoid, and (3) from the lower bound of intercritical stable eutectoid to room temperature. The micro- and macrostructural models are coupled using a sequential multiscale approach. Numerical results for graphite fraction and size distribution are compared with experimental results obtained from a cylindrical cup, in which the graphite volumetric fraction and size distribution were obtained using the Schwartz-Saltykov approach. The agreements between the experimental and numerical results for the fraction of graphite and the size distribution of spheroids reveal the importance of numerical models in the prediction of the main aspects of graphite in spheroidal cast iron.

  20. Improved modeling of two-dimensional transitions in dense phases on crystalline surfaces. Krypton–graphite system

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

    Ustinov, E. A., E-mail: eustinov@mail.wplus.net

    This paper presents a refined technique to describe two-dimensional phase transitions in dense fluids adsorbed on a crystalline surface. Prediction of parameters of 2D liquid–solid equilibrium is known to be an extremely challenging problem, which is mainly due to a small difference in thermodynamic functions of coexisting phases and lack of accuracy of numerical experiments in case of their high density. This is a serious limitation of various attempts to circumvent this problem. To improve this situation, a new methodology based on the kinetic Monte Carlo method was applied. The methodology involves analysis of equilibrium gas–liquid and gas–solid systems undergoingmore » an external potential, which allows gradual shifting parameters of the phase coexistence. The interrelation of the chemical potential and tangential pressure for each system is then treated with the Gibbs–Duhem equation to obtain the point of intersection corresponding to the liquid/solid–solid equilibrium coexistence. The methodology is demonstrated on the krypton–graphite system below and above the 2D critical temperature. Using experimental data on the liquid–solid and the commensurate–incommensurate transitions in the krypton monolayer derived from adsorption isotherms, the Kr–graphite Lennard–Jones parameters have been corrected resulting in a higher periodic potential modulation.« less

  1. Structure of spontaneously formed solid-electrolyte interphase on lithiated graphite determined using small-angle neutron scattering

    DOE PAGES

    Sacci, Robert L.; Banuelos, Jose Leobardo; Veith, Gabriel M.; ...

    2015-03-25

    We report the first small-angle neutron scattering of a chemically formed solid-electrolyte interphase from LixC6 reacting with ethylene carbonate/dimethyl carbon solvent. This provides a different and perhaps simpler view of SEI formation than the usual electrochemically-driven reaction. We show that an organic layer coats the graphite particles filling in micro-pores and is polymeric in nature being 1-3 nm thick. We used inelastic neutron scattering to probe the chemistry, and we found that the SEI showed similar inelastic scattering to polyethylene oxide.

  2. Effects of Stone-Wales and vacancy defects in atomic-scale friction on defective graphite

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

    Sun, Xiao-Yu; Key Laboratory of Hubei Province for Water Jet Theory and New Technology, Wuhan University, Wuhan 430072; Wu, RunNi

    2014-05-05

    Graphite is an excellent solid lubricant for surface coating, but its performance is significantly weakened by the vacancy or Stone-Wales (SW) defect. This study uses molecular dynamics simulations to explore the frictional behavior of a diamond tip sliding over a graphite which contains a single defect or stacked defects. Our results suggest that the friction on defective graphite shows a strong dependence on defect location and type. The 5-7-7-5 structure of SW defect results in an effectively negative slope of friction. For defective graphite containing a defect in the surface, adding a single vacancy in the interior layer will decreasemore » the friction coefficients, while setting a SW defect in the interior layer may increase the friction coefficients. Our obtained results may provide useful information for understanding the atomic-scale friction properties of defective graphite.« less

  3. Co-solvents with high coulombic efficiency in propylene carbonate based electrolytes

    DOEpatents

    Liu, Gao; Zhao, Hui; Park, Sang-Jae

    2017-06-27

    A homologous series of cyclic carbonate or propylene carbonate (PC) analogue solvents with increasing length of linear alkyl substitutes were synthesized and used as co-solvents with PC for graphite based lithium ion half cells. A graphite anode reaches a capacity around 310 mAh/g in PC and its analogue co-solvents with 99.95% Coulombic efficiency. Cyclic carbonate co-solvents with longer alkyl chains are able to prevent exfoliation of graphite when used as co-solvents with PC. The cyclic carbonate co-solvents of PC compete for solvation of Li ion with PC solvent, delaying PC co-intercalation. Reduction products of PC on graphite surfaces via single-electron path form a stable Solid Electrolyte Interphase (SEI), which allows the reversible cycling of graphite.

  4. Phase Structures and Magnetic Properties of Graphite Nanosheets and Ni-Graphite Nanocomposite Synthesized by Electrical Explosion of Wire in Liquid

    NASA Astrophysics Data System (ADS)

    Nguyen, Minh-Thuyet; Kim, Jin-Hyung; Lee, Jung-Goo; Kim, Jin-Chun

    2018-03-01

    The present work studied on phases and magnetic properties of graphite nanosheets and Ni-graphite nanocomposite synthesized using the electrical explosion of wire (EEW) in ethanol. X-ray diffraction and field emission scanning electron microscope were used to investigate the phases and the morphology of the nanopowders obtained. It was found that graphite nanosheets were absolutely fabricated by EEW with a thickness of 29 nm and 3 μm diameter. The as-synthesized Ni-graphite composite powders had a Ni-coating on the surfaces of graphite sheets. The hysteresis loop of the as-exploded, the hydrogen-treated composite nanopowders and the sintered samples were examined with a vibrating sample magnetometer at room temperature. The Ni-graphite composite exposed the magnetic behaviors which are attributed to Ni component. The magnetic properties of composite had the improvement from 10.2 emu/g for the as-exploded powders to 15.8 emu/g for heat-treated powders and 49.16 emu/g for sintered samples.

  5. The influence of buoyant forces and volume fraction of particles on the particle pushing/entrapment transition during directional solidification of Al/SiC and Al/graphite composites

    NASA Technical Reports Server (NTRS)

    Stefanescu, Doru M.; Moitra, Avijit; Kacar, A. Sedat; Dhindaw, Brij K.

    1990-01-01

    Directional solidification experiments in a Bridgman-type furnace were used to study particle behavior at the liquid/solid interface in aluminum metal matrix composites. Graphite or silicon-carbide particles were first dispersed in aluminum-base alloys via a mechanically stirred vortex. Then, 100-mm-diameter and 120-mm-long samples were cast in steel dies and used for directional solidification. The processing variables controlled were the direction and velocity of solidification and the temperature gradient at the interface. The material variables monitored were the interface energy, the liquid/particle density difference, the particle/liquid thermal conductivity ratio, and the volume fraction of particles. These properties were changed by selecting combinations of particles (graphite or silicon carbide) and alloys (Al-Cu, Al-Mg, Al-Ni). A model which consideres process thermodynamics, process kinetics (including the role of buoyant forces), and thermophysical properties was developed. Based on solidification direction and velocity, and on materials properties, four types of behavior were predicted. Sessile drop experiments were also used to determine some of the interface energies required in calculation with the proposed model. Experimental results compared favorably with model predictions.

  6. The influence of buoyant forces and volume fraction of particles on the particle pushing/entrapment transition during directional solidification of Al/SiC and Al/graphite composites

    NASA Astrophysics Data System (ADS)

    Stefanescu, Doru M.; Moitra, Avijit; Kacar, A. Sedat; Dhindaw, Brij K.

    1990-01-01

    Directional solidification experiments in a Bridgman-type furnace were used to study particle behavior at the liquid/solid interface in aluminum metal matrix composites. Graphite or siliconcarbide particles were first dispersed in aluminum-base alloys via a mechanically stirred vortex. Then, 100-mm-diameter and 120-mm-long samples were cast in steel dies and used for directional solidification. The processing variables controlled were the direction and velocity of solidification and the temperature gradient at the interface. The material variables monitored were the interface energy, the liquid/particle density difference, the particle/liquid thermal conductivity ratio, and the volume fraction of particles. These properties were changed by selecting combinations of particles (graphite or silicon carbide) and alloys (Al-Cu, Al-Mg, Al-Ni). A model which considers process thermodynamics, process kinetics (including the role of buoyant forces), and thermophysical properties was developed. Based on solidification direction and velocity, and on materials properties, four types of behavior were predicted. Sessile drop experiments were also used to determine some of the interface energies required in calculation with the proposed model. Experimental results compared favorably with model predictions.

  7. Determination of the Tribological Fundamentals of Solid Lubricated Ceramics. Volume 1. Summary

    DTIC Science & Technology

    1990-11-01

    the length of the C-axis), leading to increased critical resolved shear stress/surface shear strength of the polycrystalline graphite and...weaker nature of the graphitic regions. Wear rates of pure, polycrystalline diamond range from -4 x 10- 16 m 3/N • m in vacuum to I x 10ൗ m3/N• m...Intercalated Graphite Molds. Triboflats hand-cut, oc-SiC paper- san !ed and fine diamond paper-polished from NiCI2/ HOPG and CdCl2/ HOPG (to remove the outer 0.5

  8. Graphite furnace atomic absorption spectrometric detection of vanadium in water and food samples after solid phase extraction on multiwalled carbon nanotubes.

    PubMed

    Wadhwa, Sham Kumar; Tuzen, Mustafa; Gul Kazi, Tasneem; Soylak, Mustafa

    2013-11-15

    Vanadium(V) ions as 8-hydroxyquinoline chelates were loaded on multiwalled carbon nanotubes (MWNTs) in a mini chromatographic column. Vanadium was determined by graphite furnace atomic absorption spectrometry (GFAAS). Various analytical parameters including pH of the working solutions, amounts of 8-hydroxyquinoline, eluent type, sample volume, and flow rates were investigated. The effects of matrix ions and some transition metals were also studied. The column can be reused 250 times without any loss in its sorption properties. The preconcentration factor was found as 100. Detection limit (3 s) and limit of quantification (10 s) for the vanadium in the optimal conditions were observed to be 0.012 µg L(-1) and 0.040 μg L(-1), respectively. The capacity of adsorption was 9.6 mg g(-1). Relative standard deviation (RSD) was found to be 5%. The validation of the method was confirmed by using NIST SRM 1515 Apple leaves, NIST SRM 1570a Spinach leaves and GBW 07605 Tea certified reference materials. The procedure was applied to the determination of vanadium in tap water and bottled drinking water samples. The procedure was also successfully applied to microwave digested food samples including black tea, coffee, tomato, cabbage, zucchini, apple and chicken samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  9. Synthesis of graphene nanoribbons from amyloid templates by gallium vapor-assisted solid-phase graphitization

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

    Murakami, Katsuhisa, E-mail: k.murakami@bk.tsukuba.ac.jp; Dong, Tianchen; Kajiwara, Yuya

    2014-06-16

    Single- and double-layer graphene nanoribbons (GNRs) with widths of around 10 nm were synthesized directly onto an insulating substrate by solid-phase graphitization using a gallium vapor catalyst and carbon templates made of amyloid fibrils. Subsequent investigation revealed that the crystallinity, conductivity, and carrier mobility were all improved by increasing the temperature of synthesis. The carrier mobility of the GNR synthesized at 1050 °C was 0.83 cm{sup 2}/V s, which is lower than that of mechanically exfoliated graphene. This is considered to be most likely due to electron scattering by the defects and edges of the GNRs.

  10. In situ polymerization of monomers for polyphenylquinoxaline/graphite

    NASA Technical Reports Server (NTRS)

    Serafini, T. T.; Delvigs, P.; Vannucci, R. D.

    1973-01-01

    Methods currently used to prepare fiber reinforced, high temperature resistant polyphenylquinoxaline (PPQ) composites employ extremely viscous, low solids content solutions of high molecular weight PPQ polymers. An improved approach, described in this report, consists of impregnating the fiber with a solution of the appropriate monomers instead of a solution of previously synthesized high molecular weight polymer. Polymerization of the monomers occurs in situ on the fiber during the solvent removal and curing stages. The in situ polymerization approach greatly simplifies the fabrication of PPQ graphite fiber composites. The use of low viscosity monomeric type solutions facilitates fiber wetting, permits a high solids content, and eliminates the need for prior polymer synthesis.

  11. Use of a heated graphite scrubber as a means of reducing interferences in UV-absorbance measurements of atmospheric ozone

    NASA Astrophysics Data System (ADS)

    Turnipseed, Andrew A.; Andersen, Peter C.; Williford, Craig J.; Ennis, Christine A.; Birks, John W.

    2017-06-01

    A new solid-phase scrubber for use in conventional ozone (O3) photometers was investigated as a means of reducing interferences from other UV-absorbing species and water vapor. It was found that when heated to 100-130 °C, a tubular graphite scrubber efficiently removed up to 500 ppb ozone and ozone monitors using the heated graphite scrubber were found to be less susceptible to interferences from water vapor, mercury vapor, and aromatic volatile organic compounds (VOCs) compared to conventional metal oxide scrubbers. Ambient measurements from a graphite scrubber-equipped photometer and a co-located Federal equivalent method (FEM) ozone analyzer showed excellent agreement over 38 days of measurements and indicated no loss in the scrubber's ability to remove ozone when operated at 130 °C. The use of a heated graphite scrubber was found to reduce the interference from mercury vapor to ≤ 3 % of that obtained using a packed-bed Hopcalite scrubber. For a series of substituted aromatic compounds (ranging in volatility and absorption cross section at 253.7 nm), the graphite scrubber was observed to consistently exhibit reduced levels of interference, typically by factors of 2.5 to 20 less than with Hopcalite. Conventional solid-phase scrubbers also exhibited complex VOC adsorption and desorption characteristics that were dependent upon the relative humidity (RH), volatility of the VOC, and the available surface area of the scrubber. This complex behavior involving humidity is avoided by use of a heated graphite scrubber. These results suggest that heated graphite scrubbers could be substituted in most ozone photometers as a means of reducing interferences from other UV-absorbing species found in the atmosphere. This could be particularly important in ozone monitoring for compliance with the United States (U.S.) Clean Air Act or for use in VOC-rich environments such as in smog chambers and monitoring indoor air quality.

  12. Preparation and characterization of hierarchical porous carbons derived from solid leather waste for supercapacitor applications.

    PubMed

    Konikkara, Niketha; Kennedy, L John; Vijaya, J Judith

    2016-11-15

    Utilization of crust leather waste (CLW) as precursors for the preparation of hierarchical porous carbons (HPC) were investigated. HPCs were prepared from CLW by pre-carbonization followed by chemical activation using KOH at relatively high temperatures. Textural properties of HPC's showed an extent of micro-and mesoporosity with maximum BET surface area of 716m(2)/g. Inducements of graphitic planes in leather waste derived carbons were observed from X-ray diffraction and HR-TEM analysis. Microstructure, thermal behavior and surface functional groups were identified using FT-Raman, thermo gravimetric analysis and FT-IR techniques. HPCs were evaluated for electrochemical properties by cyclic voltammetry (CV), galvanostatic charge/discharge (GCD) and electrochemical impedance spectroscopy (EIS) by three electrode system. CLC9 sample showed a maximum capacitance of 1960F/g in 1M KCl electrolyte. Results achieved from rectangular curves of CV, GCD symmetric curves and Nyquist plots show that the leather waste carbon is suitable to fabricate supercapacitors as it possess high specific capacitance and electrochemical cycle stability. The present study proposes an effective method for solid waste management in leather industry by the way of converting toxic leather waste to new graphitic porous carbonaceous materials as a potential candidate for energy storage devices. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Electrochemical treatment of evaporated residue of soak liquor generated from leather industry.

    PubMed

    Boopathy, R; Sekaran, G

    2013-09-15

    The organic and suspended solids present in soak liquor, generated from leather industry, demands treatment. The soak liquor is being segregated and evaporated in solar evaporation pans/multiple effect evaporator due to non availability of viable technology for its treatment. The residue left behind in the pans/evaporator does not carry any reuse value and also faces disposal threat due to the presence of high concentration of sodium chloride, organic and bacterial impurities. In the present investigation, the aqueous evaporated residue of soak liquor (ERSL) was treated by electrochemical oxidation. Graphite/graphite and SS304/graphite systems were used in electrochemical oxidation of organics in ERSL. Among these, graphite/graphite system was found to be effective over SS304/graphite system. Hence, the optimised conditions for the electrochemical oxidation of organics in ERSL using graphite/graphite system was evaluated by response surface methodology (RSM). The mass transport coefficient (km) was calculated based on pseudo-first order rate kinetics for both the electrode systems (graphite/graphite and SS304/graphite). The thermodynamic properties illustrated the electrochemical oxidation was exothermic and non-spontaneous in nature. The calculated specific energy consumption at the optimum current density of 50 mA cm(-2) was 0.41 kWh m(-3) for the removal of COD and 2.57 kWh m(-3) for the removal of TKN. Copyright © 2013 Elsevier B.V. All rights reserved.

  14. A new mass spectrometer system for investigating laser-induced vaporization phenomena

    NASA Technical Reports Server (NTRS)

    Lincoln, K. A.

    1974-01-01

    A laser has been combined with a mass spectrometer in a new configuration developed for studies of high-temperature materials. A vacuum-lock, solid-sample inlet is mounted at one end of a cylindrical, high-vacuum chamber one meter in length with a nude ion-source, time-of-flight mass spectrometer at the opposite end. The samples are positioned along the axis of the chamber at distances up to one meter from the ion source, and their surfaces are vaporized by a pulsed laser beam entering via windows on one side of the chamber. The instrumentation along with its capabilities is described, and results from laser-induced vaporization of several graphites are presented.

  15. Poly(1-vinylimidazole) functionalized magnetic ion imprinted polymer for fast and selective extraction of trace gold in geological, environmental and biological samples followed by graphite furnace atomic absorption spectrometry detection

    NASA Astrophysics Data System (ADS)

    Zhao, Bingshan; He, Man; Chen, Beibei; Xu, Hongrun; Hu, Bin

    2018-05-01

    In this study, poly(1-vinylimidazole) functionalized gold ion imprinted polymer coated magnetic nanoparticles (MNPs@PVIM-Au-IIP) were prepared and characterized. The adsorption behaviors of the prepared MNPs@PVIM-Au-IIP toward gold ions (Au(III)) were studied, it was found that MNPs@PVIM-Au-IIP has good selectivity, high adsorption capacity (185.4 mg g-1) and fast adsorption kinetic for Au(III). Based on it, a new method of ion imprinted magnetic solid phase extraction (II-MSPE) coupled with graphite furnace atomic absorption spectrometry (GFAAS) detection was proposed for the analysis of trace Au(III) in real samples with complicated matrix. Factors affecting MSPE including sample pH, desorption reagent, elution concentration and volume, elution time, sample volume and adsorption time were optimized. With high enrichment factor of 100-fold, the detection limit of the proposed method is 7.9 ng L-1 for Au(III) with the relative standard deviation of 7.4% (c = 50 ng L-1, n = 7). In order to validate the accuracy of the proposed method, the Certified Reference Material of GBW07293 geological sample (platinpalladium ore) was analyzed, and the determined value was in good agreement with the certified value. The proposed II-MSPE-GFAAS method is simple, fast, selective, sensitive and has been successfully applied in the determination of trace Au in ore, sediment, environmental water and human urine samples with satisfactory results.

  16. Factors affecting the thermal shock behavior of yttria stabilized hafnia based graphite and tungsten composites.

    NASA Technical Reports Server (NTRS)

    Lineback, L. D.; Manning, C. R.

    1971-01-01

    Hafnia-based composites containing either graphite or tungsten were investigated as rocket nozzle throat inserts in solid propellant rocket engines. The thermal shock resistance of these materials is considered in terms of macroscopic thermal conductivity, thermal expansion, modulus of elasticity, and compressive fracture stress. The effect of degree of hafnia stabilization, density, and graphite or tungsten content upon these parameters is discussed. The variation of the ratio of elastic modulus to compressive fracture stress with density and its effect upon thermal shock resistance of these materials are discussed in detail.

  17. Direct laser writing of micro-supercapacitors on hydrated graphite oxide films.

    PubMed

    Gao, Wei; Singh, Neelam; Song, Li; Liu, Zheng; Reddy, Arava Leela Mohana; Ci, Lijie; Vajtai, Robert; Zhang, Qing; Wei, Bingqing; Ajayan, Pulickel M

    2011-07-31

    Microscale supercapacitors provide an important complement to batteries in a variety of applications, including portable electronics. Although they can be manufactured using a number of printing and lithography techniques, continued improvements in cost, scalability and form factor are required to realize their full potential. Here, we demonstrate the scalable fabrication of a new type of all-carbon, monolithic supercapacitor by laser reduction and patterning of graphite oxide films. We pattern both in-plane and conventional electrodes consisting of reduced graphite oxide with micrometre resolution, between which graphite oxide serves as a solid electrolyte. The substantial amounts of trapped water in the graphite oxide makes it simultaneously a good ionic conductor and an electrical insulator, allowing it to serve as both an electrolyte and an electrode separator with ion transport characteristics similar to that observed for Nafion membranes. The resulting micro-supercapacitor devices show good cyclic stability, and energy storage capacities comparable to existing thin-film supercapacitors.

  18. Direct laser writing of micro-supercapacitors on hydrated graphite oxide films

    NASA Astrophysics Data System (ADS)

    Gao, Wei; Singh, Neelam; Song, Li; Liu, Zheng; Reddy, Arava Leela Mohana; Ci, Lijie; Vajtai, Robert; Zhang, Qing; Wei, Bingqing; Ajayan, Pulickel M.

    2011-08-01

    Microscale supercapacitors provide an important complement to batteries in a variety of applications, including portable electronics. Although they can be manufactured using a number of printing and lithography techniques, continued improvements in cost, scalability and form factor are required to realize their full potential. Here, we demonstrate the scalable fabrication of a new type of all-carbon, monolithic supercapacitor by laser reduction and patterning of graphite oxide films. We pattern both in-plane and conventional electrodes consisting of reduced graphite oxide with micrometre resolution, between which graphite oxide serves as a solid electrolyte. The substantial amounts of trapped water in the graphite oxide makes it simultaneously a good ionic conductor and an electrical insulator, allowing it to serve as both an electrolyte and an electrode separator with ion transport characteristics similar to that observed for Nafion membranes. The resulting micro-supercapacitor devices show good cyclic stability, and energy storage capacities comparable to existing thin-film supercapacitors.

  19. Evaluation of co-cokes from bituminous coal with vacuum resid or decant oil, and evaluation of anthracites, as precursors to graphite

    NASA Astrophysics Data System (ADS)

    Nyathi, Mhlwazi S.

    2011-12-01

    Graphite is utilized as a neutron moderator and structural component in some nuclear reactor designs. During the reactor operaction the structure of graphite is damaged by collision with fast neutrons. Graphite's resistance to this damage determines its lifetime in the reactor. On neutron irradiation, isotropic or near-isotropic graphite experiences less structural damage than anisotropic graphite. The degree of anisotropy in a graphite artifact is dependent on the structure of its precursor coke. Currently, there exist concerns over a short supply of traditional precursor coke, primarily due to a steadily increasing price of petroleum. The main goal of this study was to study the anisotropic and isotropic properties of graphitized co-cokes and anthracites as a way of investigating the possibility of synthesizing isotropic or near-isotropic graphite from co-cokes and anthracites. Demonstrating the ability to form isotropic or near-isotropic graphite would mean that co-cokes and anthracites have a potential use as filler material in the synthesis of nuclear graphite. The approach used to control the co-coke structure was to vary the reaction conditions. Co-cokes were produced by coking 4:1 blends of vacuum resid/coal and decant oil/coal at temperatures of 465 and 500 °C for reaction times of 12 and 18 hours under autogenous pressure. Co-cokes obtained were calcined at 1420 °C and graphitized at 3000 °C for 24 hours. Optical microscopy, X-ray diffraction, temperature-programmed oxidation and Raman spectroscopy were used to characterize the products. It was found that higher reaction temperature (500 °C) or shorter reaction time (12 hours) leads to an increase in co-coke structural disorder and an increase in the amount of mosaic carbon at the expense of textural components that are necessary for the formation of anisotropic structure, namely, domains and flow domains. Characterization of graphitized co-cokes showed that the quality, as expressed by the degree of graphitization and crystallite dimensions, of the final product is dependent on the nature of the precursor co-coke. The methodology for studying anthracites was to select two anthracites on basis of rank, PSOC1515 being semi-anthracite and DECS21 anthracite. The selected anthracites were graphitized, in both native and demineralized states, under the same conditions as co-cokes. Products obtained from DECS21 showed higher degrees of graphitization and larger crystallite dimensions than products obtained from PSOC1515. Demineralization of anthracites served to increase the degree of graphitization, indicating that the minerals contained in these anthracites have no graphitization-enhancing ability. A larger crystallite length for products obtained from native versions, compared to demineralized versions, was attributed to a formation and decomposition of a silicon carbide during graphitization of native versions. In order to examine the anisotropic and isotropic properties, nuclear-grade graphite samples obtained from Oak Ridge National Laboratory (ORNL) and commercial graphite purchased from Fluka were characterized under similar conditions as graphitized co-cokes and anthracites. These samples served as representatives of "two extremes", with ORNL samples being the isotropic end and commercial graphite being the anisotropic end. Through evaluating relationships between structural parameters, it was observed that graphitized co-cokes are situated, structurally, somewhere between the "two extremes", whereas graphitized anthracites are closer to the anisotropic end. Basically, co-cokes have a better potential than anthracites to transform to isotropic or near-isotropic graphite upon graphitization. By co-coking vacuum resid/coal instead of decant oil/coal or using 500 °C instead of 465 °C, a shift away from commercial graphite towards ORNL samples was attained. Graphitizing a semi-anthracite or demineralizing anthracites before graphitization also caused a shift towards ORNL samples.

  20. Effects of pore formers on microstructure and performance of cathode membranes for solid oxide fuel cells

    NASA Astrophysics Data System (ADS)

    Nie, Lifang; Liu, Juncheng; Zhang, Yujun; Liu, Meilin

    La 0.6Sr 0.4Co 0.2Fe 0.8O 3- δ (LSCF) is the most widely used cathode material for intermediate temperature solid oxide fuel cells. In the present communication, porous LSCF cathodes are fabricated by tape casting, a low-cost and reproducible fabrication process. The effects of four different pore formers, namely, graphite, carbon black, rice starch, and corn starch, on the microstructure and electrochemical performance of the LSCF cathode are investigated. Examination of the microstructures reveals that the shape of the pores, the pore size, and the pore distribution in the final ceramic are related to the type of pore formers. Impedance analysis and cell testing show that the best performance is obtained from the cathode using graphite as the pore former. The microstructure indicates that graphite results in a porous LSCF cathode with a large surface area and high porosity, which can offer a considerably long triple phase boundary for catalytic reactions as well as channels for gas phase transport.

  1. Influence of Inner Transducer Properties on EMF Response and Stability of Solid-Contact Anion Selective Membrane Electrodes Based on Metalloporphyrin Ionophores

    PubMed Central

    Górski, Łukasz; Matusevich, Alexey; Pietrzak, Mariusz; Wang, Lin; Meyerhoff, Mark E.; Malinowska, Elżbieta

    2010-01-01

    The performance of solid-contact/coated wire type electrodes with plasticized PVC membranes containing metalloporphyrins as anion selective ionophores is reported. The membranes are deposited on transducers based on graphite pastes and graphite rods. The hydrophobicity of the underlying conductive transducer surface is found to be a key factor that influences the formation of an aqueous layer beneath the polymer film. Elimination of this ill-defined water layer greatly improves the electrochemical properties of the ion-sensors, such as EMF stability and life-time. Only highly lipophilic electrode substrates, namely graphite paste with mineral oil, were shown to prevent the formation of aqueous layer underneath the ion-sensing membrane. The possibility of employing Co(III)-tetraphenylporphyrin both as NO2− selective ionophore and as electron/ion conducting species to ensure ion-to-electron translation was also discussed based on the results of preliminary experiments. PMID:20357903

  2. Gas chromatographic detection of some nitro explosive compounds in soil samples after solid-phase microextraction with carbon ceramic copper nanoparticle fibers.

    PubMed

    Farhadi, Khalil; Bochani, Shayesteh; Hatami, Mehdi; Molaei, Rahim; Pirkharrati, Hossein

    2014-07-01

    In this research, a new solid-phase microextraction fiber based on carbon ceramic composites with copper nanoparticles followed by gas chromatography with flame ionization detection was applied for the extraction and determination of some nitro explosive compounds in soil samples. The proposed method provides an overview of trends related to synthesis of solid-phase microextraction sorbents and their applications in preconcentration and determination of nitro explosives. The sorbents were prepared by mixing of copper nanoparticles with a ceramic composite produced by mixture of methyltrimethoxysilane, graphite, methanol, and hydrochloric acid. The prepared sorbents were coated on copper wires by dip-coating method. The prepared nanocomposites were evaluated statistically and provided better limits of detection than the pure carbon ceramic. The limit of detection of the proposed method was 0.6 μg/g with a linear response over the concentration range of 2-160 μg/g and square of correlation coefficient >0.992. The new proposed fiber has been demonstrated to be a suitable, inexpensive, and sensitive candidate for extraction of nitro explosive compounds in contaminated soil samples. The constructed fiber can be used more than 100 times without the need for surface generation. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Mineralogical and isotopic characterization of graphite deposits from the Anatectic Complex of Toledo, central Spain

    NASA Astrophysics Data System (ADS)

    Martín-Méndez, Iván; Boixereu, Ester; Villaseca, Carlos

    2016-06-01

    Graphite is found dispersed in high-grade metapelitic rocks of the Anatectic Complex of Toledo (ACT) and was mined during the mid twentieth century in places where it has been concentrated (Guadamur and la Puebla de Montalbán mines). Some samples from these mines show variable but significant alteration intensity, reaching very low-T hydrothermal (supergene) conditions for some samples from the waste heap of the Guadamur site (<100 °C and 1 kbar). Micro-Raman and XRD data indicate that all the studied ACT graphite is of high crystallinity irrespective of the degree of hydrothermal alteration. Chemical differences were obtained for graphite δ13C composition. ACT granulitic graphite shows δ13CPDB values in the range of -20.5 to -27.8 ‰, indicating a biogenic origin. Interaction of graphite with hydrothermal fluids does not modify isotopic compositions even in the most transformed samples from mining sites. The different isotopic signatures of graphite from the mining sites reflect its contrasted primary carbon source. The high crystallinity of studied graphite makes this area of central Spain suitable for graphitic exploration and its potential exploitation, due to the low carbon content required for its viability and its strategic applications in advanced technologies, such as graphene synthesis.

  4. Characterization of Graphite Oxide and Reduced Graphene Oxide Obtained from Different Graphite Precursors and Oxidized by Different Methods Using Raman Spectroscopy.

    PubMed

    Muzyka, Roksana; Drewniak, Sabina; Pustelny, Tadeusz; Chrubasik, Maciej; Gryglewicz, Grażyna

    2018-06-21

    In this paper, the influences of the graphite precursor and the oxidation method on the resulting reduced graphene oxide (especially its composition and morphology) are shown. Three types of graphite were used to prepare samples for analysis, and each of the precursors was oxidized by two different methods (all samples were reduced by the same method of thermal reduction). Each obtained graphite oxide and reduced graphene oxide was analysed by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy (RS).

  5. Combustion Of Porous Graphite Particles In Oxygen Enriched Air

    NASA Technical Reports Server (NTRS)

    Delisle, Andrew J.; Miller, Fletcher J.; Chelliah, Harsha K.

    2003-01-01

    Combustion of solid fuel particles has many important applications, including power generation and space propulsion systems. The current models available for describing the combustion process of these particles, especially porous solid particles, include various simplifying approximations. One of the most limiting approximations is the lumping of the physical properties of the porous fuel with the heterogeneous chemical reaction rate constants [1]. The primary objective of the present work is to develop a rigorous modeling approach that could decouple such physical and chemical effects from the global heterogeneous reaction rates. For the purpose of validating this model, experiments with porous graphite particles of varying sizes and porosity are being performed under normal and micro gravity.

  6. In situ polymerization of monomers for polyphenylquinoxaline/graphite fiber composites

    NASA Technical Reports Server (NTRS)

    Serafini, T. T.; Delvigs, P.; Vannucci, R. D.

    1974-01-01

    Methods currently used to prepare fiber reinforced, high temperature resistant polyphenylquinoxaline (PPQ) composites employ extremely viscous, low solids content solutions of high molecular weight PPQ polymers. An improved approach, described in this report, consists of impregnating the fiber with a solution of the appropriate monomers instead of a solution of previously synthesized high molecular weight polymer. Polymerization of the monomers occurs in situ on the fiber during the solvent removal and curing stages. The in situ polymerization approach greatly simplifies the fabrication of PPQ graphite fiber composites. The use of low viscosity monomeric type solutions facilitates fiber wetting, permits a high solids content, and eliminates the need for prior polymer synthesis.

  7. Characterization of exposures to nanoscale particles and fibers during solid core drilling of hybrid carbon nanotube advanced composites.

    PubMed

    Bello, Dhimiter; Wardle, Brian L; Zhang, Jie; Yamamoto, Namiko; Santeufemio, Christopher; Hallock, Marilyn; Virji, M Abbas

    2010-01-01

    This work investigated exposures to nanoparticles and nanofibers during solid core drilling of two types of advanced carbon nanotube (CNT)-hybrid composites: (1) reinforced plastic hybrid laminates (alumina fibers and CNT); and (2) graphite-epoxy composites (carbon fibers and CNT). Multiple real-time instruments were used to characterize the size distribution (5.6 nm to 20 microm), number and mass concentration, particle-bound polyaromatic hydrocarbons (b-PAHs), and surface area of airborne particles at the source and breathing zone. Time-integrated samples included grids for electron microscopy characterization of particle morphology and size resolved (2 nm to 20 microm) samples for the quantification of metals. Several new important findings herein include generation of airborne clusters of CNTs not seen during saw-cutting of similar composites, fewer nanofibers and respirable fibers released, similarly high exposures to nanoparticles with less dependence on the composite thickness, and ultrafine (< 5 nm) aerosol originating from thermal degradation of the composite material.

  8. Processing and fabrication of mixed uranium/refractory metal carbide fuels with liquid-phase sintering

    NASA Astrophysics Data System (ADS)

    Knight, Travis W.; Anghaie, Samim

    2002-11-01

    Optimization of powder processing techniques were sought for the fabrication of single-phase, solid-solution mixed uranium/refractory metal carbide nuclear fuels - namely (U, Zr, Nb)C. These advanced, ultra-high temperature nuclear fuels have great potential for improved performance over graphite matrix, dispersed fuels tested in the Rover/NERVA program of the 1960s and early 1970s. Hypostoichiometric fuel samples with carbon-to-metal ratios of 0.98, uranium metal mole fractions of 5% and 10%, and porosities less than 5% were fabricated. These qualities should provide for the longest life and highest performance capability for these fuels. Study and optimization of processing methods were necessary to provide the quality assurance of samples for meaningful testing and assessment of performance for nuclear thermal propulsion applications. The processing parameters and benefits of enhanced sintering by uranium carbide liquid-phase sintering were established for the rapid and effective consolidation and formation of a solid-solution mixed carbide nuclear fuel.

  9. Direct determination of chromium in infant formulas employing high-resolution continuum source electrothermal atomic absorption spectrometry and solid sample analysis.

    PubMed

    Silva, Arlene S; Brandao, Geovani C; Matos, Geraldo D; Ferreira, Sergio L C

    2015-11-01

    The present work proposed an analytical method for the direct determination of chromium in infant formulas employing the high-resolution continuum source electrothermal atomic absorption spectrometry combined with the solid sample analysis (SS-HR-CS ET AAS). Sample masses up to 2.0mg were directly weighted on a solid sampling platform and introduced into the graphite tube. In order to minimize the formation of carbonaceous residues and to improve the contact of the modifier solution with the solid sample, a volume of 10 µL of a solution containing 6% (v/v) H2O2, 20% (v/v) ethanol and 1% (v/v) HNO3 was added. The pyrolysis and atomization temperatures established were 1600 and 2400 °C, respectively, using magnesium as chemical modifier. The calibration technique was evaluated by comparing the slopes of calibration curves established using aqueous and solid standards. This test revealed that chromium can be determined employing the external calibration technique using aqueous standards. Under these conditions, the method developed allows the direct determination of chromium with limit of quantification of 11.5 ng g(-1), precision expressed as relative standard deviation (RSD) in the range of 4.0-17.9% (n=3) and a characteristic mass of 1.2 pg of chromium. The accuracy was confirmed by analysis of a certified reference material of tomato leaves furnished by National Institute of Standards and Technology. The method proposed was applied for the determination of chromium in five different infant formula samples. The chromium content found varied in the range of 33.9-58.1 ng g(-1) (n=3). These samples were also analyzed employing ICP-MS. A statistical test demonstrated that there is no significant difference between the results found by two methods. The chromium concentrations achieved are lower than the maximum limit permissible for chromium in foods by Brazilian Legislation. Copyright © 2015. Published by Elsevier B.V.

  10. Thermal desorption of formamide and methylamine from graphite and amorphous water ice surfaces

    NASA Astrophysics Data System (ADS)

    Chaabouni, H.; Diana, S.; Nguyen, T.; Dulieu, F.

    2018-04-01

    Context. Formamide (NH2CHO) and methylamine (CH3NH2) are known to be the most abundant amine-containing molecules in many astrophysical environments. The presence of these molecules in the gas phase may result from thermal desorption of interstellar ices. Aims: The aim of this work is to determine the values of the desorption energies of formamide and methylamine from analogues of interstellar dust grain surfaces and to understand their interaction with water ice. Methods: Temperature programmed desorption (TPD) experiments of formamide and methylamine ices were performed in the sub-monolayer and monolayer regimes on graphite (HOPG) and non-porous amorphous solid water (np-ASW) ice surfaces at temperatures 40-240 K. The desorption energy distributions of these two molecules were calculated from TPD measurements using a set of independent Polanyi-Wigner equations. Results: The maximum of the desorption of formamide from both graphite and ASW ice surfaces occurs at 176 K after the desorption of H2O molecules, whereas the desorption profile of methylamine depends strongly on the substrate. Solid methylamine starts to desorb below 100 K from the graphite surface. Its desorption from the water ice surface occurs after 120 K and stops during the water ice sublimation around 150 K. It continues to desorb from the graphite surface at temperatures higher than160 K. Conclusions: More than 95% of solid NH2CHO diffuses through the np-ASW ice surface towards the graphitic substrate and is released into the gas phase with a desorption energy distribution Edes = 7460-9380 K, which is measured with the best-fit pre-exponential factor A = 1018 s-1. However, the desorption energy distribution of methylamine from the np-ASW ice surface (Edes = 3850-8420 K) is measured with the best-fit pre-exponential factor A = 1012 s-1. A fraction of solid methylamine monolayer of roughly 0.15 diffuses through the water ice surface towards the HOPG substrate. This small amount of methylamine desorbs later with higher binding energies (5050-8420 K) that exceed that of the crystalline water ice (Edes = 4930 K), which is calculated with the same pre-exponential factor A = 1012 s-1. The best wetting ability of methylamine compared to H2O molecules makes CH3NH2 molecules a refractory species for low coverage. Other binding energies of astrophysical relevant molecules are gathered and compared, but we could not link the chemical functional groups (amino, methyl, hydroxyl, and carbonyl) with the binding energy properties. Implications of these high binding energies are discussed.

  11. Graphene oxide-TiO2 composite solid phase extraction combined with graphite furnace atomic absorption spectrometry for the speciation of inorganic selenium in water samples.

    PubMed

    Zhang, Yanan; Chen, Beibei; Wu, Shaowei; He, Man; Hu, Bin

    2016-07-01

    In this paper, a method of graphene oxide (GO)-TiO2 composite solid phase extraction followed by graphite furnace atomic absorption spectrometry (GFAAS) detection was proposed for the speciation of inorganic selenium in environmental waters. The adsorption behavior of inorganic Se(IV) and Se(VI) on the GO-TiO2(1:1) composite was investigated. It was found that Se(IV) was quantitatively retained on the GO-TiO2 composites within a wide pH range of 0.5-10, while Se(VI) was quantitatively adsorbed on GO-TiO2(1:1) composite at pH 0.5-2, and no obvious adsorption of Se(VI) within the pH range of 4-10 was found. By selecting pH 6.0, Se(IV) could be easily determined. After reduction of Se(VI), total Se was determined by the proposed method, and Se(VI) was calculated as the difference between the total Se and Se(IV). The factors affecting the separation/preconcentration of Se(IV) and Se(VI) were studied. Under the optimum conditions, the isothermal adsorption of Se(IV) on the GO-TiO2(1:1) composite fitted Langmuir model; a linear range over 0.1-12ngmL(-1) was obtained. The limit of detection (LOD) and precision of the method for Se(IV) was 0.04ngmL(-1) and 9.4% (cSe(IV)=0.5ngmL(-1), n=7), respectively. In order to verify the accuracy of the method, a standard water sample (GSBZ50031-94) was analyzed, and the determined value was in a good agreement to the certified value. The established method was applied to inorganic Se speciation in environmental water samples and the recovery of 87.4-102% was obtained for the spiked samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Astrophysics with Presolar Stardust

    NASA Astrophysics Data System (ADS)

    Clayton, Donald D.; Nittler, Larry R.

    2004-09-01

    Meteorites and interplanetary dust particles contain presolar stardust grains: solid samples of stars that can be studied in the laboratory. The stellar origin of the grains is indicated by enormous isotopic ratio variations compared with Solar System materials, explainable only by nuclear reactions occurring in stars. Known presolar phases include diamond, SiC, graphite, Si3N4, Al2O3, MgAl2O4, CaAl12O19, TiO2, Mg(Cr,Al)2O4, and most recently, silicates. Subgrains of refractory carbides (e.g., TiC), and Fe-Ni metal have also been observed within individual presolar graphite grains. We review the astrophysical implications of these grains for the sciences of nucleosynthesis, stellar evolution, grain condensation, and the chemical and dynamic evolution of the Galaxy. Unique scientific information derives primarily from the high precision (in some cases <1%) of the measured isotopic ratios of large numbers of elements in single stardust grains. Stardust science is just now reaching maturity and will play an increasingly important role in nucleosynthesis applications.

  13. Hot filament technique for measuring the thermal conductivity of molten lithium fluoride

    NASA Technical Reports Server (NTRS)

    Jaworske, Donald A.; Perry, William D.

    1990-01-01

    Molten salts, such as lithium fluoride, are attractive candidates for thermal energy storage in solar dynamic space power systems because of their high latent heat of fusion. However, these same salts have poor thermal conductivities which inhibit the transfer of heat into the solid phase and out of the liquid phase. One concept for improving the thermal conductivity of the thermal energy storage system is to add a conductive filler material to the molten salt. High thermal conductivity pitch-based graphite fibers are being considered for this application. Although there is some information available on the thermal conductivity of lithium fluoride solid, there is very little information on lithium fluoride liquid, and no information on molten salt graphite fiber composites. This paper describes a hot filament technique for determining the thermal conductivity of molten salts. The hot filament technique was used to find the thermal conductivity of molten lithium fluoride at 930 C, and the thermal conductivity values ranged from 1.2 to 1.6 W/mK. These values are comparable to the slightly larger value of 5.0 W/mK for lithium fluoride solid. In addition, two molten salt graphite fiber composites were characterized with the hot filament technique and these results are also presented.

  14. Temperature dependence of broadline NMR spectra of water-soaked, epoxy-graphite composites

    NASA Astrophysics Data System (ADS)

    Lawing, David; Fornes, R. E.; Gilbert, R. D.; Memory, J. D.

    1981-10-01

    Water-soaked, epoxy resin-graphite fiber composites show a waterline in their broadline proton NMR spectrum which indicates a state of intermediate mobility between the solid and free water liquid states. The line is still present at -42 °C, but shows a reversible decrease in amplitude with decreasing temperature. The line is isotropic upon rotation of the fiber axis with respect to the external magnetic field.

  15. Formation of Reversible Solid Electrolyte Interface on Graphite Surface from Concentrated Electrolytes

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

    Lu, Dongping; Tao, Jinhui; Yan, Pengfei

    2017-02-10

    Interfacial phenomena have always been key determinants for the performance of energy storage technologies. The solid electrolyte interfacial (SEI) layer, pervasive on the surfaces of battery electrodes for numerous chemical couples, directly affects the ion transport, charge transfer and lifespan of the entire energy system. Almost all SEI layers, however, are unstable resulting in the continuous consumption of the electrolyte. Typically, this leads to the accumulation of degradation products on/restructuring of the electrode surface and thus increased cell impedance, which largely limits the long-term operation of the electrochemical reactions. Herein, a completely new SEI formation mechanism has been discovered, inmore » which the electrolyte components reversibly self-assemble into a protective surface coating on a graphite electrode upon changing the potential. In contrast to the established wisdom regarding the necessity of employing the solvent ethylene carbonate (EC) to form a protective SEI layer on graphite, a wide range of EC-free electrolytes are demonstrated for the reversible intercalation/deintercalation of Li+ cations within a graphite lattice, thereby providing tremendous flexibility in electrolyte tailoring for battery couples. This novel finding is broadly applicable and provides guidance for how to control interfacial reactions through the relationship between ion aggregation and solvent decomposition at polarized interfaces.« less

  16. GUM Analysis for SIMS Isotopic Ratios in BEP0 Graphite Qualification Samples, Round 2

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

    Gerlach, David C.; Heasler, Patrick G.; Reid, Bruce D.

    2009-01-01

    This report describes GUM calculations for TIMS and SIMS isotopic ratio measurements of reactor graphite samples. These isotopic ratios are used to estimate reactor burn-up, and currently consist of various ratios of U, Pu, and Boron impurities in the graphite samples. The GUM calculation is a propagation of error methodology that assigns uncertainties (in the form of standard error and confidence bound) to the final estimates.

  17. A structural study of solid electrolyte interface on negative electrode of lithium-Ion battery by electron microscopy.

    PubMed

    Matsushita, Tadashi; Watanabe, Jiro; Nakao, Tatsuya; Yamashita, Seiichi

    2014-11-01

    For the last decades, the performance of the lithium-ion battery (LIB) has been significantly improved and its applications have been expanding rapidly. However, its performance has yet to be enhanced.In the lithium-ion battery development, it is important to elucidate the electrode structure change in detail during the charge and discharge cycling. In particular, solid electrolyte interface (SEI) formed by decomposition of the electrolytes on the graphite negative electrode surface should play an important role for battery properties. Therefore, it is essential to control the structure and composition of SEI to improve the battery performance. Here, we conducted a scanning electron microscope (SEM) and transmission electron microscope (TEM) study to elucidate the structures of the SEI during the charge and discharge process using LiNi1/3Co1/3Mn1/3O2 [1] cathode and graphite anode. [2] Since SEI is a lithium-containing compound with high activity, it was observed without being exposed to the atmosphere. The electrodes including SEI were sampled after dismantling batteries with cutoff voltages of 3V and 4.2V for the charge process and 3V for the discharge process. Fig.1 shows SEM images of the graphite electrode surface during the charge and discharge process. The change of the SEI structure during the process was clearly observed. Further, TEM images showed that the SEI grew thicker during the charge process and becomes thinner when discharged. These results with regard to the reversible SEI structure could give a new insight for the battery development.jmicro;63/suppl_1/i21/DFU056F1F1DFU056F1Fig. 1.SEM images of the graphite electrode surface:(a) before charge process;(b) with charge-cutoff voltage of 3.0V; (c) with charge-cutoff voltage of 4.2V; (d) with discharge-cutoff voltage of 3.0V. © The Author 2014. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

  18. Flight service evaluation of an advanced composite empennage component on commercial transport aircraft

    NASA Technical Reports Server (NTRS)

    1976-01-01

    The development and flight evaluation of an advanced composite empennage component is presented. The recommended concept for the covers is graphite-epoxy hats bonded to a graphite-epoxy skin. The hat flare-out has been eliminated, instead the hat is continuous into the joint. The recommended concept for the spars is graphite-epoxy caps and a hybrid of Kevlar-49 and graphite-epoxy in the spar web. The spar cap, spar web stiffeners for attaching the ribs, and intermediate stiffeners are planned to be fabricated as a unit. Access hole in the web will be reinforced with a donut type, zero degree graphite-epoxy wound reinforcement. The miniwich design concept in the upper three ribs originally proposed is changed to a graphite-epoxy stiffened solid laminate design concept. The recommended configuration for the lower seven ribs remains as graphite-epoxy caps with aluminum cruciform diagonals. The indicated weight saving for the current advanced composite vertical fin configuration is 20.2% including a 24 lb growth allowance. The project production cost saving is approximately 1% based on a cumulative average of 250 aircraft and including only material, production labor, and quality assurance costs.

  19. Controlling the Surface Chemistry of Graphite by Engineered Self-Assembled Peptides

    PubMed Central

    Khatayevich, Dmitriy; So, Christopher R.; Hayamizu, Yuhei; Gresswell, Carolyn; Sarikaya, Mehmet

    2012-01-01

    The systematic control over surface chemistry is a long-standing challenge in biomedical and nanotechnological applications for graphitic materials. As a novel approach, we utilize graphite-binding dodecapeptides that self-assemble into dense domains to form monolayer thick long-range ordered films on graphite. Specifically, the peptides are rationally designed through their amino acid sequences to predictably display hydrophilic and hydrophobic characteristics while maintaining their self-assembly capabilities on the solid substrate. The peptides are observed to maintain a high tolerance for sequence modification, allowing the control over surface chemistry via their amino acid sequence. Furthermore, through a single step co-assembly of two different designed peptides, we predictably and precisely tune the wettability of the resulting functionalized graphite surfaces from 44 to 83 degrees. The modular molecular structures and predictable behavior of short peptides demonstrated here give rise to a novel platform for functionalizing graphitic materials that offers numerous advantages, including non-invasive modification of the substrate, bio-compatible processing in an aqueous environment, and simple fusion with other functional biological molecules. PMID:22428620

  20. Burning characteristics and fiber retention of graphite/resin matrix composites

    NASA Technical Reports Server (NTRS)

    Bowles, K. J.

    1980-01-01

    Graphite fiber reinforced resin matrix composites were subjected to controlled burning conditions to determine their burning characteristics and fiber retention properties. Two types of burning equipment were used. Small samples were burned with a natural gas fired torch to study the effects of fiber orientation and structural flaws such as holes and slits that were machined into the laminates. Larger laminate samples were burned in a Heat Release Rate Calorimeter. Unidirectional epoxy/graphite and polyimide/graphite composites and boron powder filled samples of each of the two composite systems were burn tested and exposed to a thermal radiation. The effects of fiber orientation, flaws, and boron filler additives to the resins were evaluated. A high char forming polyimide resin was no more effective in retaining graphite fibers than a low char forming epoxy resin when burning in air.

  1. Mass removal by oxidation and sublimation of porous graphite during fiber laser irradiation

    NASA Astrophysics Data System (ADS)

    Phillips, Grady T.; Bauer, William A.; Fox, Charles D.; Gonzales, Ashley E.; Herr, Nicholas C.; Gosse, Ryan C.; Perram, Glen P.

    2017-01-01

    The various effects of laser heating of carbon materials are key to assessing laser weapon effectiveness. Porous graphite plates, cylinders, and cones with densities of 1.55 to 1.82 g/cm3 were irradiated by a 10-kW fiber laser at 0.075 to 3.525 kW/cm2 for 120 s to study mass removal and crater formation. Surface temperatures reached steady state values as high as 3767 K. The total decrease in sample mass ranged from 0.06 to 6.29 g, with crater volumes of 0.52 to 838 mm3, and penetration times for 12.7-mm-thick plates as short as 38 s. Minor contaminants in the graphite samples produced calcium and iron oxide to be redeposited on the graphite surface. Dramatic graphite crystalline structures are also produced at higher laser irradiances. Significantly increased porosity of the sample is observed even outside the laser-irradiated region. Total mass removed increases with deposited laser energy at a rate of 4.83 g/MJ for medium extruded graphite with an apparent threshold of 0.15 MJ. At ˜3.5 kW/cm2, the fractions of the mass removed from the cylindrical samples in the crater, surrounding trench, and outer region of decreased porosity are 38%, 47%, and 15%, respectively. Graphite is particularly resistant to damage by high power lasers. The new understanding of graphite combustion and sublimation during laser irradiation is vital to the more complex behavior of carbon composites.

  2. Thixoforming of Stellite Powder Compacts

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

    Hogg, S. C.; Atkinson, H. V.; Kapranos, P.

    2007-04-07

    Thixoforming involves processing metallic alloys in the semi-solid state. The process requires the microstructure to be spheroidal when part-solid and part-liquid i.e. to consist of solid spheroids surrounded by liquid. The aim of this work was to investigate whether powder compacts can be used as feedstock for thixoforming and whether the consolidating pressure in the thixoformer can be used to remove porosity from the compact. The powder compacts were made from stellite 6 and stellite 21 alloys, cobalt-based alloys widely used for e.g. manufacturing prostheses. Isothermal heat treatments of small samples in the consolidated state showed the optimum thixoforming temperaturemore » to be in the range 1340 deg. C-1350 deg. C for both materials. The alloys were thixoformed into graphite dies and flowed easily to fill the die. Porosity in the thixoformed components was lower than in the starting material. Hardness values at various positions along the radius of the thixoformed demonstrator component were above the specification for both alloys.« less

  3. Heterogenous Combustion of Porous Graphite Particles in Normal and Microgravity

    NASA Technical Reports Server (NTRS)

    Chelliah, Harsha K.; Miller, Fletcher J.; Delisle, Andrew J.

    2001-01-01

    Combustion of solid fuel particles has many important applications, including power generation and space propulsion systems. The current models available for describing the combustion process of these particles, especially porous solid particles, include various simplifying approximations. One of the most limiting approximations is the lumping of the physical properties of the porous fuel with the heterogeneous chemical reaction rate constants. The primary objective of the present work is to develop a rigorous model that could decouple such physical and chemical effects from the global heterogeneous reaction rates. For the purpose of validating this model, experiments with porous graphite particles of varying sizes and porosity are being performed. The details of this experimental and theoretical model development effort are described.

  4. Investigating the Co-Adsorption Behavior of Nucleic-Acid Base (Thymine and Cytosine) and Melamine at Liquid/Solid Interface

    NASA Astrophysics Data System (ADS)

    Zhao, Huiling; Li, Yinli; Chen, Dong; Liu, Bo

    2016-12-01

    The co-adsorption behavior of nucleic-acid base (thymine; cytosine) and melamine was investigated by scanning tunneling microscopy (STM) technique at liquid/solid (1-octanol/graphite) interface. STM characterization results indicate that phase separation happened after dropping the mixed solution of thymine-melamine onto highly oriented pyrolytic graphite (HOPG) surface, while the hetero-component cluster-like structure was observed when cytosine-melamine binary assembly system is used. From the viewpoints of non-covalent interactions calculated by using density functional theory (DFT) method, the formation mechanisms of these assembled structures were explored in detail. This work will supply a methodology to design the supramolecular assembled structures and the hetero-component materials composed by biological and chemical compound.

  5. Graphite to ultrafine nanocrystalline diamond phase transition model and growth restriction mechanism induced by nanosecond laser processing

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

    Ren, X. D., E-mail: renxd@mail.ujs.edu.cn; Liu, R.; Zheng, L. M.

    2015-10-05

    To have a clear insight into nanocrystal growth from graphite to diamond upon high energy pulsed laser irradiation of graphite suspension, synthesis of ultrafine nanocrystalline diamonds with laser energy set up from 0.3 J to 12 J, repetition rate of 10 Hz has been studied. The method allows synthesizing ultrafine nanocrystalline particles continuously at the ambient temperature and normal pressure. The particle size is shown independent of laser energy, which is ultrafine and ranges in 2–6 nm. The theoretical grown size of nano-diamonds is found in well agreement with the experiment results. Four kinds of production were found: nano-diamond, spherical carbon nano-particles, flocculent amorphousmore » carbon, and graphene nano-ribbon rolls. A solid-vapor-plasma-liquid coexistence model describing phase transition from graphite to diamond induced by nanosecond laser processing was proposed. Graphene nano-ribbon rolls might be the intermediate phase in the conversion from graphite to diamond.« less

  6. Forgery at the Snite Museum of Art? Improving AMS Radiocarbon Dating at the University of Notre Dame

    NASA Astrophysics Data System (ADS)

    Troyer, Laura; Bagwell, Connor; Anderson, Tyler; Clark, Adam; Nelson, Austin; Skulski, Michael; Collon, Philippe

    2017-09-01

    The Snite Museum of Art recently obtained several donations of artifacts. Five of the pieces lack sufficient background information to prove authenticity and require further analysis to positively determine the artwork's age. One method to determine the artwork's age is radiocarbon dating via Accelerator Mass Spectrometry (AMS) performed at the University of Notre Dame's Nuclear Science Laboratory. Samples are prepared by combustion of a small amount of material and subsequent reduction to carbon into an iron powder matrix (graphitization). The graphitization procedure affects the maximum measurement rate, and a poor graphitization can be detrimental to the AMS measurement of the sample. Previous graphitization procedures resulted in a particle current too low or inconsistent to optimize AMS measurements. Thus, there was a desire to design and refine the graphitization system. The finalized process yielded physically darker samples and increased sample currents by two orders of magnitude. Additionally, the first testing of the samples was successful, yet analysis of the dates proved inconclusive. AMS measurements will be performed again to obtain better sampling statistics in the hopes of narrowing the reported date ranges. NSF and JINA-CEE.

  7. Solid lubrication design methodology, phase 2

    NASA Technical Reports Server (NTRS)

    Pallini, R. A.; Wedeven, L. D.; Ragen, M. A.; Aggarwal, B. B.

    1986-01-01

    The high temperature performance of solid lubricated rolling elements was conducted with a specially designed traction (friction) test apparatus. Graphite lubricants containing three additives (silver, phosphate glass, and zinc orthophosphate) were evaluated from room temperature to 540 C. Two hard coats were also evaluated. The evaluation of these lubricants, using a burnishing method of application, shows a reasonable transfer of lubricant and wear protection for short duration testing except in the 200 C temperature range. The graphite lubricants containing silver and zinc orthophosphate additives were more effective than the phosphate glass material over the test conditions examined. Traction coefficients ranged from a low of 0.07 to a high of 0.6. By curve fitting the traction data, empirical equations for slope and maximum traction coefficient as a function of contact pressure (P), rolling speed (U), and temperature (T) can be developed for each lubricant. A solid lubricant traction model was incorporated into an advanced bearing analysis code (SHABERTH). For comparison purposes, preliminary heat generation calculations were made for both oil and solid lubricated bearing operation. A preliminary analysis indicated a significantly higher heat generation for a solid lubricated ball bearing in a deep groove configuration. An analysis of a cylindrical roller bearing configuration showed a potential for a low friction solid lubricated bearing.

  8. Study on the Microstructure and Liquid Phase Formation in a Semisolid Gray Cast Iron

    NASA Astrophysics Data System (ADS)

    Benati, Davi Munhoz; Ito, Kazuhiro; Kohama, Kazuyuki; Yamamoto, Hajime; Zoqui, Eugenio José

    2017-10-01

    The development of high-quality semisolid raw materials requires an understanding of the phase transformations that occur as the material is heated up to the semisolid state, i.e., its melting behavior. The microstructure of the material plays a very important role during semisolid processing as it determines the flow behavior of the material when it is formed, making a thorough understanding of the microstructural evolution essential. In this study, the phase transformations and microstructural evolution in Fe2.5C1.5Si gray cast iron specially designed for thixoforming processes as it was heated to the semisolid state were observed using in situ high-temperature confocal laser scanning microscopy. At room temperature, the alloy has a matrix of pearlite and ferrite with fine interdendritic type D flake graphite. During heating, the main transformations observed were graphite precipitation inside the grains and at the austenite grain boundaries; graphite flakes and graphite precipitates growing and becoming coarser with the increasing temperature; and the beginning of melting at around 1413 K to 1423 K (1140 °C to 1150 °C). Melting begins with the eutectic phase ( i.e., the carbon-rich phase) and continues with the primary phase (primary austenite), which is consumed as the temperature increases. Melting of the eutectic phase composed by coarsened interdendritic graphite flakes produced a semi-continuous liquid network homogeneously surrounding and wetting the dendrites of the solid phase, causing grains to detach from each other and producing the intended solid globules immersed in liquid.

  9. Solid-phase reductive amination for glycomic analysis.

    PubMed

    Jiang, Kuan; Zhu, He; Xiao, Cong; Liu, Ding; Edmunds, Garrett; Wen, Liuqing; Ma, Cheng; Li, Jing; Wang, Peng George

    2017-04-15

    Reductive amination is an indispensable method for glycomic analysis, as it tremendously facilitates glycan characterization and quantification by coupling functional tags at the reducing ends of glycans. However, traditional in-solution derivatization based approach for the preparation of reductively aminated glycans is quite tedious and time-consuming. Here, a simpler and more efficient strategy termed solid-phase reductive amination was investigated. The general concept underlying this new approach is to streamline glycan extraction, derivatization, and purification on non-porous graphitized carbon sorbents. Neutral and sialylated standard glycans were utilized to test the feasibility of the solid-phase method. As results, almost complete labeling of those glycans with four common labels of aniline, 2-aminobenzamide (2-AB), 2-aminobenzoic acid (2-AA) and 2-amino-N-(2-aminoethyl)-benzamide (AEAB) was obtained, and negligible desialylation occurred during sample preparation. The labeled glycans derived from glycoproteins showed excellent reproducibility in high performance liquid chromatography (HPLC) and matrix assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS) analysis. Direct comparisons based on fluorescent absorbance and relative quantification using isotopic labeling demonstrated that the solid-phase strategy enabled 20-30% increase in sample recovery. In short, the solid-phase strategy is simple, reproducible, efficient, and sensitive for glycan analysis. This method was also successfully applied for N-glycan profiling of HEK 293 cells with MALDI-TOF MS, showing its attractive application in the high-throughput analysis of mammalian glycome. Published by Elsevier B.V.

  10. Behavior of graphite under heat load and in contact with a hydrogen plasma

    NASA Astrophysics Data System (ADS)

    Bohdansky, J.; Croessmann, C. D.; Linke, J.; McDonald, J. M.; Morse, D. H.; Pontau, A. E.; Watson, R. D.; Whitley, J. B.; Goebel, D. M.; Hirooka, Y.; Leung, K.; Conn, R. W.; Roth, J.; Ottenberger, W.; Kotzlowski, H. E.

    1987-05-01

    Graphite is extensively used in large tokamaks today. In these machines the material is exposed to vacuum, to intense heat loads, and to the edge plasma. The use of graphite in such machines, therefore, depends on the outgassing behavior, the heat shock resistance, and thermochemical properties in a hydrogen plasma. Investigations of these properties made at different laboratories are described here. Experiments conducted at Sandia National Laboratories (SNL), Livermore, and the Max-Planck-Institut für Plasmaphysik (IPP) in Garching showed that the outgassing behavior of fine-grain reactor-grade graphite and carbon fiber composites depends on the pretreatment (manufacturing and/or storage). However, after proper outgassing the samples tested behave similarly in the case of fine-grain graphite, but the outgassing remains high for the carbon fiber composites. Heat shock tests have been made with the Electron Beam Test System (EBTS) at SNL, Albuquerque. Directly cooled graphite samples (FE 159 graphite brazed onto Mo tubes) showed no failure at a heat load of 700 W/cm 2, 20 s; or 10 kW, 1 s. Thermal erosion due to sublimination and particle emission from the graphite surface was observed. This effect is related to the surface temperature and becomes significant at temperatures above 2500°K. Fourteen different types of graphite were tested; the main differences among these samples were the different surface temperatures obtained under the same heating conditions. Cracking due to heat shocks was observed in some of the samples, but none of the carbon fiber composites failed. Thermochemical properties have been tested in the PISCES plasma generator at UCLA for ion energies of around 100 eV. The formation of C-H compounds was observed spectroscopically at sample temperatures of around 600°C. However, this chemical reaction did not lead to erosion as observed in beam experiments but to a drastic change of the surface structure due to redeposition. Carbon-hydrogen lines were still observed at sample temperatures of around 100°C. Under these conditions the erosion yield is high and in agreement with those measured in beam experiments.

  11. Quenchable compressed graphite synthesized from neutron-irradiated highly oriented pyrolytic graphite in high pressure treatment at 1500 °C

    NASA Astrophysics Data System (ADS)

    Niwase, Keisuke; Terasawa, Mititaka; Honda, Shin-ichi; Niibe, Masahito; Hisakuni, Tomohiko; Iwata, Tadao; Higo, Yuji; Hirai, Takeshi; Shinmei, Toru; Ohfuji, Hiroaki; Irifune, Tetsuo

    2018-04-01

    The super hard material of "compressed graphite" (CG) has been reported to be formed under compression of graphite at room temperature. However, it returns to graphite under decompression. Neutron-irradiated graphite, on the other hand, is a unique material for the synthesis of a new carbon phase, as reported by the formation of an amorphous diamond by shock compression. Here, we investigate the change of structure of highly oriented pyrolytic graphite (HOPG) irradiated with neutrons to a fluence of 1.4 × 1024 n/m2 under static pressure. The neutron-irradiated HOPG sample was compressed to 15 GPa at room temperature and then the temperature was increased up to 1500 °C. X-ray diffraction, high-resolution transmission electron microscopy on the recovered sample clearly showed the formation of a significant amount of quenchable-CG with ordinary graphite. Formation of hexagonal and cubic diamonds was also confirmed. The effect of irradiation-induced defects on the synthesis of quenchable-CG under high pressure and high temperature treatment was discussed.

  12. Enhancement of oxidation resistance of graphite foams by polymer derived-silicon carbide coating for concentrated solar power applications

    DOE PAGES

    Kim, T.; Singh, D.; Singh, M.

    2015-05-01

    Graphite foam with extremely high thermal conductivity has been investigated to enhance heat transfer of latent heat thermal energy storage (LHTES) systems. However, the use of graphite foam for elevated temperature applications (>600 °C) is limited due to poor oxidation resistance of graphite. In the present study, oxidation resistance of graphite foam coated with silicon carbide (SiC) was investigated. A pre-ceramic polymer derived coating (PDC) method was used to form a SiC coating on the graphite foams. Post coating deposition, the samples were analyzed by scanning electron microscopy and energy dispersive spectroscopy. The oxidation resistance of PDC-SiC coating was quantifiedmore » by measuring the weight of the samples at several measuring points. The experiments were conducted under static argon atmosphere in a furnace. After the experiments, oxidation rates (%/hour) were calculated to predict the lifetime of the graphite foams. The experimental results showed that the PDC-SiC coating could prevent the oxidation of graphite foam under static argon atmosphere up to 900 °C.« less

  13. Phase equilibrium in argon films stabilized by homogeneous surfaces and thermodynamics of two-stage melting transition.

    PubMed

    Ustinov, E A

    2014-02-21

    Freezing of gases adsorbed on open surfaces (e.g., graphite) and in narrow pores is a widespread phenomenon which is a subject of a large number of publications. Modeling of the gas/liquid-solid transition is usually accomplished with a molecular simulation technique. However, quantitative analysis of the gas/liquid-solid coexistence and thermodynamic properties of the solid layer still encounters serious difficulties. This is mainly due to the effect of simulation box size on the lattice constant. Since the lattice constant is a function of loading and temperature, once the ordering transition has occurred, the simulation box size must be corrected in the course of simulation according to the Gibbs-Duhem equation. A significant problem is also associated with accurate prediction of the two-dimensional liquid-solid coexistence because of a small difference in densities of coexisting phases. The aim of this study is thermodynamic analysis of the two-dimensional phase coexistence in systems involving crystal-like free of defects layers in narrow slit pores. A special attention was paid to the determination of triple point temperatures. It is shown that intrinsic properties of argon monolayer adsorbed on the graphite surface are similar to those of isolated monolayer accommodated in the slit pore having width of two argon collision diameters. Analysis of the latter system is shown to be clearer and less time-consuming than the former one, which has allowed for explanation of the experimentally observed two-stage melting transition of argon monolayer on graphite without invoking the periodic surface potential modulation and orientational transition.

  14. Phase equilibrium in argon films stabilized by homogeneous surfaces and thermodynamics of two-stage melting transition

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

    Ustinov, E. A., E-mail: eustinov@mail.wplus.net

    Freezing of gases adsorbed on open surfaces (e.g., graphite) and in narrow pores is a widespread phenomenon which is a subject of a large number of publications. Modeling of the gas/liquid–solid transition is usually accomplished with a molecular simulation technique. However, quantitative analysis of the gas/liquid–solid coexistence and thermodynamic properties of the solid layer still encounters serious difficulties. This is mainly due to the effect of simulation box size on the lattice constant. Since the lattice constant is a function of loading and temperature, once the ordering transition has occurred, the simulation box size must be corrected in the coursemore » of simulation according to the Gibbs–Duhem equation. A significant problem is also associated with accurate prediction of the two-dimensional liquid–solid coexistence because of a small difference in densities of coexisting phases. The aim of this study is thermodynamic analysis of the two-dimensional phase coexistence in systems involving crystal-like free of defects layers in narrow slit pores. A special attention was paid to the determination of triple point temperatures. It is shown that intrinsic properties of argon monolayer adsorbed on the graphite surface are similar to those of isolated monolayer accommodated in the slit pore having width of two argon collision diameters. Analysis of the latter system is shown to be clearer and less time-consuming than the former one, which has allowed for explanation of the experimentally observed two-stage melting transition of argon monolayer on graphite without invoking the periodic surface potential modulation and orientational transition.« less

  15. Rapid analysis method for the determination of 14C specific activity in irradiated graphite

    PubMed Central

    Remeikis, Vidmantas; Lagzdina, Elena; Garbaras, Andrius; Gudelis, Arūnas; Garankin, Jevgenij; Juodis, Laurynas; Duškesas, Grigorijus; Lingis, Danielius; Abdulajev, Vladimir; Plukis, Artūras

    2018-01-01

    14C is one of the limiting radionuclides used in the categorization of radioactive graphite waste; this categorization is crucial in selecting the appropriate graphite treatment/disposal method. We propose a rapid analysis method for 14C specific activity determination in small graphite samples in the 1–100 μg range. The method applies an oxidation procedure to the sample, which extracts 14C from the different carbonaceous matrices in a controlled manner. Because this method enables fast online measurement and 14C specific activity evaluation, it can be especially useful for characterizing 14C in irradiated graphite when dismantling graphite moderator and reflector parts, or when sorting radioactive graphite waste from decommissioned nuclear power plants. The proposed rapid method is based on graphite combustion and the subsequent measurement of both CO2 and 14C, using a commercial elemental analyser and the semiconductor detector, respectively. The method was verified using the liquid scintillation counting (LSC) technique. The uncertainty of this rapid method is within the acceptable range for radioactive waste characterization purposes. The 14C specific activity determination procedure proposed in this study takes approximately ten minutes, comparing favorably to the more complicated and time consuming LSC method. This method can be potentially used to radiologically characterize radioactive waste or used in biomedical applications when dealing with the specific activity determination of 14C in the sample. PMID:29370233

  16. Rapid analysis method for the determination of 14C specific activity in irradiated graphite.

    PubMed

    Remeikis, Vidmantas; Lagzdina, Elena; Garbaras, Andrius; Gudelis, Arūnas; Garankin, Jevgenij; Plukienė, Rita; Juodis, Laurynas; Duškesas, Grigorijus; Lingis, Danielius; Abdulajev, Vladimir; Plukis, Artūras

    2018-01-01

    14C is one of the limiting radionuclides used in the categorization of radioactive graphite waste; this categorization is crucial in selecting the appropriate graphite treatment/disposal method. We propose a rapid analysis method for 14C specific activity determination in small graphite samples in the 1-100 μg range. The method applies an oxidation procedure to the sample, which extracts 14C from the different carbonaceous matrices in a controlled manner. Because this method enables fast online measurement and 14C specific activity evaluation, it can be especially useful for characterizing 14C in irradiated graphite when dismantling graphite moderator and reflector parts, or when sorting radioactive graphite waste from decommissioned nuclear power plants. The proposed rapid method is based on graphite combustion and the subsequent measurement of both CO2 and 14C, using a commercial elemental analyser and the semiconductor detector, respectively. The method was verified using the liquid scintillation counting (LSC) technique. The uncertainty of this rapid method is within the acceptable range for radioactive waste characterization purposes. The 14C specific activity determination procedure proposed in this study takes approximately ten minutes, comparing favorably to the more complicated and time consuming LSC method. This method can be potentially used to radiologically characterize radioactive waste or used in biomedical applications when dealing with the specific activity determination of 14C in the sample.

  17. A Fluorinated Ether Electrolyte Enabled High Performance Prelithiated Graphite/Sulfur Batteries

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

    Chen, Shuru; Yu, Zhaoxin; Gordin, Mikhail L.

    Lithium/sulfur (Li/S) batteries have attracted great attention as a promising energy storage technology, but so far their practical applications are greatly hindered by issues of polysulfide shuttling and unstable lithium/electrolyte interface. To address these issues, a feasible strategy is to construct a rechargeable prelithiated graphite/sulfur batteries. In this study, a fluorinated ether of bis(2,2,2-trifluoroethyl) ether (BTFE) was reported to blend with 1,3-dioxolane (DOL) for making a multifunctional electrolyte of 1.0 M LiTFSI DOL/BTFE (1:1, v/v) to enable high performance prelithiated graphite/S batteries. First, the electrolyte significantly reduces polysulfide solubility to suppress the deleterious polysulfide shuttling and thus improves capacity retentionmore » of sulfur cathodes. Second, thanks to the low viscosity and good wettability, the fluorinated electrolyte dramatically enhances the reaction kinetics and sulfur utilization of high-areal-loading sulfur cathodes. More importantly, this electrolyte forms a stable solid-electrolyte interphase (SEI) layer on graphite surface and thus enables remarkable cyclability of graphite anodes. Lastly, by coupling prelithiated graphite anodes with sulfur cathodes with high areal capacity of ~3 mAh cm -2, we demonstrate prelithiated graphite/sulfur batteries that show high sulfur-specific capacity of ~1000 mAh g -1 and an excellent capacity retention of >65% after 450 cycles at C/10.« less

  18. Synthesis and characterization of SiC based composite materials for immobilizing radioactive graphite

    NASA Astrophysics Data System (ADS)

    Wang, Qing; Teng, Yuancheng; Wu, Lang; Zhang, Kuibao; Zhao, Xiaofeng; Hu, Zhuang

    2018-06-01

    In order to immobilize high-level radioactive graphite, silicon carbide based composite materials{ (1-x) SiC· x MgAl2O4 (0.1 ≤ x≤0.4) } were fabricated by solid-state reaction at 1370 °C for 2 h in vacuum. Residual graphite and precipitated corundum were observed in the as-synthesized product, which attributed to the interface reaction of element silicon and magnesium compounds. To further understand the reasons for the presence of graphite and corundum, the effects of mole ratio of Si/C, MgAl2O4 content and non-stoichiometry of MgAl2O4 on the synthesis were investigated. To immobilize graphite better, residual graphite should be eliminated. The target product was obtained when the mole ratio of Si/C was 1.3:1, MgAl2O4 content was x = 0.2, and the mole ratio of Al to Mg in non-stoichiometric MgAl2O4 was 1.7:1. In addition, the interface reaction between magnesium compounds and silicon not graphite was displayed by conducting a series of comparative experiments. The key factor for the occurrence of interface reaction is that oxygen atom is transferred from magnesium compound to SiO gas. Infrared and Raman spectrum revealed the increased disorders of graphite after being synthesized.

  19. A Fluorinated Ether Electrolyte Enabled High Performance Prelithiated Graphite/Sulfur Batteries

    DOE PAGES

    Chen, Shuru; Yu, Zhaoxin; Gordin, Mikhail L.; ...

    2017-02-03

    Lithium/sulfur (Li/S) batteries have attracted great attention as a promising energy storage technology, but so far their practical applications are greatly hindered by issues of polysulfide shuttling and unstable lithium/electrolyte interface. To address these issues, a feasible strategy is to construct a rechargeable prelithiated graphite/sulfur batteries. In this study, a fluorinated ether of bis(2,2,2-trifluoroethyl) ether (BTFE) was reported to blend with 1,3-dioxolane (DOL) for making a multifunctional electrolyte of 1.0 M LiTFSI DOL/BTFE (1:1, v/v) to enable high performance prelithiated graphite/S batteries. First, the electrolyte significantly reduces polysulfide solubility to suppress the deleterious polysulfide shuttling and thus improves capacity retentionmore » of sulfur cathodes. Second, thanks to the low viscosity and good wettability, the fluorinated electrolyte dramatically enhances the reaction kinetics and sulfur utilization of high-areal-loading sulfur cathodes. More importantly, this electrolyte forms a stable solid-electrolyte interphase (SEI) layer on graphite surface and thus enables remarkable cyclability of graphite anodes. Lastly, by coupling prelithiated graphite anodes with sulfur cathodes with high areal capacity of ~3 mAh cm -2, we demonstrate prelithiated graphite/sulfur batteries that show high sulfur-specific capacity of ~1000 mAh g -1 and an excellent capacity retention of >65% after 450 cycles at C/10.« less

  20. Dynamics of solid dispersions in oil during the lubrication of point contacts. Part 1: Graphite

    NASA Technical Reports Server (NTRS)

    Cusano, C.; Sliney, H. E.

    1981-01-01

    A Hertzian contact was lubricated with dispersed graphite in mineral oils under boundary lubrication conditions. The contact was optically observed under pure rolling, combined rolling and sliding, and pure sliding conditions. The contact was formed with a steel ball on the flat surface of a glass disk. Photomicrographs are presented which show the distribution of the graphite in and around the contact. Friction and surface damage are also shown for conditions when the base oils are used alone and when graphite is added to the base oils. Under pure rolling and combined rolling and sliding conditions, it is found that, for low speeds, a graphite film can form which will separate the contacting surfaces. Under pure sliding conditions, graphite accumulates at the inlet and sweeps around the contact, but very little of the graphite passes through the contact. The accumulated graphite appears to act as a barrier which reduces the supply of oil available to the contact for boundary lubrication. Friction data show no clear short term beneficial or detrimental effect caused by addition of graphite to the base oil. However, during pure sliding, more abrasion occurs on the polished balls lubricated with the dispersion than on those lubricated with the base oil alone. All observations were for the special case of a highly-polished ball on a glass surface and may not be applicable to other geometries and materials, or to rougher surfaces.

  1. Data Report on Post-Irradiation Dimensional Change of AGC-1 Samples

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

    William Windes

    This report summarizes the initial dimensional changes for loaded and unloaded AGC-1 samples. The dimensional change for all samples is presented as a function of dose. The data is further presented by graphite type and applied load levels to illustrate the differences between graphite forming processes and stress levels within the graphite components. While the three different loads placed on the samples have been verified [ ref: Larry Hull’s report] verification of the AGC-1 sample temperatures and dose levels are expected in the summer of 2012. Only estimated dose and temperature values for the samples are presented in this reportmore » to allow a partial analysis of the results.« less

  2. The radioactivity estimation of 14C and 3H in graphite waste samples of the KRR-2.

    PubMed

    Reyoung Kim, Hee

    2013-09-01

    The radioactivity of (14)C and (3)H in graphite samples from the dismantled Korea Research Reactor-2 (the KRR-2) site was analyzed by high-temperature oxidation and liquid scintillation counting, and the graphite waste was suggested to be disposed of as a low-level radioactive waste. The graphite samples were oxidized at a high temperature of 800 °C, and their counting rates were measured by using a liquid scintillation counter (LSC). The combustion ratio of the graphite was about 99% on the sample with a maximum weight of 1g. The recoveries from the combustion furnace were around 100% and 90% in (14)C and (3)H, respectively. The minimum detectable activity was 0.04-0.05 Bq/g for the (14)C and 0.13-0.15 Bq/g for the (3)H at the same background counting time. The activity of (14)C was higher than that of (3)H over all samples with the activity ratios of the (14)C to (3)H, (14)C/(3)H, being between 2.8 and 25. The dose calculation was carried out from its radioactivity analysis results. The dose estimation gave a higher annual dose than the domestic legal limit for a clearance. It was thought that the sampled graphite waste from the dismantled research reactor was not available for reuse or recycling and should be monitored as low-level radioactive waste. Copyright © 2013 Elsevier Ltd. All rights reserved.

  3. Literature Review: Materials with Negative Poisson’s Ratios and Potential Applications to Aerospace and Defence

    DTIC Science & Technology

    2006-08-01

    and defence industries. In fact, some materials with such anomalous (i.e. NPR) properties have been used in applications such as pyrolytic graphite...real applications such as pyrolytic graphite with NPR of -0.21 for thermal protection in aerospace (Garber, 1963), large single crystals of Ni3Al with...Foundations of Solid Mechanics, Prentice-Hall, p.353, 1968. Garber, A.M., Pyrolytic materials for thermal protection systems, Aerospace Eng., Vol

  4. Investigation of anti-wear and extreme pressure properties of nano-lubricant using graphite and Ag nanoparticles.

    PubMed

    Choi, Youngmin; Hwang, Yujin; Park, Minchan; Lee, Jaekeun; Choi, Cheol; Jung, Mihee; Oh, Jemyung; Lee, Jung Eun

    2011-01-01

    The tribological behavior of graphite and Ag nanoparticles as solid additive to base oil was evaluated on a four-ball test machine and a disc-on-disc tribotester. Extreme pressure and anti-wear results are shown according to ASTM D4172 and D2783 standard methods. It is found that Ag nanoparticles have better anti-wear behavior, and especially the smaller size nanoparticle have better anti-wear behavior.

  5. Mussel-Inspired Polydopamine Coating for Enhanced Thermal Stability and Rate Performance of Graphite Anodes in Li-Ion Batteries.

    PubMed

    Park, Seong-Hyo; Kim, Hyeon Jin; Lee, Junmin; Jeong, You Kyeong; Choi, Jang Wook; Lee, Hochun

    2016-06-08

    Despite two decades of commercial history, it remains very difficult to simultaneously achieve both high rate capability and thermal stability in the graphite anodes of Li-ion batteries because the stable solid electrolyte interphase (SEI) layer, which is essential for thermal stability, impedes facile Li(+) ion transport at the interface. Here, we resolve this longstanding challenge using a mussel-inspired polydopamine (PD) coating via a simple immersion process. The nanometer-thick PD coating layer allows the formation of an SEI layer on the coating surface without perturbing the intrinsic properties of the SEI layer of the graphite anodes. PD-coated graphite exhibits far better performances in cycling test at 60 °C and storage test at 90 °C than bare graphite. The PD-coated graphite also displays superior rate capability during both lithiation and delithiation. As evidenced by surface free energy analysis, the enhanced performance of the PD-coated graphite can be ascribed to the Lewis basicity of the PD, which scavenges harmful hydrofluoric acid and forms an intermediate triple-body complex among a Li(+) ion, solvent molecules, and the PD's basic site. The usefulness of the proposed PD coating can be expanded to various electrodes in rechargeable batteries that suffer from poor thermal stability and interfacial kinetics.

  6. A new graphite preparation line for AMS 14C dating in the Zagreb Radiocarbon Laboratory

    NASA Astrophysics Data System (ADS)

    Krajcar Bronić, I.; Horvatinčić, N.; Sironić, A.; Obelić, B.; Barešić, J.; Felja, I.

    2010-04-01

    The new line for preparation of graphite samples for 14C dating by AMS has been constructed in the Zagreb Radiocarbon Laboratory. The performance of the rig and sample preparation procedure has been validated by preparing graphites from various reference materials of known 14C activity. The yield of the graphitization was good and the measured fraction of modern carbon ( Fm) values have not significantly deviated from the expected ones. Detailed analysis of measured Fm values indicates a slight bias to more positive values and should be carefully investigated.

  7. Arc ignition at heating of graphite by fixed current

    NASA Astrophysics Data System (ADS)

    Polistchook, V. P.; Samoylov, I. S.; Amirov, R. Kh; Kiselev, V. I.

    2017-11-01

    Arc ignition after the destruction of graphite samples under prolonged heating by electric current was described. Evidences of liquid film formation on the graphite surface at a temperature of 3.3 kK were presented.

  8. EFFECT OF MASSIVE NEUTRON EXPOSURE ON THE DISTORTION OF REACTOR GRAPHITE

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

    Helm, J.W.; Davidson, J.M.

    1963-05-28

    Distortion of reactor-grade graphites was studied at varying neutron exposures ranging up to 14 x 10/sup 21/ neutrons per cm/sup 2/ (nvt)/sup */ at temperatures of irradiation ranging from 425 to 800 deg C. This exposure level corresponds to approximately 100,000 megawatt days per adjacent ton of fuel (Mwd/ At) in a graphite-moderated reactor. A conventionalcoke graphite, CSF, and two needle-coke graphites, NC-7 and NC-8, were studied. At all temperatures of irradiation the contraction rate of the samples cut parallel to the extrusion axis increased with increasing neutron exposure. For parallel samples the needle- coke graphites and the CSF graphitemore » contracted approximately the same amount. In the transverse direction the rate of cortraction at the higher irradiation temperntures appeared to be decreasing. Volume contractions derived from the linear contractions are discussed. (auth)« less

  9. GUM Analysis for TIMS and SIMS Isotopic Ratios in Graphite

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

    Heasler, Patrick G.; Gerlach, David C.; Cliff, John B.

    2007-04-01

    This report describes GUM calculations for TIMS and SIMS isotopic ratio measurements of reactor graphite samples. These isotopic ratios are used to estimate reactor burn-up, and currently consist of various ratios of U, Pu, and Boron impurities in the graphite samples. The GUM calculation is a propagation of error methodology that assigns uncertainties (in the form of standard error and confidence bound) to the final estimates.

  10. Sensitive Determination of Cd in Small-Volume Samples by Miniaturized Liquid Drop Anode Atmospheric Pressure Glow Discharge Optical Emission Spectrometry.

    PubMed

    Jamroz, Piotr; Greda, Krzysztof; Dzimitrowicz, Anna; Swiderski, Krzysztof; Pohl, Pawel

    2017-06-06

    A novel liquid drop anode (LDA) direct current atmospheric pressure glow discharge (dc-APGD) system was applied for direct determination of Cd in liquid microsamples (50 μL) by optical emission spectrometry (OES). The microdischarge was generated in open-to-air atmosphere between a solid pin type tungsten cathode and a liquid drop placed on a graphite disk anode. The arrangement of the graphite disk placed on a PTFE chip platform as well as the solid pin type cathode was simple and robust. The limit of detection (LOD) of Cd for the developed LDA-APGD-OES method was 0.20-0.40 μg L -1 , while precision (as the relative standard deviation for the repeated measurements) was within 2-5%. By using the liquid drop of 50 μL, the linearity range of 1-1000 μg L -1 was achieved. The effect of addition of the low-molecular weight (LMW) organic compounds, easily ionized elements (EIEs), i.e., Ca, K, Mg, and Na, as well as the foreign ions (Al, Cu, Fe, Mn, Zn) to the solution on the in situ atomization and excitation processes occurred during operation of the LDA-APGD system, and the response of Cd was studied. Validation of the proposed method was demonstrated by analysis of Lobster hepatopancreas (TORT-2), pig kidney (ERM-BB186), and groundwater (ERM-CA615) certified reference materials (CRMs) and recoveries of Cd from water samples spiked with 25 μg L -1 of Cd. Very good agreement between the found and certified values of Cd in the CRMs (the recoveries were within the range of 96.3-99.6%) indicated trueness of the method and its reliability for determination of traces of Cd. In the case of the spiked water samples, the recoveries obtained were in the range from 95.2 to 99.5%.

  11. Conformationally pre-organized and pH-responsive flat dendrons: synthesis and self-assembly at the liquid-solid interface.

    PubMed

    El Malah, Tamer; Ciesielski, Artur; Piot, Luc; Troyanov, Sergey I; Mueller, Uwe; Weidner, Steffen; Samorì, Paolo; Hecht, Stefan

    2012-01-21

    Efficient Cu-catalyzed 1,3-dipolar cycloaddition reactions have been used to prepare two series of three regioisomers of G-1 and G-2 poly(triazole-pyridine) dendrons. The G-1 and G-2 dendrons consist of branched yet conformationally pre-organized 2,6-bis(phenyl/pyridyl-1,2,3-triazol-4-yl)pyridine (BPTP) monomeric and trimeric cores, respectively, carrying one focal and either two or four peripheral alkyl side chains. In the solid state, the conformation and supramolecular organization were studied by means of a single crystal X-ray structure analysis of one derivative. At the liquid-solid interface, the self-assembly behavior was investigated by scanning tunneling microscopy (STM) on graphite surfaces. Based on the observed supramolecular organization, it appears that the subtle balance between conformational preferences inherent in the dendritic backbone on the one side and the adsorption and packing of the alkyl side chains on the graphite substrate on the other side dictate the overall structure formation in 2D.

  12. 40 CFR 180.930 - Inert ingredients applied to animals; exemptions from the requirement of a tolerance.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... clay Solid diluent, carrier Barium sulfate (CAS Reg. No. 7727-43-7) Carrier, density control agent...-Difluoroethane (CAS Reg. No. 75-37-6) For aerosol pesticide formulations used for insect control in food- and... tris-12-hydroxystearate Flow control agent Graphite Solid diluent, carrier n-Hexyl alcohol (CAS Reg. No...

  13. Graphite fiber reinforced thermoplastic resins

    NASA Technical Reports Server (NTRS)

    Novak, R. C.

    1975-01-01

    Mechanical properties of neat resin samples and graphite fiber reinforced samples of thermoplastic resins were characterized with particular emphasis directed to the effects of environmental exposure (humidity, temperature and ultraviolet radiation). Tensile, flexural, interlaminar shear, creep and impact strengths were measured for polysulfone, polyarylsulfone and a state-of-the-art epoxy resin samples. In general, the thermoplastic resins exhibited environmental degradation resistance equal to or superior to the reference epoxy resin. Demonstration of the utility and quality of a graphite/thermoplastic resin system was accomplished by successfully thermoforming a simulated compressor blade and a fan exit guide vane.

  14. A contrastive study of three graphite anodes in the piperidinium based electrolytes for lithium ion batteries

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

    Jiang, Xiao-Tao; Wang, Chen-Yi; Gao, Kun, E-mail: gaokun0451@163.com

    Graphical abstract: The fitting results of R{sub sei} and R{sub ct} of three graphite/Li cells. Besides three graphite/Li cells show the similar R{sub sei}, the NG198/Li cell demonstrates a higher R{sub ct} value in all test temperatures. Especially, the R{sub ct} at 333 K is even up to 355.8 Ω cm{sup 2}. Obviously, the narrow distribution of edge plane for NG198 caused this result, and then greatly restricts its cell capacity. By contrast, CMB with bigger specific surface area and more Li{sup +} insertion points shows lower resistance at room temperature, which should help to improve its capacity. - Highlights:more » • SEI film is closely related to graphite structures and formation temperature. • The graphite with bigger surface area and more Li{sup +} insertion points behaves better. • The graphite with narrow edge plane is uncompetitive for ionic liquid electrolyte. - Abstract: The electrochemical behaviors of natural graphite (NG198), artificial graphite (AG360) and carbon microbeads (CMB) in an ionic liquid based electrolyte are investigated by cyclic voltammetry (CV). The surface and structure of three graphite materials are characterized by scanning electron microscope (SEM) and X-ray diffraction (XRD) before and after cycling. It is found that solid electrolyte interface (SEI) is closely related to graphite structure. Benefiting from larger specific surface area and more dispersed Li{sup +} insertion points, CMB shows a better Li{sup +} insertion/de-insertion behavior than NG198 and AG360. Furthermore, electrochemical impedance spectra (EIS) prove that the SEI of different graphite electrodes has different intrinsic resistance and Li{sup +} penetrability. By comparison, CMB behaves better cell performances than AG360, while the narrow edge plane makes NG198 uncompetitive as a potential anode for the ionic liquids (ILs)-type Li-ion battery.« less

  15. Simultaneous Determination of Perfluorinated Compounds in Edible Oil by Gel-Permeation Chromatography Combined with Dispersive Solid-Phase Extraction and Liquid Chromatography-Tandem Mass Spectrometry.

    PubMed

    Yang, Lili; Jin, Fen; Zhang, Peng; Zhang, Yanxin; Wang, Jian; Shao, Hua; Jin, Maojun; Wang, Shanshan; Zheng, Lufei; Wang, Jing

    2015-09-30

    A simple analytical method was developed for the simultaneous analysis of 18 perfluorinated compounds (PFCs) in edible oil. The target compounds were extracted by acetonitrile, purified by gel permeation chromatography (GPC) and dispersive solid-phase extraction (DSPE) using graphitized carbon black (GCB) and octadecyl (C18), and analyzed by liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ES-MS/MS) in negative ion mode. Recovery studies were performed at three fortification levels. The average recoveries of all target PFCs ranged from 60 to 129%, with an acceptable relative standard deviation (RSD) (1-20%, n = 3). The method detection limits (MDLs) ranged from 0.004 to 0.4 μg/kg, which was significantly improved compared with the existing liquid-liquid extraction and cleanup method. The method was successfully applied for the analysis of all target PFCs in edible oil samples collected from markets in Beijing, China, and the results revealed that C6-C10 perfluorocarboxylic acid (PFCAs) and C7 perfluorosulfonic acid PFSAs were the major PFCs detected in oil samples.

  16. Installation of hybrid ion source on the 1-MV LLNL BioAMS spectrometer

    PubMed Central

    Ognibene, T. J.; Salazar, G. A.

    2012-01-01

    A second ion source was recently installed onto the LLNL 1-MV AMS spectrometer, which is dedicated to the quantification of 14C and 3H within biochemical samples. This source is unique among the other LLNL cesium sputter ion sources in that it can ionize both gaseous and solid samples. Also, the injection beam line has been designed to directly measure 14C/12C isotope ratios without the need for electrostatic bouncing. Preliminary tests show that this source can ionize transient CO2 gas pulses containing less than 1 ug carbon with approximately 1.5% efficiency. We demonstrate that the measured 14C/12C isotope ratio is largely unaffected by small drifts in the argon stripper gas density. We also determine that a tandem accelerating voltage of 670 kV enables the highest 14C transmission through the system. Finally, we describe a series of performance tests using solid graphite targets spanning nearly 3 orders in magnitude dynamic range and compare the results to our other ion source. PMID:23467295

  17. Application of multiwall carbon nanotubes-based matrix solid phase dispersion extraction for determination of hormones in butter by gas chromatography mass spectrometry.

    PubMed

    Su, Rui; Wang, Xinghua; Xu, Xu; Wang, Ziming; Li, Dan; Zhao, Xin; Li, Xueyuan; Zhang, Hanqi; Yu, Aimin

    2011-08-05

    The multiwall carbon nanotubes (MWCNTs)-based matrix solid phase dispersion (MSPD) was applied for the extraction of hormones, including 17-α-ethinylestradiol, 17-α-estradiol, estriol, 17-β-estradiol, estrone, medroxyprogesterone, progesterone and norethisterone acetate in butter samples. The method includes MSPD extraction of the target analytes from butter samples, derivatization of hormones with heptafluorobutyric acid anhydride-acetonitrile mixture, and determination by gas chromatography-mass spectrometry. The mixture containing 0.30 g graphitized MWCNTs and 0.10 g MWCNTs was selected as absorbent. Ethyl acetate was used as elution solvent. The elution solvent volume and flow rate were 12 mL and 0.9 mL min(-1), respectively. The recoveries of hormones obtained by analyzing the five spiked butter samples were from 84.5 to 111.2% and relative standard deviations from 1.9 to 8.9%. Limits of detection and quantification for determining the analytes were in the range of 0.2-1.3 and 0.8-4.5 μg kg(-1), respectively. Compared with other traditional methods, the proposed method is simpler in the operation and shorter in the sample pretreatment time. Copyright © 2011 Elsevier B.V. All rights reserved.

  18. Controlling Fundamentals in High-Energy High-Rate Pulsed Power Materials Processing of Powdered Tungsten, Titanium Aluminides, and Copper-Graphite Composites

    DTIC Science & Technology

    1990-10-01

    phase systems such as tungsten; plastic flow of a minor low -temperature phase in a two phase non-interacting system such as tungsten- copper ; and...consolidation heat treatment. The de- the wetting of graphite by copper or during consolidation by this tech- tailed phase transformation evolution other...The driving potential for this solid state phase transformation is the free surface energy associated with the total powder particle surface area in the

  19. SEM/XPS analysis of fractured adhesively bonded graphite fibre surface resin-rich/graphite fibre composites

    NASA Technical Reports Server (NTRS)

    Devilbiss, T. A.; Wightman, J. P.; Progar, D. J.

    1988-01-01

    Samples of graphite fiber-reinforced polyimide were fabricated allowing the resin to accumulate at the composite surface. These surface resin-rich composites were then bonded together and tested for lap shear strength both before and after thermal aging. Lap shear strength did not appear to show a significant improvement over that previously recorded for resin-poor samples and was shown to decrease with increasing aging time and temperature.

  20. Measurement of absorbed dose with a bone-equivalent extrapolation chamber.

    PubMed

    DeBlois, François; Abdel-Rahman, Wamied; Seuntjens, Jan P; Podgorsak, Ervin B

    2002-03-01

    A hybrid phantom-embedded extrapolation chamber (PEEC) made of Solid Water and bone-equivalent material was used for determining absorbed dose in a bone-equivalent phantom irradiated with clinical radiation beams (cobalt-60 gamma rays; 6 and 18 MV x rays; and 9 and 15 MeV electrons). The dose was determined with the Spencer-Attix cavity theory, using ionization gradient measurements and an indirect determination of the chamber air-mass through measurements of chamber capacitance. The collected charge was corrected for ionic recombination and diffusion in the chamber air volume following the standard two-voltage technique. Due to the hybrid chamber design, correction factors accounting for scatter deficit and electrode composition were determined and applied in the dose equation to obtain absorbed dose in bone for the equivalent homogeneous bone phantom. Correction factors for graphite electrodes were calculated with Monte Carlo techniques and the calculated results were verified through relative air cavity dose measurements for three different polarizing electrode materials: graphite, steel, and brass in conjunction with a graphite collecting electrode. Scatter deficit, due mainly to loss of lateral scatter in the hybrid chamber, reduces the dose to the air cavity in the hybrid PEEC in comparison with full bone PEEC by 0.7% to approximately 2% depending on beam quality and energy. In megavoltage photon and electron beams, graphite electrodes do not affect the dose measurement in the Solid Water PEEC but decrease the cavity dose by up to 5% in the bone-equivalent PEEC even for very thin graphite electrodes (<0.0025 cm). In conjunction with appropriate correction factors determined with Monte Carlo techniques, the uncalibrated hybrid PEEC can be used for measuring absorbed dose in bone material to within 2% for high-energy photon and electron beams.

  1. Synthesis and characterization of nanocrystalline graphite from coconut shell with heating process

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

    Wachid, Frischa M., E-mail: frischamw@yahoo.com, E-mail: adhiyudhaperkasa@yahoo.com, E-mail: afandisar@yahoo.com, E-mail: nurulrosyidah92@gmail.com, E-mail: darminto@physics.its.ac.id; Perkasa, Adhi Y., E-mail: frischamw@yahoo.com, E-mail: adhiyudhaperkasa@yahoo.com, E-mail: afandisar@yahoo.com, E-mail: nurulrosyidah92@gmail.com, E-mail: darminto@physics.its.ac.id; Prasetya, Fandi A., E-mail: frischamw@yahoo.com, E-mail: adhiyudhaperkasa@yahoo.com, E-mail: afandisar@yahoo.com, E-mail: nurulrosyidah92@gmail.com, E-mail: darminto@physics.its.ac.id

    Graphite were synthesized and characterized by heating process of coconut shell with varying temperature (400, 800 and 1000°C) and holding time (3 and 5 hours). After heating process, the samples were characterized by X-ray diffraction (XRD) and analyzed by X'pert HighScore Plus Software, Scanning Electron Microcope-Energy Dispersive X-Ray (SEM-EDX) and Transmission Electron Microscope-Energy Dispersive X-Ray (TEM-EDX). Graphite and londsdaelite phase were analyzed by XRD. According to EDX analysis, the sample was heated in 1000°C got the highest content of carbon. The amorphous carbon and nanocrystalline graphite were observed by SEM-EDX and TEM-EDX.

  2. Structural changes in a commercial lithium-ion battery during electrochemical cycling: An in situ neutron diffraction study

    NASA Astrophysics Data System (ADS)

    Sharma, Neeraj; Peterson, Vanessa K.; Elcombe, Margaret M.; Avdeev, Maxim; Studer, Andrew J.; Blagojevic, Ned; Yusoff, Rozila; Kamarulzaman, Norlida

    The structural response to electrochemical cycling of the components within a commercial Li-ion battery (LiCoO 2 cathode, graphite anode) is shown through in situ neutron diffraction. Lithuim insertion and extraction is observed in both the cathode and anode. In particular, reversible Li incorporation into both layered and spinel-type LiCoO 2 phases that comprise the cathode is shown and each of these components features several phase transitions attributed to Li content and correlated with the state-of-charge of the battery. At the anode, a constant cell voltage correlates with a stable lithiated graphite phase. Transformation to de-lithiated graphite at the discharged state is characterised by a sharp decrease in both structural cell parameters and cell voltage. In the charged state, a two-phase region exists and is composed of the lithiated graphite phase and about 64% LiC 6. It is postulated that trapping Li in the solid|electrolyte interface layer results in minimal structural changes to the lithiated graphite anode across the constant cell voltage regions of the electrochemical cycle.

  3. Effects of Propylene Carbonate Content in CsPF6-Containing Electrolytes on the Enhanced Performances of Graphite Electrode for Lithium-Ion Batteries

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

    Zheng, Jianming; Yan, Pengfei; Cao, Ruiguo

    2016-02-10

    Cesium salt has been demonstrated as an efficient electrolyte additive in suppressing the lithium (Li) dendrite formation and directing the formation of an ultrathin and stable solid electrolyte interphase (SEI) even in propylene carbonate (PC)-ethylene carbonate (EC)-based electrolytes. Here, we further investigate the effect of PC content in the presence of CsPF6 additive (0.05 M) on the performances of graphite electrode in Li||graphite half cells and in graphite||LiNi0.80Co0.15Al0.05O2 (NCA) full cells. It is found that the performance of graphite electrode is also affected by PC content even though CsPF6 additive is present in the electrolytes. An optimal PC content ofmore » 20% by weight in the solvent mixtures is identified. The enhanced electrochemical performance of graphite electrode is attributed to the synergistic effects of the Cs+ additive and the PC solvent. The formation of a robust, ultrathin and compact SEI layer containing lithium-enriched species on the graphite electrode, directed by Cs+, effectively suppresses the PC co-intercalation and thus prevents the graphite exfoliation. This SEI layer is only permeable for de-solvated Li+ ions and allows fast Li+ ion transport through it, which therefore largely alleviates the Li dendrite formation on graphite electrode during lithiation even at high current densities. The presence of low-melting-point PC solvent also enables the sustainable operation of the graphite||NCA full cells under a wide spectrum of temperatures. The fundamental findings of this work shed light on the importance of manipulating/maintaining the electrode/electrolyte interphasial stability in a variety of energy storage devices.« less

  4. Effects of Propylene Carbonate Content in CsPF 6 -Containing Electrolytes on the Enhanced Performances of Graphite Electrode for Lithium-Ion Batteries

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

    Zheng, Jianming; Yan, Pengfei; Cao, Ruiguo

    2016-02-15

    The effects Of propylene carbonate (PC) content in CsPF6-containing electrolytes on the performances of graphite electrode in lithium half cells and in graphite parallel to LiNi0.80Co0.15Al0.05O2 (NCA) full cells are investigated. It is found that the performance of graphite electrode is significantly-affected by PC content in the CsPF6-containing electrolytes. An optimal PC content of 20% by weight in the solvent mixtures is identified. The enhanced electrochemical performance of graphite electrode can be attributed to the synergistic effects of the PC solvent and the Cs+ additive. The synergistic effects of Cs+ additive and appropriate amount of PC enable the formation ofmore » a robust, ultrathin, and compact solid electrolyte interphase (SEI) layer on the surface of graphite electrode, which is only permeable for desolvated Li+ ions and allows fast Li+ ion transport through it. Therefore, this SEI layer effectively suppresses the PC cointercalation and largely alleviates the Li dendrite formation on graphite electrode during lithiation even at relatively high current densities. The presence of low-melting-point PC solvent improves the sustainable operation of graphite parallel to NCA full cells under a wide temperature range. The fundamental findings also shed light On the importance of manipulating/maintaining the electrode/electrolyte interphasial stability in various energy-storage devices.« less

  5. Highly Flexible and Planar Supercapacitors Using Graphite Flakes/Polypyrrole in Polymer Lapping Film.

    PubMed

    Raj, C Justin; Kim, Byung Chul; Cho, Won-Je; Lee, Won-gil; Jung, Sang-Don; Kim, Yong Hee; Park, Sang Yeop; Yu, Kook Hyun

    2015-06-24

    Flexible supercapacitor electrodes have been fabricated by simple fabrication technique using graphite nanoflakes on polymer lapping films as flexible substrate. An additional thin layer of conducting polymer polypyrrole over the electrode improved the surface conductivity and exhibited excellent electrochemical performances. Such capacitor films showed better energy density and power density with a maximum capacitance value of 37 mF cm(-2) in a half cell configuration using 1 M H2SO4 electrolyte, 23 mF cm(-2) in full cell, and 6 mF cm(-2) as planar cell configuration using poly(vinyl alcohol) (PVA)/phosphoric acid (H3PO4) solid state electrolyte. Moreover, the graphite nanoflakes/polypyrrole over polymer lapping film demonstrated good flexibility and cyclic stability.

  6. Self-assembled monolayers of shape-persistent macrocycles on graphite: interior design and conformational polymorphism.

    PubMed

    Vollmeyer, Joscha; Eberhagen, Friederike; Höger, Sigurd; Jester, Stefan-S

    2014-01-01

    Three shape-persistent naphthylene-phenylene-acetylene macrocycles of identical backbone structures and extraannular substitution patterns but different (empty, apolar, polar) nanopore fillings are self-assembled at the solid/liquid interface of highly oriented pyrolytic graphite and 1,2,4-trichlorobenzene. Submolecularly resolved images of the resulting two-dimensional (2D) crystalline monolayer patterns are obtained by in situ scanning tunneling microscopy. A concentration-dependent conformational polymorphism is found, and open and more dense packing motifs are observed. For all three compounds alike lattice parameters are found, therefore the intermolecular macrocycle distances are mainly determined by their size and symmetry. This is an excellent example that the graphite acts as a template for the macrocycle organization independent from their specific interior.

  7. Examination of Surface Deposits on Oldbury Reactor Core Graphite to Determine the Concentration and Distribution of 14C.

    PubMed

    Payne, Liam; Heard, Peter J; Scott, Thomas B

    2016-01-01

    Pile Grade A graphite was used as a moderator and reflector material in the first generation of UK Magnox nuclear power reactors. As all of these reactors are now shut down there is a need to examine the concentration and distribution of long lived radioisotopes, such as 14C, to aid in understanding their behaviour in a geological disposal facility. A selection of irradiated graphite samples from Oldbury reactor one were examined where it was observed that Raman spectroscopy can distinguish between underlying graphite and a surface deposit found on exposed channel wall surfaces. The concentration of 14C in this deposit was examined by sequentially oxidising the graphite samples in air at low temperatures (450°C and 600°C) to remove the deposit and then the underlying graphite. The gases produced were captured in a series of bubbler solutions that were analysed using liquid scintillation counting. It was observed that the surface deposit was relatively enriched with 14C, with samples originating lower in the reactor exhibiting a higher concentration of 14C. Oxidation at 600°C showed that the remaining graphite material consisted of two fractions of 14C, a surface associated fraction and a graphite lattice associated fraction. The results presented correlate well with previous studies on irradiated graphite that suggest there are up to three fractions of 14C; a readily releasable fraction (corresponding to that removed by oxidation at 450°C in this study), a slowly releasable fraction (removed early at 600°C in this study), and an unreleasable fraction (removed later at 600°C in this study).

  8. Examination of Surface Deposits on Oldbury Reactor Core Graphite to Determine the Concentration and Distribution of 14C

    PubMed Central

    Payne, Liam; Heard, Peter J.; Scott, Thomas B.

    2016-01-01

    Pile Grade A graphite was used as a moderator and reflector material in the first generation of UK Magnox nuclear power reactors. As all of these reactors are now shut down there is a need to examine the concentration and distribution of long lived radioisotopes, such as 14C, to aid in understanding their behaviour in a geological disposal facility. A selection of irradiated graphite samples from Oldbury reactor one were examined where it was observed that Raman spectroscopy can distinguish between underlying graphite and a surface deposit found on exposed channel wall surfaces. The concentration of 14C in this deposit was examined by sequentially oxidising the graphite samples in air at low temperatures (450°C and 600°C) to remove the deposit and then the underlying graphite. The gases produced were captured in a series of bubbler solutions that were analysed using liquid scintillation counting. It was observed that the surface deposit was relatively enriched with 14C, with samples originating lower in the reactor exhibiting a higher concentration of 14C. Oxidation at 600°C showed that the remaining graphite material consisted of two fractions of 14C, a surface associated fraction and a graphite lattice associated fraction. The results presented correlate well with previous studies on irradiated graphite that suggest there are up to three fractions of 14C; a readily releasable fraction (corresponding to that removed by oxidation at 450°C in this study), a slowly releasable fraction (removed early at 600°C in this study), and an unreleasable fraction (removed later at 600°C in this study). PMID:27706228

  9. Improved graphite furnace atomizer

    DOEpatents

    Siemer, D.D.

    1983-05-18

    A graphite furnace atomizer for use in graphite furnace atomic absorption spectroscopy is described wherein the heating elements are affixed near the optical path and away from the point of sample deposition, so that when the sample is volatilized the spectroscopic temperature at the optical path is at least that of the volatilization temperature, whereby analyteconcomitant complex formation is advantageously reduced. The atomizer may be elongated along its axis to increase the distance between the optical path and the sample deposition point. Also, the atomizer may be elongated along the axis of the optical path, whereby its analytical sensitivity is greatly increased.

  10. Finite Element Simulation of Solid Rocket Booster Separation Motors During Motor Firing

    NASA Technical Reports Server (NTRS)

    Yu. Weiping; Crane, Debora J.

    2007-01-01

    One of the toughest challenges facing Solid Rocket Booster (SRB) engineers is to ensure that any design changes made to the Shuttle-Derived Booster Separation Motors (BSM) for future space exploration vehicles is able to withstand the increasingly hostile motor firing environment without cracking its critical component - the graphite throat. This paper presents a critical analysis methodology and techniques for assessing effects of BSM design changes with great accuracy and precision. For current Space Shuttle operation, the motor firing occurs at SRB separation - approximately 125 seconds after Shuttle launch at an altitude of about 28 miles. The motor operation event lasts about two seconds, however, the surface temperature of the graphite throat increases approximately 3400 F in less than one second with a corresponding increase in surface pressure of approximately 2200 pounds per square inch (psi) in less than one-tenth of a second. To capture this process fully and accurately, a two-phase sequentially coupled thermal-mechanical finite element approach was developed. This method allows the time- and location-dependent pressure fields to interact with the spatial-temporal thermal fields throughout the operation. The material properties of graphite throat are orthotropic and temperature-dependent. The analysis involves preload and multiple body contacts.

  11. Lithium dendrite and solid electrolyte interphase investigation using OsO4

    NASA Astrophysics Data System (ADS)

    Zier, Martin; Scheiba, Frieder; Oswald, Steffen; Thomas, Jürgen; Goers, Dietrich; Scherer, Torsten; Klose, Markus; Ehrenberg, Helmut; Eckert, Jürgen

    2014-11-01

    Osmium tetroxide (OsO4) staining, commonly used to enhance scattering contrast in electron microscopy of biologic tissue and polymer blends, has been adopted for studies of graphite anodes in lithium-ion batteries. OsO4 shows a coordinated reaction with components of the solid electrolyte interphase (SEI) and lithium dendrites, thereby increasing material contrast for scanning electron microscopy investigations. Utilizing the high affinity of lithium metal to react with osmium tetroxide it was possible to localize even small lithium deposits on graphite electrodes. In spite of their reaction with the OsO4 fume, the lithium dendrite morphology remains almost untouched by the staining procedure, offering information on the dendrite growth process. Correlating the quantity of osmium detected with the amount of residual ("dead") lithium of a discharged electrode, it was possible to obtain a practical measure for lithium plating and stripping efficiencies. EDX mappings allowed for a localization of electrochemically stripped lithium dendrites by their residual stained SEI shells. Cross sections, prepared by focused ion beam (FIB) of cycled graphite electrodes treated with OsO4, revealed important information about deposition and distribution of metallic lithium and the electrolyte reduction layer across the electrode.

  12. Burning characteristics and fiber retention of graphite/resin matrix composites

    NASA Technical Reports Server (NTRS)

    Bowles, K. J.

    1980-01-01

    Graphite fiber reinforced resin matrix composites were subjected to controlled burning conditions to determine their burning characteristics and fiber retention properties. Small samples were burned with a natural gas fired torch to study the effects of fiber orientation and structural flaws such as holes and slits that were machined into the laminates. Larger laminate samples were burned in a modified heat release rate calorimeter. Unidirectional epoxy/graphite and polyimide/graphite composites and boron powder filled samples of each of the two composite systems were burn tested. The composites were exposed to a thermal radiation of 5.3 Btu/sq ft-sec in air. Samples of each of the unfilled composite were decomposed anaerobically in the calorimeter. Weight loss data were recorded for burning and decomposition times up to thirty-five minutes. The effects of fiber orientation, flaws, and boron filler additives to the resins were evaluated. A high char forming polyimide resin was no more effective in retaining graphite fibers than a low char forming epoxy resin when burned in air. Boron powder additions to both the polyimide and the epoxy resins stabilized the chars and effectively controlled the fiber release.

  13. Durability of Intercalated Graphite Epoxy Composites in Low Earth Orbit

    NASA Technical Reports Server (NTRS)

    Gaier, James R.; Davidson, Michelle L.; Shively, Rhonda

    1996-01-01

    The electrical conductivity of graphite epoxy composites can be substantially increased by intercalating (inserting guest atoms or molecules between the graphene planes) the graphite fibers before composite formation. The resulting high strength, low density, electrically conducting composites have been proposed for EMI shielding in spacecraft. Questions have been raised, however, about their durability in the space environment, especially with respect to outgassing of the intercalates, which are corrosive species such as bromine. To answer those concerns, six samples of bromine intercalated graphite epoxy composites were included in the third Evaluation of Oxygen Interaction with Materials (EOIM-3) experiment flown on the Space Shuttle Discovery (STS-46). Changes in electrical conductivity, optical reflectance, surface texture, and mass loss for SiO2 protected and unprotected samples were measured after being exposed to the LEO environment for 42 hours. SiO2 protected samples showed no degradation, verifying conventional protection strategies are applicable to bromine intercalated composites. The unprotected samples showed that bromine intercalation does not alter the degradation of graphite-epoxy composites. No bromine was detected to have been released by the fibers allaying fears that outgassing could be disruptive to the sensitive electronics the EMI shield is meant to protect.

  14. Chemically reduced graphene contains inherent metallic impurities present in parent natural and synthetic graphite.

    PubMed

    Ambrosi, Adriano; Chua, Chun Kiang; Khezri, Bahareh; Sofer, Zdeněk; Webster, Richard D; Pumera, Martin

    2012-08-07

    Graphene-related materials are in the forefront of nanomaterial research. One of the most common ways to prepare graphenes is to oxidize graphite (natural or synthetic) to graphite oxide and exfoliate it to graphene oxide with consequent chemical reduction to chemically reduced graphene. Here, we show that both natural and synthetic graphite contain a large amount of metallic impurities that persist in the samples of graphite oxide after the oxidative treatment, and chemically reduced graphene after the chemical reduction. We demonstrate that, despite a substantial elimination during the oxidative treatment of graphite samples, a significant amount of impurities associated to the chemically reduced graphene materials still remain and alter their electrochemical properties dramatically. We propose a method for the purification of graphenes based on thermal treatment at 1,000 °C in chlorine atmosphere to reduce the effect of such impurities on the electrochemical properties. Our findings have important implications on the whole field of graphene research.

  15. Chemically reduced graphene contains inherent metallic impurities present in parent natural and synthetic graphite

    PubMed Central

    Ambrosi, Adriano; Chua, Chun Kiang; Khezri, Bahareh; Sofer, Zdeněk; Webster, Richard D.; Pumera, Martin

    2012-01-01

    Graphene-related materials are in the forefront of nanomaterial research. One of the most common ways to prepare graphenes is to oxidize graphite (natural or synthetic) to graphite oxide and exfoliate it to graphene oxide with consequent chemical reduction to chemically reduced graphene. Here, we show that both natural and synthetic graphite contain a large amount of metallic impurities that persist in the samples of graphite oxide after the oxidative treatment, and chemically reduced graphene after the chemical reduction. We demonstrate that, despite a substantial elimination during the oxidative treatment of graphite samples, a significant amount of impurities associated to the chemically reduced graphene materials still remain and alter their electrochemical properties dramatically. We propose a method for the purification of graphenes based on thermal treatment at 1,000 °C in chlorine atmosphere to reduce the effect of such impurities on the electrochemical properties. Our findings have important implications on the whole field of graphene research. PMID:22826262

  16. Dynamic Mechanical Properties of Bio-Polymer Graphite Thin Films

    NASA Astrophysics Data System (ADS)

    Saddam Kamarudin, M.; Rus, Anika Zafiah M.; Munirah Abdullah, Nur; Abdullah, M. F. L.

    2017-08-01

    Waste cooking oil is used as the main substances in producing graphite biopolymer thin films. Biopolymer is produce from the reaction of bio-monomer and cross linker with the ratio of 2:1 and addition of graphite with an increment of 2% through a slip casting method. The morphological surface properties of the samples are observed by using Scanning Electron Microscope (SEM). It is shown that the graphite particle is well mixed and homogenously dispersed in biopolymer matrix. Meanwhile, the mechanical response of materials by monitoring the change in the material properties in terms of frequency and temperature of the samples were determined using Dynamic Mechanical Analysis (DMA). The calculated cross-linked density of biopolymer composites revealed the increment of graphite particle loading at 8% gives highest results with 260.012 x 103 M/m3.

  17. Processing of solid solution, mixed uranium/refractory metal carbides for advanced space nuclear power and propulsion systems

    NASA Astrophysics Data System (ADS)

    Knight, Travis Warren

    Nuclear thermal propulsion (NTP) and space nuclear power are two enabling technologies for the manned exploration of space and the development of research outposts in space and on other planets such as Mars. Advanced carbide nuclear fuels have been proposed for application in space nuclear power and propulsion systems. This study examined the processing technologies and optimal parameters necessary to fabricate samples of single phase, solid solution, mixed uranium/refractory metal carbides. In particular, the pseudo-ternary carbide, UC-ZrC-NbC, system was examined with uranium metal mole fractions of 5% and 10% and corresponding uranium densities of 0.8 to 1.8 gU/cc. Efforts were directed to those methods that could produce simple geometry fuel elements or wafers such as those used to fabricate a Square Lattice Honeycomb (SLHC) fuel element and reactor core. Methods of cold uniaxial pressing, sintering by induction heating, and hot pressing by self-resistance heating were investigated. Solid solution, high density (low porosity) samples greater than 95% TD were processed by cold pressing at 150 MPa and sintering above 2600 K for times longer than 90 min. Some impurity oxide phases were noted in some samples attributed to residual gases in the furnace during processing. Also, some samples noted secondary phases of carbon and UC2 due to some hyperstoichiometric powder mixtures having carbon-to-metal ratios greater than one. In all, 33 mixed carbide samples were processed and analyzed with half bearing uranium as ternary carbides of UC-ZrC-NbC. Scanning electron microscopy, x-ray diffraction, and density measurements were used to characterize samples. Samples were processed from powders of the refractory mono-carbides and UC/UC 2 or from powders of uranium hydride (UH3), graphite, and refractory metal carbides to produce hypostoichiometric mixed carbides. Samples processed from the constituent carbide powders and sintered at temperatures above the melting point of UC showed signs of liquid phase sintering and were shown to be largely solid solutions. Pre-compaction of mixed carbide powders prior to sintering was shown to be necessary to achieve high densities. Hypostoichiometric, samples processed at 2500 K exhibited only the initial stage of sintering and solid solution formation. Based on these findings, a suggested processing methodology is proposed for producing high density, solid solution, mixed carbide fuels. Pseudo-binary, refractory carbide samples hot pressed at 3100 K and 6 MPa showed comparable densities (approximately 85% of the theoretical value) to samples processed by cold pressing and sintering at temperatures of 2800 K.

  18. Transformation of graphite by tectonic and hydrothermal processes in an active plate boundary fault zone, Alpine Fault, New Zealand

    NASA Astrophysics Data System (ADS)

    Kirilova, Matina; Toy, Virginia; Timms, Nicholas; Halfpenny, Angela; Menzies, Catriona; Craw, Dave; Rooney, Jeremy; Giorgetti, Carolina

    2017-04-01

    Graphite is a material with one of the lowest frictional strengths, with coefficient of friction of 0.1 and thus in natural fault zones it may act as a natural solid lubricant. Graphitization, or the transformation of organic matter (carbonaceous material, or CM) into crystalline graphite, is induced by compositional and structural changes during diagenesis and metamorphism. The supposed irreversible nature of this process has allowed the degree of graphite crystallinity to be calibrated as an indicator of the peak temperatures reached during progressive metamorphism. We examine processes of graphite emplacement and deformation in the Alpine Fault Zone, New Zealand's active continental tectonic plate boundary. Raman spectrometry indicates that graphite in the distal, amphibolite-facies Alpine Schist, which experienced peak metamorphic temperatures up to 640 ◦C, is highly crystalline and occurs mainly along grain boundaries within quartzo-feldspathic domains. The subsequent mylonitisation in the Alpine Fault Zone resulted in progressive reworking of CM under lower temperature conditions (500◦C-600◦C) in a structurally controlled environment, resulting in spatial clustering in lower-strain protomylonites, and further foliation-alignment in higher-strain mylonites. Subsequent brittle deformation of the mylonitised schists resulted in cataclasites that contain over three-fold increase in the abundance of graphite than mylonites. Furthermore, cataclasites contain graphite with two different habits: highly-crystalline, foliated forms that are inherited mylonitic graphite; and lower-crystallinity, less mature patches of finer-grained graphite. The observed graphite enrichment and the occurrence of poorly-organised graphite in the Alpine Fault cataclasites could result from: i) hydrothermal precipitation from carbon-supersaturated fluids; and/or ii) mechanical degradation by structural disordering of mylonitic graphite combined with strain-induced graphite localisation. The lack of published systematic studies of mechanical modification of the structure of graphite inhibits further conclusion to be drawn. Thus, we performed laboratory deformation experiments during which we sheared highly crystalline graphite powder at room temperature, normal stresses of 5 MPa and 25 MPa and sliding velocities of 1 µm/s, 10 µm/s and 100 µm/s. The degree of graphite crystallinity, both in the starting and resulting materials, was analysed by Raman microspectroscopy. Our results demonstrate consistent decrease of graphite crystallinity with increasing shear strain. We conclude that: i) graphite 'thermometers' are unreliable in brittely deformed rocks; ii) a shear strain calibration of graphite 'thermometers' is needed; iii) fault creep is very likely responsible for the observed structural and textural characteristics of graphite in the Alpine Fault cataclasites. Finally, to investigate the possibility of hydrothermal origin for at least some of the graphite in the Alpine Fault cataclasites we will also present synchrotron FTIR and carbon isotope analysis of the Alpine fault rocks.

  19. Investigation on MoS2 and graphite coatings and their effects on the tribological properties of the radial spherical plain bearings

    NASA Astrophysics Data System (ADS)

    Qiu, Ming; Lu, Jianjun; Li, Yingchun; Lv, Guisen

    2016-07-01

    With constant enlargement of the application areas of the spherical plain bearings, higher quality lubrication of the bearings is required. To solve the lubricating problems of spherical plain bearings under high temperature, high vacuum, high speed, heavy loads and strong oxidation conditions, it is urgent for us to develop more excellent self-lubricating technologies. In this paper, the bonded solid lubricant coatings, which use inorganic phosphate as the binder, the mixture of MoS2 and graphite with two different weight proportions as the solid lubricant, are prepared by spraying under three different spray gun pressures. The bonding strength tests on the coatings show that the best spraying pressure is 0.2 MPa and the better mixing proportion of MoS2 to Graphite is 3:1. Then for the radial spherical plain bearings with steel/steel friction pair, after the coatings are made on the inner ring outer surfaces, the friction coefficient, the wear loss and the friction temperature of the bearings under four oscillating frequencies are investigated by a self-made tribo-tester. The test results, SEM of the worn morphologies and EDS of worn areas show that tribological properties of the bearing are obviously improved by the bonded solid lubricant coatings. When sprayed under the spray gun pressure of 0.2 MPa, the bearings have better anti-friction and anti-wear properties than those sprayed under 0.1 MPa and 0.3 MPa. Further as proved from the XPS analysis, between the coating with 3:1 mixing ratio of MoS2 to Graphite and the coating with 1:1 ratio, the former has less oxidation occurred on the surface and therefore has better tribological characteristics than the latter. This paper provides a reference to developing a new product of the radial spherical plain bearings with high bonding strength, oxidation resistance and abrasion resistance.

  20. Laser excited atomic fluorescence spectrometry as a powerful tool for analytical applications and spectroscopic studies

    NASA Astrophysics Data System (ADS)

    Gornushkin, Igor B.

    1997-12-01

    Laser-excited atomic fluorescence spectrometry (LEAFS) with a novel diffusive tube electrothermal atomizer (ETA) has been used for the study of atomization and diffusion processes and for the direct trace analysis of complex matrices. A novel ETA was a graphite tube sealed by two graphite electrodes. A sample was introduced into the tube and the furnace assembly was heated. The vaporized sample diffused through the hot graphite and the atomic fraction of the vapor was excited by a tunable dye laser above the tube. Temporal behavior of atomic fluorescence of Cu, Ag, and Ni atoms, diffused through the furnace tube, was studied at different temperatures; the values for activation energies and diffusion coefficients were derived on the basis of the diffusion/vaporization kinetic model. The femtogram/nanogram concentrations of silver were determined in coastal Atlantic water and soil samples. Use of the new ETA resulted in significant reduction of matrix interferences, ultra-low limits of detection, good accuracy and precision. LEAFS coupled with laser ablation (LA) was studied in terms of its analytical and spectroscopic potential. Low concentrations of lead (0.15 ppm-750 ppm) in metallic matrices (copper, brass, steel, and zinc) were measured in a low pressure argon atmosphere. No matrix effect was observed, providing a universal calibration curve for all samples. A limit of detection of 22 ppb (0.5 fg) was achieved. Also, the lifetime of the metastable 6p21D level of lead was measured and found to be in good agreement with the literature data. A simple open-air LA-LEAFS system was used for the determination of cobalt in solid matrices (graphite, soil, and steel). The fluorescence of cobalt was excited from a level which was already populated in the ablation plasma and was monitored at the Stokes-shifted wavelength. Detection limits in the ppb to ppm range and linearity over four orders of magnitude were achieved. The resonance shadowgraph technique has been developed for time-resolved imaging of laser-produced plasmas. The shadowgraphs were obtained by igniting the plasma on the lead or tin surface and by illuminating the plasma by a laser tuned in resonance with a strong atomic transition. UV-photodecomposition of lead and tin clusters was visualized. The evolution of the plasmas was studied at different pressures of argon. A shock wave produced by the laser ablation was monitored and its speed was measured.

  1. Influence of graphite-alloy interactions on corrosion of Ni-Mo-Cr alloy in molten fluorides

    NASA Astrophysics Data System (ADS)

    Ai, Hua; Hou, Juan; Ye, Xiang-Xi; Zeng, Chao Liu; Sun, Hua; Li, Xiaoyun; Yu, Guojun; Zhou, Xingtai; Wang, Jian-Qiang

    2018-05-01

    In this study, the effects of graphite-alloy interaction on corrosion of Ni-Mo-Cr alloy in molten FLiNaK salt were investigated. The corrosion tests of Ni-Mo-Cr alloys were conducted in graphite crucibles, to examine the differences of test specimens in conditions of electric contact and isolated with graphite, respectively. The corrosion attack is severer with more weight loss and deeper Cr depletion layer in samples electric contact with graphite than those isolated with graphite. The occurrence of galvanic corrosion between alloy specimens and graphite container was confirmed by electrochemical measurement. The corrosion is controlled by nonelectric transfer in isolated test while electrochemical reaction accelerated corrosion in electric contact test.

  2. Status report on the Zagreb Radiocarbon Laboratory - AMS and LSC results of VIRI intercomparison samples

    NASA Astrophysics Data System (ADS)

    Sironić, Andreja; Krajcar Bronić, Ines; Horvatinčić, Nada; Barešić, Jadranka; Obelić, Bogomil; Felja, Igor

    2013-01-01

    A new line for preparation of the graphite samples for 14C dating by Accelerator Mass Spectrometry (AMS) in the Zagreb Radiocarbon Laboratory has been validated by preparing graphite from various materials distributed within the Fifth International Radiocarbon Intercomparison (VIRI) study. 14C activity of prepared graphite was measured at the SUERC AMS facility. The results are statistically evaluated by means of the z-score and u-score values. The mean z-score value of 28 prepared VIRI samples is (0.06 ± 0.23) showing excellent agreement with the consensus VIRI values. Only one sample resulted in the u-score value above the limit of acceptability (defined for the confidence interval of 99%) and this was probably caused by a random contamination of the graphitization rig. After the rig had been moved to the new adapted and isolated room, all u-score values laid within the acceptable limits. Our LSC results of VIRI intercomparison samples are also presented and they are all accepted according to the u-score values.

  3. Catalytic graphitization behavior of phenolic resins by addition of in situ formed nano-Fe particles

    NASA Astrophysics Data System (ADS)

    Rastegar, H.; Bavand-vandchali, M.; Nemati, A.; Golestani-Fard, F.

    2018-07-01

    This work presents the catalytic graphitization process of phenolic resins (PR's) by addition of in situ nano-Fe particles as catalyst. Pyrolysis treatments of prepared compositions including various contents of nano-Fe particles were carried out at 600-1200 °C for 3 h under reducing atmosphere and graphitization process were evaluated by different techniques such as X-Ray diffraction (XRD), Field Emission Scanning Electron Microscopy (FESEM), High Resolution Transmission Electron Microscopy (HRTEM), Simultaneous Thermal Analysis (STA) and Raman spectroscopy that mainly performed to identify the phase and microstructural analysis, oxidation resistance and extend of graphitized carbon formation. Results indicate that, in situ graphitic carbon development were already observed after firing the samples at 800 °C for 3 h under reducing atmosphere, increasing temperature and amount of nano-Fe led to a more effective graphitization level. In addition, the different nano crystalline carbon shapes such as onion and bamboo like and carbon nanotubes (CNTs) were in situ identified during graphitization process of nano-Fe containing samples. It was suggested that formation of these different nano carbon structures related to nano-Fe catalyst behavior and the carbon shell growth.

  4. Carbon doping in molecular beam epitaxy of GaAs from a heated graphite filament

    NASA Technical Reports Server (NTRS)

    Malik, R. J.; Nottenberg, R. N.; Schubert, E. F.; Walker, J. F.; Ryan, R. W.

    1988-01-01

    Carbon doping of GaAs grown by molecular beam epitaxy has been obtained for the first time by use of a heated graphite filament. Controlled carbon acceptor concentrations over the range of 10 to the 17th-10 to the 20th/cu cm were achieved by resistively heating a graphite filament with a direct current power supply. Capacitance-voltage, p/n junction and secondary-ion mass spectrometry measurements indicate that there is negligible diffusion of carbon during growth and with postgrowth rapid thermal annealing. Carbon was used for p-type doping in the base of Npn AlGaAs/GaAs heterojunction bipolar transistors. Current gains greater than 100 and near-ideal emitter heterojunctions were obtained in transistors with a carbon base doping of 1 x 10 to the 19th/cu cm. These preliminary results indicate that carbon doping from a solid graphite source may be an attractive substitute for beryllium, which is known to have a relatively high diffusion coefficient in GaAs.

  5. Enhanced photocatalytic activity of graphitic carbon nitride/carbon nanotube/Bi2WO6 ternary Z-scheme heterojunction with carbon nanotube as efficient electron mediator.

    PubMed

    Jiang, Deli; Ma, Wanxia; Xiao, Peng; Shao, Leqiang; Li, Di; Chen, Min

    2018-02-15

    All-solid-state Z-scheme heterojunction has attracted much attention in photocatalytic field because of its strong ability in charge separation and transfer. In the present study, all-solid-state ternary Z-scheme heterojunction constructed by graphitic carbon nitride (CN) nanosheet, carbon nanotube (CNT), and Bi 2 WO 6 (BWO) nanosheet, in which CNT was employed as the electron mediator. The CN/CNT/BWO ternary Z-scheme heterojunction shows the enhanced photocatalytic activity towards the degradation of tetracycline hydrochloride (TC) as compared to the pristine g-C 3 N 4 , Bi 2 WO 6 , CNT/BWO, CNT/CN, and CN/BWO. The significantly improved photocatalytic activity can be mainly ascribed to the formed CNT-mediated Z-scheme heterojunction, which facilitates the separation and transfer of photogenerated electron-hole pairs. Our work provides a rational design of all-solid-state Z-scheme heterojunction with CNT as the electron mediator for highly efficient photocatalysis. Copyright © 2017 Elsevier Inc. All rights reserved.

  6. Mechanical Degradation of Graphite/PVDF Composite Electrodes: A Model-Experimental Study

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

    Takahashi, Kenji; Higa, Kenneth; Mair, Sunil

    2015-12-11

    Mechanical failure modes of a graphite/polyvinylidene difluoride (PVDF) composite electrode for lithium-ion batteries were investigated by combining realistic stress-stain tests and mathematical model predictions. Samples of PVDF mixed with conductive additive were prepared in a similar way to graphite electrodes and tested while submerged in electrolyte solution. Young's modulus and tensile strength values of wet samples were found to be approximately one-fifth and one-half of those measured for dry samples. Simulations of graphite particles surrounded by binder layers given the measured material property values suggest that the particles are unlikely to experience mechanical damage during cycling, but that the fatemore » of the surrounding composite of PVDF and conductive additive depends completely upon the conditions under which its mechanical properties were obtained. Simulations using realistic property values produced results that were consistent with earlier experimental observations.« less

  7. A fracture mechanics analysis of impact damage in a thick composite laminate

    NASA Technical Reports Server (NTRS)

    Poe, C. C., Jr.

    1985-01-01

    Graphite/epoxy filament-wound cases (FWC) for the solid rocket motors of the space shuttle are being made by NASA. The FWC cases are wound with AS4W graphite fiber impregnated with an epoxy resin and are about 1.4 inches or more thick. Graphite-epoxy composite laminates, unlike metals, can be damaged easily by low velocity impacts of objects like dropped tools. The residual tension strength of the FWC laminate, after impact, is being studied at Langley Research Center. The conditions that give minimum visual evidence of damage are being emphasized. A fracture mechanics analysis was developed to predict the residual strength, after impact, using radiographs to measure the size of the damage and an equivalent surface crack to represent the damage.

  8. Analysis of the neurotoxin anisatin in star anise by LC-MS/MS.

    PubMed

    Mathon, Caroline; Bongard, Benjamin; Duret, Monique; Ortelli, Didier; Christen, Philippe; Bieri, Stefan

    2013-01-01

    The aim of this work was to develop an analytical method capable of determining the presence of anisatin in star anise. This neurotoxin may induce severe side effects such as epileptic convulsions. It is therefore of prime importance to have rapid and accurate analytical methods able to detect and quantify anisatin in samples that are purportedly edible star anise. The sample preparation combined an automated accelerated solvent extraction with a solid-supported liquid-liquid purification step on EXtrelut®. Samples were analysed on a porous graphitic carbon HPLC column and quantified by tandem mass spectrometry operating in the negative ionisation mode. The quantification range of anisatin was between 0.2 and 8 mg kg⁻¹. The applicability of this validated method was demonstrated by the analysis of several Illicium species and star anise samples purchased on the Swiss market. High levels of anisatin were measured in Illicium lanceolatum, I. majus and I. anisatum, which may cause health concerns if they are misidentified or mixed with edible Illicium verum.

  9. The First Discovery of Presolar Graphite Grains from the Highly Reducing Qingzhen (EH3) Meteorite

    NASA Astrophysics Data System (ADS)

    Xu, Yuchen; Lin, Yangting; Zhang, Jianchao; Hao, Jialong

    2016-07-01

    Presolar graphite grains have been extensively studied, but are limited in carbonaceous chondrites, particularly in Murchison (CM2) and Orgueil (CI1), which sampled materials from the oxidizing regions in the solar nebula. Here, we report the first discovery of presolar graphite grains from the Qingzhen (EH3) enstatite chondrite which formed under a highly reducing condition. Eighteen presolar graphite grains were identified by C-isotope mapping of the low-density fraction (1.75-1.85 g cm-3) from Qingzhen acid residue. Another 58 graphite spherules were found in different areas of the same sample mount using a scanning electron microscope and were classified into three morphologies, including cauliflower, onion, and cauliflower-onion. The Raman spectra of these spherules vary from ordered, disordered, and glassy to kerogen-like, suggestive of a wide range of thermal metamorphisms. NanoSIMS analysis of the C- and Si-isotopes of these graphite spherules confirmed 23 presolar grains. The other 35 graphite spherules have no significant isotopic anomalies, but they share similar morphologies and Raman spectra with the presolar ones. Another three grains were identified during NanoSIMS analysis. Of all the 44 presolar graphite grains identified, six grains show 28Si-excesses, suggestive of supernovae origins, and four grains are 12C- and 29,30Si-rich, consistent with low-metallicity asymptotic giant branch star origins. Another two graphite spherules have extremely low 12C/13C ratios with marginal solar Si-isotopes. The morphologies, Raman spectra, and C- and Si-isotopic distributions of the presolar graphite grains from the Qingzhen enstatite chondrite are similar to those of the low-density fractions from Murchison carbonaceous chondrites. This study suggests a homogeneous distribution of presolar graphite grains in the solar nebula.

  10. The Design and Testing of a High-Temperature Graphite Dilatometer

    DTIC Science & Technology

    1992-06-24

    26 11. Data from three-point-bend samples of PAA, phenolic, and furfural resin samples that were...TEMPERATURE (0C) Fig. 11. Data from three-point-bend samples of (a) PAA, (b) phenolic, and (c) furfural resin samples that were precured to 350*C. The max- imum...graphitization tempera- tures (20000C); and furfural resin carbon absorbs less at all temperatures. 28 V. CONCLUSIONS The dilatometer system described

  11. Solid State Physics. Nitrogen Adsorption by Thermoexfoliated Graphite / Slāpekļa Adsorbcija Uz Termoeksfoliētā Grafīta

    NASA Astrophysics Data System (ADS)

    Grehov, V.; Kalnacs, J.; Matzui, L.; Knite, M.; Murashov, A.; Vilken, A.

    2013-02-01

    Adsorption by thermochemically exfoliated graphite (TEG) is studied and compared with that by other carbon structures under the same conditions. In BET determination of the specific surface area (SBET) for the TEG samples it was found that good approximation could be observed in two different pressure ranges. Such ranges of BET approximation are also visible in the isotherms of aquadag and milled graphite. The experimental results are discussed and their interpretation proposed Ar sorbcijas iekārtu Autosorb-1 (Quantochrome Instruments Co, Florida, USA) pētīta termiski eksfoliēta grafīta slāpekļa sorbcijas spēja salīdzinājumā ar citu oglekļa struktūru sorbciju tādos pašos apstākļos. Atrasti divi izotermu rajoni, kas raksturojas ar mazu (SBET1) un palielinātu (SBET2) īpatnējo virsmu.. Šāda veida izotermas raksturīgas slikti adsorbējošiem materiāliem, pie kādiem pieder arī akvadags. Labi adsorbējošās oglekļa struktūrām, tādām kā aktīvā ogle un oglekļa nanocaurules, raksturīgas cita veida izotermas. Apspriesta eksperimentālā rezultāta interpretācija

  12. Nucleotide and Nucleotide Sugar Analysis by Liquid Chromatography-Electrospray Ionization-Mass Spectrometry on Surface-Conditioned Porous Graphitic Carbon

    PubMed Central

    2010-01-01

    We examined the analysis of nucleotides and nucleotide sugars by chromatography on porous graphitic carbon with mass spectrometric detection, a method that evades contamination of the MS instrument with ion pairing reagent. At first, adenosine triphosphate (ATP) and other triphosphate nucleotides exhibited very poor chromatographic behavior on new columns and could hardly be eluted from columns previously cleaned with trifluoroacetic acid. Satisfactory performance of both new and older columns could, however, be achieved by treatment with reducing agent and, unexpectedly, hydrochloric acid. Over 40 nucleotides could be detected in cell extracts including many isobaric compounds such as ATP, deoxyguanosine diphosphate (dGTP), and phospho-adenosine-5′-phosphosulfate or 3′,5′-cyclic adenosine 5'-monophosphate (AMP) and its much more abundant isomer 2′,3′-cylic AMP. A fast sample preparation procedure based on solid-phase extraction on carbon allowed detection of very short-lived analytes such as cytidine 5'-monophosphate (CMP)-2-keto-deoxy-octulosonic acid. In animal cells and plant tissues, about 35 nucleotide sugars were detected, among them rarely considered metabolites such as uridine 5'-diphosphate (UDP)-l-arabinopyranose, UDP-l-arabinofuranose, guanosine 5'-diphosphate (GDP)-l-galactofuranose, UDP-l-rhamnose, and adenosine diphosphate (ADP)-sugars. Surprisingly, UDP-arabinopyranose was also found in Chinese hamster ovary (CHO) cells. Due to the unique structural selectivity of graphitic carbon, the method described herein distinguishes more nucleotides and nucleotide sugars than previously reported approaches. PMID:21043458

  13. Test Report - Fault Current Through Graphite Filament Reinforced Plastic

    NASA Technical Reports Server (NTRS)

    Evans, R. W.

    1997-01-01

    Tests were performed to determine the damage to samples of composite material when a current carrying wire is shorted to the surface of the composite material, and to determine whether enough current can flow through the material to blow a fuse before damage can occur. Fault current tests were performed on samples of graphite epoxy materials. Samples consisted of six layers of IM7 graphite fiber mat in Hercules 8552 epoxy resin. A variable power supply provided up to 35 amps of current. The high voltage side of the power supply was attached to a wire at the end of a hinged arm, and the low side was attached to the edge of the sample. To test joints, the return was connected to the edge of one sample, and the high side was shorted to the top of the other sample. Tests show that when current exceeds approximately 5 amps, the graphite glows, and the epoxy melts out at the shorted contact. At higher current levels the epoxy burns. At voltages above 15 volts the epoxy outer coat is easily broken, and fire, flame, and a rise in current occur suddenly. When joints are introduced, resistance is increased, and the maximum current resulting from a short circuit to the graphite epoxy is reduced. This condition can easily result in fault current lower than the circuit breaker limit and higher than the 5 amp ignition level. The shorting contact and the joint become hot spots with melting epoxy, smoke, and fire.

  14. Synthesis and photocatalytic activity of N-doped TiO2 produced in a solid phase reaction

    NASA Astrophysics Data System (ADS)

    Xin, Gang; Pan, Hongfei; Chen, Dan; Zhang, Zhihua; Wen, Bin

    2013-02-01

    N-doped TiO2 was synthesized by calcining a mixture of titanic acid and graphitic carbon nitride (g-C3N4) at temperatures above 500 °C. The final samples were characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), electron energy loss spectroscopy (EELS), and UV-vis diffuse reflectance spectra. The photocatalytic activity of N-doped TiO2 was studied by assessing the degradation of methylene blue in an aqueous solution, under visible light and UV light irradiation. It was found that the N-doped TiO2 displayed higher photocatalytic activity than pure TiO2, under both visible and UV light.

  15. Boron nitride as desalting material in combination with phosphopeptide enrichment in shotgun proteomics.

    PubMed

    Furuhashi, Takeshi; Nukarinen, Ella; Ota, Shigenori; Weckwerth, Wolfram

    2014-05-01

    Hydrophilic peptides in shotgun proteomics have been shown to be problematic in conventional chromatography. Typically, C18 solid phase extraction or peptide traps are used for desalting the sample prior to mass spectrometry analysis, but the capacity to retain hydrophilic peptides is not very high, causing a bias toward more hydrophobic peptides. This is particularly problematic in phosphoproteomic studies. We tested the compatibility of commercially available boron nitride as a novel material for peptide desalting. Boron nitride can be used to recover a wide range of peptides with different physicochemical properties comparable to combined C18 and graphite carbon material. Copyright © 2014. Published by Elsevier Inc.

  16. Purification and preparation of graphite oxide from natural graphite

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

    Panatarani, C., E-mail: c.panatarani@phys.unpad.ac.id; Muthahhari, N.; Joni, I. Made

    2016-03-11

    Graphite oxide has attracted much interest as a possible route for preparation of natural graphite in the large-scale production and manipulation of graphene as a material with extraordinary electronic properties. Graphite oxide was prepared by modified Hummers method from purified natural graphite sample from West Kalimantan. We demonstrated that natural graphite is well-purified by acid leaching method. The purified graphite was proceed for intercalating process by modifying Hummers method. The modification is on the reaction time and temperature of the intercalation process. The materials used in the intercalating process are H{sub 2}SO{sub 4} and KMNO{sub 4}. The purified natural graphitemore » is analyzed by carbon content based on Loss on Ignition test. The thermo gravimetricanalysis and the Fouriertransform infrared spectroscopy are performed to investigate the oxidation results of the obtained GO which is indicated by the existence of functional groups. In addition, the X-ray diffraction and energy dispersive X-ray spectroscopy are also applied to characterize respectively for the crystal structure and elemental analysis. The results confirmed that natural graphite samples with 68% carbon content was purified into 97.68 % carbon content. While the intercalation process formed a formation of functional groups in the obtained GO. The results show that the temperature and reaction times have improved the efficiency of the oxidation process. It is concluded that these method could be considered as an important route for large-scale production of graphene.« less

  17. Critical evaluation of the stability of highly concentrated LiTFSI - Acetonitrile electrolytes vs. graphite, lithium metal and LiFePO4 electrodes

    NASA Astrophysics Data System (ADS)

    Nilsson, Viktor; Younesi, Reza; Brandell, Daniel; Edström, Kristina; Johansson, Patrik

    2018-04-01

    Highly concentrated LiTFSI - acetonitrile electrolytes have recently been shown to stabilize graphite electrodes in lithium-ion batteries (LIBs) much better than comparable more dilute systems. Here we revisit this system in order to optimise the salt concentration vs. both graphite and lithium metal electrodes with respect to electrochemical stability. However, we observe an instability regardless of concentration, making lithium metal unsuitable as a counter electrode, and this also affects evaluation of e.g. graphite electrodes. While the highly concentrated electrolytes have much improved electrochemical stabilities, their reductive decomposition below ca. 1.2 V vs. Li+/Li° still makes them less practical vs. graphite electrodes, and the oxidative reaction with Al at ca. 4.1 V vs. Li+/Li° makes them problematic for high voltage LIB cells. The former originates in an insufficiently stable solid electrolyte interphase (SEI) dissolving and continuously reforming - causing self-discharge, as observed by paused galvanostatic cycling, while the latter is likely caused by aluminium current collector corrosion. Yet, we show that medium voltage LiFePO4 positive electrodes can successfully be used as counter and reference electrodes.

  18. Degradation of lithium ion batteries employing graphite negatives and nickel-cobalt-manganese oxide + spinel manganese oxide positives: Part 2, chemical-mechanical degradation model

    NASA Astrophysics Data System (ADS)

    Purewal, Justin; Wang, John; Graetz, Jason; Soukiazian, Souren; Tataria, Harshad; Verbrugge, Mark W.

    2014-12-01

    Capacity fade is reported for 1.5 Ah Li-ion batteries containing a mixture of Li-Ni-Co-Mn oxide (NCM) + Li-Mn oxide spinel (LMO) as positive electrode material and a graphite negative electrode. The batteries were cycled at a wide range of temperatures (10 °C-46 °C) and discharge currents (0.5C-6.5C). The measured capacity losses were fit to a simple physics-based model which calculates lithium inventory loss from two related mechanisms: (1) mechanical degradation at the graphite anode particle surface caused by diffusion-induced stresses (DIS) and (2) chemical degradation caused by lithium loss to continued growth of the solid-electrolyte interphase (SEI). These two mechanisms are coupled because lithium is consumed through SEI formation on newly exposed crack surfaces. The growth of crack surface area is modeled as a fatigue phenomenon due to the cyclic stresses generated by repeated lithium insertion and de-insertion of graphite particles. This coupled chemical-mechanical degradation model is consistent with the observed capacity loss features for the NCM + LMO/graphite cells.

  19. Thermal transport in three-dimensional foam architectures of few-layer graphene and ultrathin graphite.

    PubMed

    Pettes, Michael Thompson; Ji, Hengxing; Ruoff, Rodney S; Shi, Li

    2012-06-13

    At a very low solid concentration of 0.45 ± 0.09 vol %, the room-temperature thermal conductivity (κ(GF)) of freestanding graphene-based foams (GF), comprised of few-layer graphene (FLG) and ultrathin graphite (UG) synthesized through the use of methane chemical vapor deposition on reticulated nickel foams, was increased from 0.26 to 1.7 W m(-1) K(-1) after the etchant for the sacrificial nickel support was changed from an aggressive hydrochloric acid solution to a slow ammonium persulfate etchant. In addition, κ(GF) showed a quadratic dependence on temperature between 11 and 75 K and peaked at about 150 K, where the solid thermal conductivity (κ(G)) of the FLG and UG constituents reached about 1600 W m(-1) K(-1), revealing the benefit of eliminating internal contact thermal resistance in the continuous GF structure.

  20. Carbon solids in oxygen-deficient explosives (LA-UR-13-21151)

    NASA Astrophysics Data System (ADS)

    Peery, Travis

    2013-06-01

    The phase behavior of excess carbon in oxygen-deficient explosives has a significant effect on detonation properties and product equations of state. Mixtures of fuel oil in ammonium nitrate (ANFO) above a stoichiometric ratio demonstrate that even small amounts of graphite, on the order of 5% by mole fraction, can substantially alter the Chapman-Jouget (CJ) state properties, a central ingredient in modeling the products equation of state. Similar effects can be seen for Composition B, which borders the carbon phase boundary between graphite and diamond. Nano-diamond formation adds complexity to the product modeling because of surface adsorption effects. I will discuss these carbon phase issues in our equation of state modeling of detonation products, including our statistical mechanics description of carbon clustering and surface chemistry to properly treat solid carbon formation. This work is supported by the Advanced Simulation and Computing Program, under the NNSA.

  1. Transfer impedance measurements of the space shuttle Solid Rocket Motor (SRM) joints, wire meshes and a carbon graphite motor case

    NASA Technical Reports Server (NTRS)

    Papazian, Peter B.; Perala, Rodney A.; Curry, John D.; Lankford, Alan B.; Keller, J. David

    1988-01-01

    Using three different current injection methods and a simple voltage probe, transfer impedances for Solid Rocket Motor (SRM) joints, wire meshes, aluminum foil, Thorstrand and a graphite composite motor case were measured. In all cases, the surface current distribution for the particular current injection device was calculated analytically or by finite difference methods. The results of these calculations were used to generate a geometric factor which was the ratio of total injected current to surface current density. The results were validated in several ways. For wire mesh measurements, results showed good agreement with calculated results for a 14 by 18 Al screen. SRM joint impedances were independently verified. The filiment wound case measurement results were validated only to the extent that their curve shape agrees with the expected form of transfer impedance for a homogeneous slab excited by a plane wave source.

  2. Analyses of moisture in polymers and composites

    NASA Technical Reports Server (NTRS)

    Ryan, L. E.; Vaughan, R. W.

    1980-01-01

    A suitable method for the direct measurement of moisture concentrations after humidity/thermal exposure on state of the art epoxy and polyimide resins and their graphite and glass fiber reinforcements was investigated. Methods for the determination of moisture concentration profiles, moisture diffusion modeling and moisture induced chemical changes were examined. Carefully fabricated, precharacterized epoxy and polyimide neat resins and their AS graphite and S glass reinforced composites were exposed to humid conditions using heavy water (D20), at ambient and elevated temperatures. These specimens were fixtured to theoretically limit the D20 permeation to a unidirectional penetration axis. The analytical techniques evaluated were: (1) laser pyrolysis gas chromatography mass spectrometry; (2) solids probe mass spectrometry; (3) laser pyrolysis conventional infrared spectroscopy; and (4) infrared imaging thermovision. The most reproducible and sensitive technique was solids probe mass spectrometry. The fabricated exposed specimens were analyzed for D20 profiling after humidity/thermal conditioning at three exposure time durations.

  3. Tribological Behavior of Nano-Onions in Krytox 143AB Evaluated

    NASA Technical Reports Server (NTRS)

    Street, Kenneth W.; VanderWal, Randy L.; Marchetti, Mario; Tomasek, Aaron J.

    2005-01-01

    Nanoparticles have been developed over the past 10 years and have found several applications. This work presents the use of carbon nano-onions as a potential oil additive for aerospace applications. Researchers at the NASA Glenn Research Center tested lubricant lifetimes in ambient air and ultrahigh vacuum and characterized the breakdown products of the friction and wear. These carbon nanoparticles can provide adequate lubrication very similar to that of graphitic material when run in air. Soot represents one of the very first nanostructured materials, although it has rarely been considered as such. Changes in the carbon nanostructure, resulting in increased graphitic layer plane length, correlate with reactivity loss. Upon heating spherically shaped nanometer-sized carbon black in the absence of oxidant, graphene sheets form, and the initial soot particle templates the growth of a graphitic particle into what is best described as a sphere with many flat sides having a hollow interior. Because there are no edge sites, these polygonal graphitic particles, or nano-onions, are relatively resistant to oxidation. Graphite is used as a solid lubricant because of its stability at moderately high temperatures. However, the temperature at which graphite oxidizes rapidly is strongly influenced by surface area. With the size of particles typically employed in lubrication, a great amount of thermal stability is lost because of size reduction either during preparation or during lubrication of contacting parts. Therefore, we have undertaken a study of the lubricating ability of graphitic nano-onions (ref. 1).

  4. Comparison of irradiation behaviour of HTR graphite grades

    NASA Astrophysics Data System (ADS)

    Heijna, M. C. R.; de Groot, S.; Vreeling, J. A.

    2017-08-01

    The INNOGRAPH irradiations were executed in the High Flux Reactor (HFR) in Petten by NRG supported by the European Framework programs HTR-M, RAPHAEL, and ARCHER to generate data on the irradiation behaviour of graphite grades for High Temperature Reactor (HTR) application available at that time. Samples of the graphite grades NBG-10, NBG-17, NBG-18, NBG-20, NBG-25, PCEA, PPEA, PCIB, and IG-110 have been irradiated at 750 °C and 950 °C. The inherent scatter induced by the probabilistic material behaviour of graphite requires uncertainty and scatter induced by test conditions and post-irradiation examination to be minimized. The INNOGRAPH irradiations supplied an adequate number of irradiated samples to enable accurate determination of material properties and their evolution under irradiation. This allows comparison of different graphite grades and a qualitative assessment of their appropriateness for HTR applications, as a basis of selection, design and core component lifetime. The results indicate that coarse grained graphite grades exhibit more favourable behaviour for application in HTRs due to their low dimensional anisotropy and fracture propagation resilience.

  5. Effective Thermal Conductivity of Graphite Materials with Cracks

    NASA Astrophysics Data System (ADS)

    Pestchaanyi, S. E.; Landman, I. S.

    The dependence of effective thermal diffusivity on temperature caused by volumetric cracks is modelled for macroscopic graphite samples using the three-dimensional thermomechanics code Pegasus-3D. At high off-normal heat loads typical of the divertor armour, thermostress due to the anisotropy of graphite grains is much larger than that due to the temperature gradient. Numerical simulation demonstrated that the volumetric crack density both in fine grain graphites and in the CFC matrix depends mainly on the local sample temperature, not on the temperature gradient. This allows to define an effective thermal diffusivity for graphite with cracks. The results obtained are used to explain intense cracking and particle release from carbon based materials under electron beam heat load. Decrease of graphite thermal diffusivity with increase of the crack density explains particle release mechanism in the experiments with CFC where a clear energy threshold for the onset of particle release has been observed in J. Linke et al. Fusion Eng. Design, in press, Bazyler et al., these proceedings. Surface temperature measurement is necessary to calibrate the Pegasus-3D code for simulation of ITER divertor armour brittle destruction.

  6. Nonlinear optical characterization of graphite oxide thin film by open aperture Z-scan technique

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

    Sreeja, V. G.; Reshmi, R.; Devasia, Sebin

    In this paper we explore the structural characterization of graphite oxide powder prepared from graphite powder by oxidation via modified Hummers method. The nonlinear optical properties of the spin coated graphite oxide thin film is also explored by open aperture Z-Scan technique. Structural and physiochemical properties of the samples were investigated with the help of Fourier Transform Infrared Spectroscopy (FTIR) and Raman Spectroscopy (Raman).The results of FT-IR and Raman spectroscopy showed that the graphite is oxidized by strong oxidants and the oxygen atoms are introduced into the graphite layers forming C=C, O-H and –C-H groups. The synthesized sample has goodmore » crystalline nature with lesser defects. The nonlinear optical property of GO thin film was studied by open aperture Z-Scan technique using Q-switched Nd-Yag Laser at 532 nm. The Z-scan plot showed that the investigated GO thin film has saturable absorption behavior. The nonlinear absorption coefficient and saturation intensity were also estimated to explore its applications in Q switched mode locking laser systems.« less

  7. NANOWIRE CATHODE MATERIAL FOR LITHIUM-ION BATTERIES

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

    John Olson, PhD

    2004-07-21

    This project involved the synthesis of nanowire ã-MnO2 and characterization as cathode material for high-power lithium-ion batteries for EV and HEV applications. The nanowire synthesis involved the edge site decoration nanowire synthesis developed by Dr. Reginald Penner at UC Irvine (a key collaborator in this project). Figure 1 is an SEM image showing ã-MnO2 nanowires electrodeposited on highly oriented pyrolytic graphite (HOPG) electrodes. This technique is unique to other nanowire template synthesis techniques in that it produces long (>500 um) nanowires which could reduce or eliminate the need for conductive additives due to intertwining of fibers. Nanowire cathode for lithium-ionmore » batteries with surface areas 100 times greater than conventional materials can enable higher power batteries for electric vehicles (EVs) and hybrid electric vehicles (HEVs). The synthesis of the ã-MnO2 nanowires was successfully achieved. However, it was not found possible to co-intercalate lithium directly in the nanowire synthesis. Based on input from proposal reviewers, the scope of the project was altered to attempt the conversion into spinel LiMn2O4 nanowire cathode material by solid state reaction of the ã-MnO2 nanowires with LiNO3 at elevated temperatures. Attempts to perform the conversion on the graphite template were unsuccessful due to degradation of the graphite apparently caused by oxidative attack by LiNO3. Emphasis then shifted to quantitative removal of the nanowires from the graphite, followed by the solid state reaction. Attempts to quantitatively remove the nanowires by several techniques were unsatisfactory due to co-removal of excess graphite or poor harvesting of nanowires. Intercalation of lithium into ã-MnO2 electrodeposited onto graphite was demonstrated, showing a partial demonstration of the ã-MnO2 material as a lithium-ion battery cathode material. Assuming the issues of nanowires removal can be solved, the technique does offer potential for creating high-power lithium-ion battery cathode needed for advanced EV and HEVs. Several technical advancements will still be required to meet this goal, and are likely topics for future SBIR feasibility studies.« less

  8. Preparation and Characterization of Graphite Waste/CeO2 Composites

    NASA Astrophysics Data System (ADS)

    Kusrini, E.; Utami, C. S.; Nasruddin; Prasetyanto, E. A.; Bawono, Aji A.

    2018-03-01

    In this research, the chemical modification of graphite waste with CeO2 was developed and characterized. Graphite waste was pretreated with mechanical to obtain the size 200 mesh (75 μm), and thermal methods at 110°C oven for 6 hours. Here, we demonstrate final properties of graphite before modification (GBM), activated graphite (GA) and graphite/CeO2 composite with variation of 0.5, 1 and 2 g of CeO2 (G0.5; G1; G2). The effect of CeO2 concentration was observed. The presence of cerium in modified graphite samples (G0.5; G1; G2) were analyzed using SEM-EDX. The results show that the best surface area was found in G2 is 26.82 m2/g. The presence of CeO2 onto graphite surface does not significantly increase the surface area of composites.

  9. The state of understanding of the lithium-ion-battery graphite solid electrolyte interphase (SEI) and its relationship to formation cycling

    DOE PAGES

    An, Seong Jin; Li, Jianlin; Daniel, Claus; ...

    2016-04-09

    An in-depth review is presented on the science of lithium-ion battery (LIB) solid electrolyte interphase (SEI) formation on the graphite anode, including structure, morphology, chemical composition, electrochemistry, formation mechanism, and LIB formation cycling. During initial operation of LIBs, the SEI layer forms on the graphite surfaces, the most commonly used anode material, due to side reactions with the electrolyte solvent/salt at low electro-reduction potentials. It is accepted that the SEI layer is essential to the long-term performance of LIBs, and it also has an impact on its initial capacity loss, self-discharge characteristics, cycle life, rate capability, and safety. While themore » presence of the anode SEI layer is vital, it is difficult to control its formation and growth, as the chemical composition, morphology, and stability depend on several factors. These factors include the type of graphite, electrolyte composition, electrochemical conditions, and cell temperature. Thus, SEI layer formation and electrochemical stability over long-term operation should be a primary topic of future investigation in the development of LIB technology. We review the progression of knowledge gained about the anode SEI, from its discovery in 1979 to the current state of understanding, and covers its formation process, differences in the chemical and structural makeup when cell materials and components are varied, methods of characterization, and associated reactions with the liquid electrolyte phase. It also discusses the relationship of the SEI layer to the LIB formation step, which involves both electrolyte wetting and subsequent slow charge-discharge cycles to grow the SEI.« less

  10. Determination of Pd, Pt and Rh in vehicles escape fumes by GF-AAS and ICP-OES.

    PubMed

    Goncalves, Antonio; Domínguez, José R; Alvarado, José

    2008-04-15

    Automotive exhaust gases from vehicles using catalytic converters were filtered through cellulose filter papers to collect suspended particles expulsed along with the engine's escape fumes. A specially designed sample collector was used for supporting the filter papers during collection. The collector was manufactured from a new car's exhaust pipe. A cellulose circular paper filter, 11 cm diameter, was attached to one end of the pipe and kept centered by pressing it against the borders of the pipe by means of a perforated aluminum cap, slightly wider than the pipe, used to cover this end of the collector. Filter papers loaded with the solid particles were acid-digested using a modified domestic microwave oven to bring the solid material into solution. The resulting solutions were analyzed for Pt by graphite furnace atomic absorption spectrometry (GF-AAS) and for Pd and Rh by inductively coupled plasma (ICP-OES). Results indicate that concentration of these analytes in the particulate is higher for new vehicles, having new catalytic converters, than for old ones. Maximum Pd, Pt and Rh in the samples analyzed were found to be 5.36, 12.60 and 1.03 microg g(-1), respectively.

  11. An Ultrahigh Capacity Graphite/Li 2S Battery with Holey-Li 2S Nanoarchitectures

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

    Ye, Fangmin; Noh, Hyungjun; Lee, Hongkyung

    The pairing of high-capacity Li 2S cathode (1166 mAh g -1) and lithium-free anode (LFA) provides an unparalleled potential in developing safe and energy-dense next-generation secondary batteries. However, the low utilization of the Li 2S cathode and the lack of electrolytes compatible to both electrodes are impeding the development. Here, a novel graphite/Li 2S battery system, which features a self-assembled, holey-Li 2S nanoarchitecture and a stable solid electrolyte interface (SEI) on the graphite electrode, is reported. The holey structure on Li 2S is beneficial in decomposing Li 2S at the first charging process due to the enhanced Li ion extractionmore » and transfer from the Li 2S to the electrolyte. In addition, the concentrated dioxolane (DOL)-rich electrolyte designed lowers the irreversible capacity loss for SEI formation. By using the combined strategies, the graphite/holey-Li 2S battery delivers an ultrahigh discharge capacity of 810 mAh g -1 at 0.1 C (based on the mass of Li 2S) and of 714 mAh g -1 at 0.2 C. Moreover, it exhibits a reversible capacity of 300 mAh g -1 after a record lifecycle of 600 cycles at 1 C. These results suggest the great potential of the designed LFA/holey-Li 2S batteries for practical use.« less

  12. An Ultrahigh Capacity Graphite/Li 2S Battery with Holey-Li 2S Nanoarchitectures

    DOE PAGES

    Ye, Fangmin; Noh, Hyungjun; Lee, Hongkyung; ...

    2018-05-07

    The pairing of high-capacity Li 2S cathode (1166 mAh g -1) and lithium-free anode (LFA) provides an unparalleled potential in developing safe and energy-dense next-generation secondary batteries. However, the low utilization of the Li 2S cathode and the lack of electrolytes compatible to both electrodes are impeding the development. Here, a novel graphite/Li 2S battery system, which features a self-assembled, holey-Li 2S nanoarchitecture and a stable solid electrolyte interface (SEI) on the graphite electrode, is reported. The holey structure on Li 2S is beneficial in decomposing Li 2S at the first charging process due to the enhanced Li ion extractionmore » and transfer from the Li 2S to the electrolyte. In addition, the concentrated dioxolane (DOL)-rich electrolyte designed lowers the irreversible capacity loss for SEI formation. By using the combined strategies, the graphite/holey-Li 2S battery delivers an ultrahigh discharge capacity of 810 mAh g -1 at 0.1 C (based on the mass of Li 2S) and of 714 mAh g -1 at 0.2 C. Moreover, it exhibits a reversible capacity of 300 mAh g -1 after a record lifecycle of 600 cycles at 1 C. These results suggest the great potential of the designed LFA/holey-Li 2S batteries for practical use.« less

  13. Graphite sample preparation for AMS in a high pressure and temperature press

    USGS Publications Warehouse

    Rubin, M.; Mysen, B.O.; Polach, H.

    1984-01-01

    A high pressure-high temperature press is used to make target material for accelerator mass spectrometry. Graphite was produced from typical 14C samples including oxalic acid and carbonates. Beam strength of 12C was generally adequate, but random radioactive contamination by 14C made age measurements impractical. ?? 1984.

  14. Graphite sample preparation for AMS in a high pressure and temperature press

    USGS Publications Warehouse

    Rubin, Meyer; Mysen, Bjorn O.; Polach, Henry

    1984-01-01

    A high pressure-temperature press is used to make target material for accelerator mass spectrometry. Graphite was produced from typical **1**4C samples including oxalic acid and carbonates. Beam strength of **1**2C was generally adequate, but random radioactive contamination by **1**4C made age measurements impractical.

  15. Fluid-deposited graphitic inclusions in quartz: Comparison between KTB (German Continental Deep-Drilling) core samples and artificially reequilibrated natural inclusions

    USGS Publications Warehouse

    Pasteris, J.D.; Chou, I.-Ming

    1998-01-01

    We used Raman microsampling spectroscopy (RMS) to determine the degree of crystallinity of minute (2-15 ??m) graphite inclusions in quartz in two sets of samples: experimentally reequilibrated fluid inclusions in a natural quartz grain and biotite-bearing paragneisses from the KTB deep drillhole in SE Germany. Our sequential reequilibration experiments at 725??C on initially pure CO2 inclusions in a quartz wafer and the J. Krautheim (1993) experiments at 900-1100??C on organic compounds heated in gold or platinum capsules suggest that, at a given temperature, (1) fluid-deposited graphite will have a lower crystallinity than metamorphosed organic matter and (2) that the crystallinity of fluid-deposited graphite is affected by the composition of the fluid from which it was deposited. We determined that the precipitation of more-crystalline graphite is favored by lower fH2 (higher fO2), and that the crystallinity of graphite is established by the conditions (including gas fugacities) that pertain as the fluid first reaches graphite saturation. Graphite inclusions within quartz grains in the KTB rocks show a wide range in crystallinity index, reflecting three episodes of carbon entrapment under different metamorphic conditions. Isolated graphite inclusions have the spectral properties of totally ordered, completely crystalline graphite. Such crystallinity suggests that the graphite was incorporated from the surrounding metasedimentary rocks, which underwent metamorphism at upper amphibolite-facies conditions. Much of the fluid-deposited graphite in fluid inclusions, however, shows some spectral disorder. The properties of that graphite resemble those of experimental precipitates at temperatures in excess of 700??C and at elevated pressures, suggesting that the inclusions represent precipitates from C-O-H fluids trapped under conditions near those of peak metamorphism at the KTB site. In contrast, graphite that is intimately associated with chlorite and other (presumably low-temperature) silicates in inclusions is highly disordered and spectrally resembles kerogens. This graphite probably was deposited during later greenschist-facies retrograde metamorphism at about 400-500??C. The degree of crystallinity of fluid-deposited graphite is shown to be a much more complex function of temperature than is the crystallinity of metamorphic graphite. To some extent, experiments can provide temperature-calibration of the crystallinity index. However, the difference in time scales between experimental runs and geologic processes makes it difficult to infer specific temperatures for naturally precipitated graphite. Copyright ?? 1998 Elsevier Science Ltd.

  16. Magnetic solid-phase extraction combined with graphite furnace atomic absorption spectrometry for speciation of Cr(III) and Cr(VI) in environmental waters.

    PubMed

    Jiang, Hong-mei; Yang, Ting; Wang, Yan-hong; Lian, Hong-zhen; Hu, Xin

    2013-11-15

    A new approach of magnetic solid phase extraction (MSPE) coupled with graphite furnace atomic absorption spectrometry (GFAAS) has been developed for the speciation of Cr(III) and Cr(VI) using zincon-immobilized silica-coated magnetic Fe3O4 nanoparticles (Zincon-Si-MNPs) as the MSPE absorbent. Cr(III) was quantitatively reserved on the absorbent at pH 9.1 while total Cr was reserved at pH 6.5. The absorbed Cr species were eluted by using 2 mol/L HCl and detected by GFAAS. The concentration of Cr(VI) could be calculated by subtracting Cr(III) from total Cr. All the parameters affecting the separation and extraction efficiency of Cr species such as pH, extraction time, concentration and volume of eluent, sample volume and influence of co-existing ions were systematically examined and the optimized conditions were established accordingly. The detection limit (LOD) of the method was 0.016 and 0.011 ng mL(-1) for Cr(III) and Cr(VI), respectively, with the enrichment factor of 100 and 150. The precisions of this method (Relative standard deviation, RSD, n=7) for Cr(III) and Cr(VI) at 0.1 ng mL(-1) were 6.0% and 6.2%, respectively. In order to validate the proposed method, a certified reference material of environmental water was analyzed, and the result of Cr speciation was in good agreement with the certified value. This MSPE-GFAAS method has been successfully applied for the speciation of Cr(III) and Cr(VI) in lake and tap waters with the recoveries of 88-109% for the spiked samples. Moreover, the MSPE separation mechanism of Cr(III) and Cr(VI) based on their adsorption-desorption on Zincon-Si-MNPs has been explained through various spectroscopic characterization. © 2013 Elsevier B.V. All rights reserved.

  17. Determination of diphenylarsinic acid, phenylarsonic acid and inorganic arsenic in drinking water by graphite-furnace atomic-absorption spectrometry after simultaneous separation and preconcentration with solid-phase extraction disks.

    PubMed

    Hagiwara, Kenta; Inui, Tetsuo; Koike, Yuya; Nakamura, Toshihiro

    2013-01-01

    A simple method of graphite-furnace atomic-absorption spectrometry (GFAAS) after solid-phase extraction (SPE) was developed for the determination of diphenylarsinic acid (DPAA), phenylarsonic acid (PAA), and inorganic arsenic (iAs) in drinking water. This method involves the simultaneous collection of DPAA, PAA, and iAs using three stacked SPE disks, i.e., an Empore SDB-XD disk (the upper layer), an activated carbon disk (the middle layer), and a Cation-SR disk loaded with Zr and Ca (ZrCa-CED; the lower layer). A 200-mL aqueous sample was adjusted to pH 3 with nitric acid and passed through the SPE disks at a flow rate of 15 mL min(-1), to concentrate DPAA on the SDB-XD disk, PAA on the activated carbon disk, and iAs on the ZrCa-CED. The As compounds were eluted from the disks with 10 mL of ethanol containing 0.5 mol L(-1) ammonia solution for DPAA, 20 mL of 1 mol L(-1) ammonia solution for PAA, and 20 mL of 6 mol L(-1) hydrochloric acid for iAs. The eluates of DPAA, PAA, and iAs were diluted to 20, 25, and 25 mL, respectively, with deionized water, and then analyzed by GFAAS. The detection limits of As (three-times the standard deviation (n = 3) of the blank values) were 0.13 and 0.16 μg L(-1) at enrichment factors of 10 and 8, respectively, using a 200-mL water sample. Spike tests with 2 μg (10 μg L(-1)) of DPAA, PAA, and iAs in 200 mL of tap water and bottled drinking water showed good recoveries (96.1-103.8%).

  18. Formation mechanism of the protective layer in a blast furnace hearth

    NASA Astrophysics Data System (ADS)

    Jiao, Ke-xin; Zhang, Jian-liang; Liu, Zheng-jian; Xu, Meng; Liu, Feng

    2015-10-01

    A variety of techniques, such as chemical analysis, scanning electron microscopy-energy dispersive spectroscopy, and X-ray diffraction, were applied to characterize the adhesion protective layer formed below the blast furnace taphole level when a certain amount of titanium- bearing burden was used. Samples of the protective layer were extracted to identify the chemical composition, phase assemblage, and distribution. Furthermore, the formation mechanism of the protective layer was determined after clarifying the source of each component. Finally, a technical strategy was proposed for achieving a stable protective layer in the hearth. The results show that the protective layer mainly exists in a bilayer form in the sidewall, namely, a titanium-bearing layer and a graphite layer. Both the layers contain the slag phase whose major crystalline phase is magnesium melilite (Ca2MgSi2O7) and the main source of the slag phase is coke ash. It is clearly determined that solid particles such as graphite, Ti(C,N) and MgAl2O4 play an important role in the formation of the protective layer, and the key factor for promoting the formation of a stable protective layer is reasonable control of the evolution behavior of coke.

  19. Effects of varying oxygen partial pressure on molten silicon-ceramic substrate interactions

    NASA Technical Reports Server (NTRS)

    Ownby, D. P.; Barsoum, M. W.

    1980-01-01

    The silicon sessile drop contact angle was measured on hot pressed silicon nitride, silicon nitride coated on hot pressed silicon nitride, silicon carbon coated on graphite, and on Sialon to determine the degree to which silicon wets these substances. The post-sessile drop experiment samples were sectioned and photomicrographs were taken of the silicon-substrate interface to observe the degree of surface dissolution and degradation. Of these materials, silicon did not form a true sessile drop on the SiC on graphite due to infiltration of the silicon through the SiC coating, nor on the Sialon due to the formation of a more-or-less rigid coating on the liquid silicon. The most wetting was obtained on the coated Si3N4 with a value of 42 deg. The oxygen concentrations in a silicon ribbon furnace and in a sessile drop furnace were measured using the protable thoria-yttria solid solution electrolyte oxygen sensor. Oxygen partial pressures of 10 to the minus 7 power atm and 10 to the minus 8 power atm were obtained at the two facilities. These measurements are believed to represent nonequilibrium conditions.

  20. Graphite Microstructural Characterization Using Time-Domain and Correlation-Based Ultrasonics

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

    Spicer, James

    Among techniques that have been used to determine elastic modulus in nuclear graphites, ultrasonic methods have enjoyed wide use and standards using contacting piezoelectric tranducers have been developed to ensure repeatability of these types of measurements. However, the use of couplants and the pressures used to effectively couple transducers to samples can bias measurements and produce results that are not wholly related to the properties of the graphite itself. In this work, we have investigated the use of laser ultrasonic methods for making elastic modulus measurements in nuclear graphites. These methods use laser-based transmitters and receivers to gather data andmore » do not require use of ultrasonic couplants or mechanical contact with the sample. As a result, information directly related to the elastic responses of graphite can be gathered even if the graphite is porous, brittle and compliant. In particular, we have demonstrated the use of laser ultrasonics for the determination of both Young’s modulus and shear modulus in a range of nuclear graphites including those that are being considered for use in future nuclear reactors. These results have been analyzed to assess the contributions of porosity and microcracking to the elastic responses of these graphites. Laser-based methods have also been used to assess the moduli of NBG-18 and IG-110 where samples of each grade were oxidized to produce specific changes in porosity. These data were used to develop new models for the elastic responses of nuclear graphites and these models have been used to infer specific changes in graphite microstructure that occur during oxidation that affect elastic modulus. Specifically, we show how ultrasonic measurements in oxidized graphites are consistent with nano/microscale oxidation processes where basal plane edges react more readily than basal plane surfaces. We have also shown the use of laser-based methods to perform shear-wave birefringence measurements and have shown how these measurements can be used to assess elastic anisotropy in nuclear graphites. Using models developed in this program, ultrasonic data were interpreted to extract orientation distribution coefficients that could be used to represent anisotropy in these materials. This demonstration showed the use of ultrasonic methods to quantify anisotropy and how these methods provide more detailed information than do measurements of thermal expansion – a technique commonly used for assessing anisotropy in nuclear graphites. Finally, we have employed laser-based, ultrasonic-correlation techniques in attempts to quantify aspects of graphite microstructure such as pore size and distribution. Results of these measurements indicate that additional work must be performed to make this ultrasonic approach viable for quantitative microstructural characterization.« less

  1. Fractography of modern engineering materials: composites and metals

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

    Masters, J.E.; Au, J.J.

    1987-01-01

    The fractographic analysis of fracture surfaces in composites and metals is discussed in reviews and reports of recent theoretical and experimental investigations. Topics addressed include fracture-surface micromorphology in engineering solids, SEM fractography of pure and mixed-mode interlaminar fractures in graphite/epoxy composites, determination of crack propagation directions in graphite/epoxy structures, and the fracture surfaces of irradiated composites. Consideration is given to fractographic feature identification and characterization by digital imaging analysis, fractography of pressure-vessel steel weldments, the micromechanisms of major/minor cycle fatigue crack growth in Inconel 718, and fractographic analysis of hydrogen-assisted cracking in alpha-beta Ti alloys.

  2. Graphite in an Apollo 17 impact melt breccia.

    PubMed

    Steele, A; McCubbin, F M; Fries, M; Glamoclija, M; Kater, L; Nekvasil, H

    2010-07-02

    We report on the detection of discrete grains of crystalline graphite and graphite whiskers (GWs) in an Apollo 17 impact melt breccia. Multiple instances of graphite and GWs within a discrete area of the sample imply that these grains are not terrestrial contamination. Both graphite and GWs are indicative of high-temperature conditions and are probably the result of the impact processes responsible for breccia formation. This suggests that impact processes may be an additional formation mechanism for GWs in the solar system and indicates that the Moon contains a record of ancient carbonaceous material delivered at the time of the Late Heavy Bombardment.

  3. Analysis of vibrational response in graphite oxide nanoplatelets

    NASA Astrophysics Data System (ADS)

    Prias Barragan, Jhon Jairo; Gross, Katherine; Lajaunie, Luc; Arenal, Raul; Ariza Calderon, Hernando; Prieto, Pedro

    In this work, we present a new low-cost fabrication process to obtain graphite oxide nanoplatelets from bamboo pyroligneous acid (GO-BPA) by thermal decomposition method using a pyrolysis system for different carbonization temperatures from 673 to 973 K. The GO-BPA samples were characterized by using Raman, FTIR, XRD, SEM and TEM techniques, whose results suggest that increased carbonization temperature increases graphite conversion, boundary defects, desorption of some organic compounds and phonon response, respectively. We discuss potential applications of the GO-BPA samples involving phonon response that would benefit from a fully scaled technology, advanced electronic sensors and devices.

  4. Inductively Coupled Plasma Optical Emission Spectrometry for Rare Earth Elements Analysis

    NASA Astrophysics Data System (ADS)

    He, Man; Hu, Bin; Chen, Beibei; Jiang, Zucheng

    2017-01-01

    Inductively coupled plasma optical emission spectrometry (ICP-OES) merits multielements capability, high sensitivity, good reproducibility, low matrix effect and wide dynamic linear range for rare earth elements (REEs) analysis. But the spectral interference in trace REEs analysis by ICP-OES is a serious problem due to the complicated emission spectra of REEs, which demands some correction technology including interference factor method, derivative spectrum, Kalman filtering algorithm and partial least-squares (PLS) method. Matrix-matching calibration, internal standard, correction factor and sample dilution are usually employed to overcome or decrease the matrix effect. Coupled with various sample introduction techniques, the analytical performance of ICP-OES for REEs analysis would be improved. Compared with conventional pneumatic nebulization (PN), acid effect and matrix effect are decreased to some extent in flow injection ICP-OES, with higher tolerable matrix concentration and better reproducibility. By using electrothermal vaporization as sample introduction system, direct analysis of solid samples by ICP-OES is achieved and the vaporization behavior of refractory REEs with high boiling point, which can easily form involatile carbides in the graphite tube, could be improved by using chemical modifier, such as polytetrafluoroethylene and 1-phenyl-3-methyl-4-benzoyl-5-pyrazone. Laser ablation-ICP-OES is suitable for the analysis of both conductive and nonconductive solid samples, with the absolute detection limit of ng-pg level and extremely low sample consumption (0.2 % of that in conventional PN introduction). ICP-OES has been extensively employed for trace REEs analysis in high-purity materials, and environmental and biological samples.

  5. Macrosegregation Caused by Convection Associated with Directional Solidification through Cross-Section Change

    NASA Technical Reports Server (NTRS)

    Ghods, M.; Lauer, M.; Tewari, S. N.; Poirier, D. R..; Grugel, R. N.

    2015-01-01

    Al-7 wt% Si and Pb-6 wt% Sb alloy samples were directionally solidified (DS), with liquid above and solid below and gravity pointing down, in cylindrical graphite crucibles through an abrupt cross-section change. Fraction eutectic distribution in the microstructure, primary dendrite spacing and primary dendrite trunk diameters have been measured in the DS samples in the vicinity of section change in order to examine the effect of convection associated with the combined influence of thermosolutal factors and solidification shrinkage. It is observed that convection not only produces extensive radial and axial macrosegregation near cross-section change, it also affects the dendritic array morphology. Primary dendrite spacing and primary dendrite trunk diameter, both, are influenced by this convection. In addition to the experimental results, preliminary results from a numerical model which includes solidification shrinkage and thermosolutal convection in the mushy zone in its analysis will also be presented

  6. Chemical Characterization and Removal of C-14 from Irradiated Graphite-12010

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

    Cleaver, James; McCrory, Shilo; Smith, Tara E.

    2012-07-01

    Quantities of irradiated graphite waste are expected to drastically increase, which indicates the need for a graphite waste management strategy. Of greatest concern for long-term disposal of irradiated graphite is carbon-14 (C-14), with a half-life of 5730 years. Study of irradiated graphite from nuclear reactors indicates C-14 is concentrated on the outer 5 mm of the graphite structure. The aim of the research described here is to identify the chemical form of C-14 in irradiated graphite and develop a practical method by which C-14 can be removed. Characterization of pre- and post-irradiation graphite was conducted to determine bond type, functionalmore » groups, location and concentration of C-14 and its precursors via the use of surface sensitive characterization techniques. Because most surface C-14 originates from neutron activation of nitrogen, an understanding of nitrogen bonding to graphite may lead to a greater understanding of the formation pathway of C-14. However, no single technique provides a complete picture. Therefore, a portfolio of techniques has been developed, with each technique providing another piece to the puzzle that is the chemical nature of the C-14. Scanning Electron Microscopy (SEM), X-Ray Diffraction (XRD), and Raman Spectroscopy were used to evaluate the morphological features of graphite samples. The concentration, chemical composition, and bonding characteristics of C-14 and its precursors were determined through X-ray Photoelectron Spectroscopy (XPS), Time-of-Flight Secondary Ion Mass Spectrometry (SIMS), and Auger and Energy Dispersive X-ray Analysis Spectroscopy (EDX). High-surface-area graphite foam, POCOFoam{sup R}, was exposed to liquid nitrogen and irradiated. Characterization of this material has shown C-14 to C-12 ratios of 0.035. This information was used to optimize the thermal treatment of graphite. Thermal treatment of irradiated graphite as reported by Fachinger et al. (2007) uses naturally adsorbed oxygen complexes to gasify graphite, thus its effectiveness is highly dependent on the availability of adsorbed oxygen compounds. In research presented, the quantity and form of adsorbed oxygen complexes in pre- and post irradiated graphite was studied using SIMS and XPS. SIMS and XPS detected adsorbed oxygen compounds on both irradiated and unirradiated graphite. During thermal treatment graphite samples are heated in the presence of inert argon gas, which carries off gaseous products released during treatment. Experiments were performed at 900 deg. C and 1400 deg. C to evaluate the selective removal of C-14. (authors)« less

  7. THE FIRST DISCOVERY OF PRESOLAR GRAPHITE GRAINS FROM THE HIGHLY REDUCING QINGZHEN (EH3) METEORITE

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

    Xu, Yuchen; Lin, Yangting; Zhang, Jianchao

    Presolar graphite grains have been extensively studied, but are limited in carbonaceous chondrites, particularly in Murchison (CM2) and Orgueil (CI1), which sampled materials from the oxidizing regions in the solar nebula. Here, we report the first discovery of presolar graphite grains from the Qingzhen (EH3) enstatite chondrite which formed under a highly reducing condition. Eighteen presolar graphite grains were identified by C-isotope mapping of the low-density fraction (1.75–1.85 g cm{sup 3}) from Qingzhen acid residue. Another 58 graphite spherules were found in different areas of the same sample mount using a scanning electron microscope and were classified into three morphologies,more » including cauliflower, onion, and cauliflower–onion. The Raman spectra of these spherules vary from ordered, disordered, and glassy to kerogen-like, suggestive of a wide range of thermal metamorphisms. NanoSIMS analysis of the C- and Si-isotopes of these graphite spherules confirmed 23 presolar grains. The other 35 graphite spherules have no significant isotopic anomalies, but they share similar morphologies and Raman spectra with the presolar ones. Another three grains were identified during NanoSIMS analysis. Of all the 44 presolar graphite grains identified, six grains show {sup 28}Si-excesses, suggestive of supernovae origins, and four grains are {sup 12}C- and {sup 29,30}Si-rich, consistent with low-metallicity asymptotic giant branch star origins. Another two graphite spherules have extremely low {sup 12}C/{sup 13}C ratios with marginal solar Si-isotopes. The morphologies, Raman spectra, and C- and Si-isotopic distributions of the presolar graphite grains from the Qingzhen enstatite chondrite are similar to those of the low-density fractions from Murchison carbonaceous chondrites. This study suggests a homogeneous distribution of presolar graphite grains in the solar nebula.« less

  8. Galvanic Corrosion In (Graphite/Epoxy)/Alloy Couples

    NASA Technical Reports Server (NTRS)

    Danford, Merlin D.; Higgins, Ralph H.

    1988-01-01

    Effects of galvanic coupling between graphite/epoxy composite material, G/E, and D6AC steel, 6061-T6 aluminum, and Inconel(R) 718 nickel alloy in salt water described in report. Introductory section summarizes previous corrosion studies of G/E with other alloys. Details of sample preparation presented along with photographs of samples before and after immersion.

  9. Rapid reduction of MORB glass in piston cylinder experiments with graphite capsule - a XANES study

    NASA Astrophysics Data System (ADS)

    Ni, P.; Zhang, Y.; Fiege, A.; Newville, M.; Lanzirotti, A.

    2017-12-01

    Graphite capsules have been widely used in high-pressure, high-temperature experiments to prevent iron loss from iron-bearing samples. One common uncertainty with this experimental setup is the oxygen fugacity (fO2) inside the capsule imposed by the presence of graphite. As Holloway et al. (1992) pointed out, the use of graphite capsule places an upper limit on the fO2 in the experiment to be below CCO (graphite-CO-CO2 buffer). More recently, Medard et al. (2015) estimated the fO2 for their experiments using Pt-graphite or graphite-only capsules to be CCO-0.8. Despite the improved understanding on the fO2 using graphite capsule, the mechanism and kinetics of fO2 control in graphite capsule is still poorly understood. Such knowledge is especially important to understand whether equilibrium fO2 is reached in the sample when short experiment durations are needed (e.g. for kinetic experiments). In this study, MORB glasses after olivine dissolution (Chen and Zhang 2008) and plagioclase dissolution (Yu et al. 2016) experiments at 0.5 GPa and 1300 ºC with durations ranging from 10 s to 30 min are analyzed by XANES to obtain Fe3+/Fetotal profiles from their contact with the graphite capsule. The results show rapid Fe reduction away from the graphite-melt interface, causing a decrease of Fe3+/Fetotal from 12% to 3%. In a duration of 30 min, the 1200-µm-thick and 2000-µm-diameter basaltic glass reached near equilibrium in its iron oxidation state, with Fe3+/Fetotal ranging from 3% to 4% throughout the run product. The equilibrium Fe3+/Fetotal ratio corresponds to an fO2 of CCO-1.4, which is within error compared to the result in Medard et al. (2015). Even in the shortest experiment with an effective duration of only 10 s, a 60 µm long reduction profile was detected. Such a rapid fO2 change can be explained by rapid H2 diffusion in melt and its reaction with ferric iron: H2+Fe2O3=2FeO+H2O, which is also supported by the H2O concentration profiles measured along the reduction profile. Our results indicate rapid fO2 equilibration in MORB-glass-composition samples during nominally anhydrous graphite capsule experiments at 1300°C, and can be used to guide experimental designs.

  10. Shock Initiation of Thermally Expanded TATB

    NASA Astrophysics Data System (ADS)

    Mulford, Roberta; Swift, Damian

    2011-06-01

    The plastic-bonded explosive PBX-9502 undergoes unusual hysteretic thermal expansion, or ``ratchet growth'' as a consequence of the uniaxial thermal expansion of the graphitic structure of the major component, TATB explosive. Upon thermal cycling, the density of the material can be reduced by as much as 9%, resulting in a distinct increase in the shock sensitivity of the solid. Run distances to detonation have been measured in thermally expanded samples of PBX-9502, using embedded particle velocity gauges and shock tracker gauges. Uniaxial shocks were generated using a light gas gun, to provide a repeatable stimulus for initiation of detonation. We have applied a porosity model to adjust standard Pop plot data to the reduced density of our samples, to investigate whether the sensitivity of the PBX 9502 increases ideally with the decreasing density, or whether the microscopically non-uniform expansion that occurs during ``ratchet growth'' leads to abnormal sensitivity, possibly as a result of cracking or debonding from the binder, as observed in micrographs of the sample.

  11. Graphite-(Mo,W)S2 intergrowth as a palaeoenvironmental proxy in metasedimentary rocks

    NASA Astrophysics Data System (ADS)

    Cabral, Alexandre Raphael; Zeh, Armin; da Silva Viana, Nívea Cristina; Schirmer, Thomas; Lehmann, Bernd

    2017-12-01

    Molybdenum enrichment in pristine organic-C-rich sedimentary rocks forms the basis for inferring the presence of dissolved oxygen in seawater. Organic matter removes dissolved hexavalent Mo from seawater where anoxic and euxinic conditions are attained. However, it is unknown whether this Mo-based proxy is retained under metamorphic conditions where organic C is no longer preserved. Here, we describe aggregates of graphite and molybdenite (MoS2) containing up to 21 mass per cent of W as tungstenite (WS2) in solid solution. These aggregates are disseminated in a sulfide-rich Mn-silicate-carbonate rock (queluzite), metamorphosed under amphibolite-facies conditions within the Archaean Barbacena greenstone belt in Minas Gerais, Brazil. Our finding indicates that: (i) W is, like Mo, a palaeoenvironmental proxy; (ii) the W proxy is sensitive to high fS2/fO2 environments; (iii) both Mo and W proxies survive amphibolite-facies overprint as (Mo,W)S2 intergrown with graphite. Archaean greenstones are potential candidates for storing palaeoenvironmental information as (Mo,W)S2-graphite intergrowths.

  12. Overview of SBIR Phase II Work on Hollow Graphite Fibers

    NASA Technical Reports Server (NTRS)

    Stallcup, Michael; Brantley, Lott W. (Technical Monitor)

    2001-01-01

    Ultra-Lightweight materials are enabling for producing space based optical components and support structures. Heretofore, innovative designs using existing materials has been the approach to produce lighter-weight optical systems. Graphite fiber reinforced composites, because of their light weight, have been a material of frequent choice to produce space based optical components. Hollow graphite fibers would be lighter than standard solid graphite fibers and, thus, would save weight in optical components. The Phase I SBIR program demonstrated it is possible to produce hollow carbon fibers that have strengths up to 4.2 GPa which are equivalent to commercial fibers, and composites made from the hollow fibers had substantially equivalent composite strengths as commercial fiber composites at a 46% weight savings. The Phase II SBIR program will optimize processing and properties of the hollow carbon fiber and scale-up processing to produce sufficient fiber for fabricating a large ultra-lightweight mirror for delivery to NASA. Information presented here includes an overview of the strength of some preliminary hollow fibers, photographs of those fibers, and a short discussion of future plans.

  13. The Role of Cesium Cation in Controlling Interphasial Chemistry on Graphite Anode in Propylene Carbonate-Rich Electrolytes

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

    Xiang, Hongfa; Mei, Donghai; Yan, Pengfei

    2015-09-10

    Propylene carbonate (PC) is seldom used in lithium-ion batteries (LIBs) due to its sustained co-intercalation into graphene structure and the eventual graphite exfoliation, despite potential advantages it brings, such as wider liquid range and lower cost. Here we discover that cesium cation (Cs+), originally used to suppress dendrite growth of Li metal anode, directs the formation of solid electrolyte interphase (SEI) on graphitic anode in PC-rich electrolytes through preferential solvation. Effective suppression of PC-decomposition and graphite-exfoliation was achieved when the ratio of ethylene carbonate (EC)/PC in electrolytes was so adjusted that the reductive decomposition of Cs+-(EC)m (1≤m≤2) complex precedes thatmore » of Li+-(PC)n (3≤n≤5). The interphase directed by Cs+ is stable, ultrathin and compact, leading to significant improvements in LIB performances. In a broader context, the accurate tailoring of SEI chemical composition by introducing a new solvation center represents a fundamental breakthrough in manipulating interfacial reactions processes that once were elusive.« less

  14. Graphite Black shale of Vendas de Ceira, Coimbra, Portugal

    NASA Astrophysics Data System (ADS)

    Quinta-Ferreira, Mário; Silva, Daniela; Coelho, Nuno; Gomes, Ruben; Santos, Ana; Piedade, Aldina

    2017-04-01

    The graphite black shale of Vendas de Ceira located in south of Coimbra (Portugal), caused serious instability problems in recent road excavation slopes. The problems increased with the rain, transforming shales into a dark mud that acquires a metallic hue when dried. The black shales are attributed to the Devonian or eventually, to the Silurian. At the base of the slope is observed graphite black shale and on the topbrown schist. Samples were collected during the slope excavation works. Undisturbed and less altered materials were selected. Further, sampling was made difficult as the graphite shale was covered by a thick layer of reinforced concrete, which was used to stabilize the excavated surfaces. The mineralogy is mainly constituted by quartz, muscovite, ilite, ilmenite and feldspar without the presence of expansive minerals. The organic matter content is 0.3 to 0.4%. The durability evaluated by the Slake Durability Test varies from very low (Id2 of 6% for sample A) to high (98% for sample C). The grain size distribution of the shale particles, was determined after disaggregation with water, which allowed verifying that sample A has 37% of fines (5% of clay and 32% of silt) and 63% of sand, while sample C has only 14% of fines (2% clay and 12% silt) and 86% sand, showing that the decrease in particle size contributes to reduce durability. The unconfined linear expansion confirms the higher expandability (13.4%) for sample A, reducing to 12.1% for sample B and 10.5% for sample C. Due the shale material degradated with water, mercury porosimetry was used. While the dry weight of the three samples does not change significantly, around 26 kN/m3, the porosity is much higher in sample A with 7.9% of pores, reducing to 1.4% in sample C. The pores size vary between 0.06 to 0.26 microns, does not seem to have any significant influence in the shale behaviour. In order to have a comparison term, a porosity test was carried out on the low weatherable brown shale, which is quite abundant at the site. The main difference to the graphite shale is the high porosity of the brown shale with 14.7% and the low volume weight of 23 kN/m3, evidencing the distinct characteristics of the graphite schists. The maximum strength was evaluated by the Schmidt hammer, as the point load test could not be performed as the rock was very soft. The maximum estimated values on dry samples were 32 MPa for sample A and 85 MPa for sample C. The results show a singular material characterized by significant heterogeneity. It can be concluded that for the graphite schists the smaller particle size and higher porosity make the soft rock extremely weatherable when decompressed and exposed to water, as a result of high capillary tension and reduced cohesion. They also exhibit high expansion and an enormous degradation of the rock presenting a behaviour close to a soil. The graphite black schist is a highly weatherable soft rock, without expansive minerals, with small pores, in which the porosity, low strength and low cohesion allow their rapid degradation when decompressed and exposed to the action of Water.

  15. Formation mechanism of graphite hexagonal pyramids by argon plasma etching of graphite substrates

    NASA Astrophysics Data System (ADS)

    Glad, X.; de Poucques, L.; Bougdira, J.

    2015-12-01

    A new graphite crystal morphology has been recently reported, namely the graphite hexagonal pyramids (GHPs). They are hexagonally-shaped crystals with diameters ranging from 50 to 800 nm and a constant apex angle of 40°. These nanostructures are formed from graphite substrates (flexible graphite and highly ordered pyrolytic graphite) in low pressure helicon coupling radiofrequency argon plasma at 25 eV ion energy and, purportedly, due to a physical etching process. In this paper, the occurrence of peculiar crystals is shown, presenting two hexagonal orientations obtained on both types of samples, which confirms such a formation mechanism. Moreover, by applying a pretreatment step with different time durations of inductive coupling radiofrequency argon plasma, for which the incident ion energy decreases at 12 eV, uniform coverage of the surface can be achieved with an influence on the density and size of the GHPs.

  16. Structural properties of atactic polystyrene adsorbed onto solid surfaces.

    PubMed

    Tatek, Yergou B; Tsige, Mesfin

    2011-11-07

    In the present work, we are studying the local conformation of chains in a thin film of polystyrene adsorbed on a solid substrate by using atomistically detailed simulations. The simulations are carried out by using the readily available and massively parallel molecular dynamics code known as LAMMPS. In particular, a special emphasis is given to the density and orientation of side chains (which consist of phenyl groups and methylene units) at solid/polymer and polymer/vacuum interfaces. Three types of substrates were used in our study: α-quartz, graphite, and amorphous silica. Our investigation was restricted to atactic polystyrene. Our results show that the density and structural properties of side chains depend on the type of surface. An excess of phenyl rings is observed near the α-quartz substrate while the film adsorbed on graphite is depleted in C(6)H(5). Moreover, the orientation of the rings and methylene units on the substrate/film interface show a strong dependence on the type of the substrate, while the rings at the film/vacuum interface show a marked tendency to point outward, away from the film. The results we obtained are in a large part in good agreement with previous experimental and simulation results.

  17. Sintering polycrystalline olivine and polycrystalline clinopyroxene containing trace amount of graphite from natural crystals

    NASA Astrophysics Data System (ADS)

    Tsubokawa, Yumiko; Ishikawa, Masahiro

    2017-09-01

    Graphite-bearing polycrystalline olivine and polycrystalline clinopyroxene with submicron to micron grain size were successfully sintered from a single crystal of naturally occurring olivine (Fo88-92Fa12-8: Mg1.76-1.84Fe0.16-0.24SiO4) and a single crystal of naturally occurring clinopyroxene (Di99Hed1: Ca0.92Na0.07Mn0.01Mg0.93Fe0.01Al0.06Si2O6). The milled powders of both these crystals were sintered under argon gas flow at temperatures ranging from 1130 to 1350 °C for 2 h. As the sintering temperature increased, the average grain size of olivine increased from 0.2 to 1.4 µm and that of clinopyroxene increased from 0.1 to 2.4 µm. The porosity of sintered samples remained at an almost-constant volume of 2-5% for olivine and 3-4% for clinopyroxene. The samples sintered from powders milled with ethanol exhibited trace amount of graphite, identified via Raman spectroscopy analysis. As the sintering temperature increased, the intensity of the graphite Raman peak decreased, compared with both olivine and clinopyroxene peaks. The carbon content of the sintered samples was estimated to be a few hundred ppm. The in-plane size ( L a ) of graphite in the sintered olivine was estimated to be <15 nm. Our experiments demonstrate new possibilities for preparing graphite-bearing silicate-mantle mineral rocks, and this method might be useful in understanding the influence of the physical properties of graphite on grain-size-sensitive rheology or the seismic velocity of the Earth's mantle.[Figure not available: see fulltext.

  18. Preparation and characterization of copper-graphite composites by electrical explosion of wire in liquid.

    PubMed

    Bien, T N; Gul, W H; Bac, L H; Kim, J C

    2014-11-01

    Copper-graphite nanocomposites containing 5 vol.% graphite were prepared by a powder metallurgy route using an electrical wire explosion (EEW) in liquid method and spark plasma sintering (SPS) process. Graphite rods with a 0.3 mm diameter and copper wire with a 0.2 mm diameter were used as raw materials for EEWin liquid. To compare, a pure copper and copper-graphite mixture was also prepared. The fabricated graphite was in the form of a nanosheet, onto which copper particles were coated. Sintering was performed at 900 degrees C at a heating rate of 30 degrees C/min for 10 min and under a pressure of 70 MPa. The density of the sintered composite samples was measured by the Archimedes method. A wear test was performed by a ball-on-disc tribometer under dry conditions at room temperature in air. The presence of graphite effectively reduced the wear of composites. The copper-graphite nanocomposites prepared by EEW had lower wear rates than pure copper material and simple mixed copper-graphite.

  19. Study of evaporating the irradiated graphite in equilibrium low-temperature plasma

    NASA Astrophysics Data System (ADS)

    Bespala, E. V.; Novoselov, I. Yu.; Pavlyuk, A. O.; Kotlyarevskiy, S. G.

    2018-01-01

    The paper describes a problem of accumulation of irradiated graphite due to operation of uranium-graphite nuclear reactors. The main noncarbon contaminants that contribute to the overall activity of graphite elements are iso-topes 137Cs, 60Co, 90Sr, 36Cl, and 3H. A method was developed for processing of irradiated graphite ensuring the volu-metric decontamination of samples. The calculation results are presented for equilibrium composition of plasma-chemical reactions in systems "irradiated graphite-argon" and "irradiated graphite-helium" for a wide range of tem-peratures. The paper describes a developed mathematical model for the process of purification of a porous graphite surface treated by equilibrium low-temperature plasma. The simulation results are presented for the rate of sublimation of radioactive contaminants as a function of plasma temperature and plasma flow velocity when different plasma-forming gases are used. The extraction coefficient for the contaminant 137Cs from the outer side of graphite pores was calculated. The calculations demonstrated the advantages of using a lighter plasma forming gas, i.e., helium.

  20. Measurement of leakage neutron spectra from graphite cylinders irradiated with D-T neutrons for validation of evaluated nuclear data.

    PubMed

    Luo, F; Han, R; Chen, Z; Nie, Y; Shi, F; Zhang, S; Lin, W; Ren, P; Tian, G; Sun, Q; Gou, B; Ruan, X; Ren, J; Ye, M

    2016-10-01

    A benchmark experiment for validation of graphite data evaluated from nuclear data libraries was conducted for 14MeV neutrons irradiated on graphite cylinder samples. The experiments were performed using the benchmark experimental facility at the China Institute of Atomic Energy (CIAE). The leakage neutron spectra from the surface of graphite (Φ13cm×20cm) at 60° and 120° and graphite (Φ13cm×2cm) at 60° were measured by the time-of-flight (TOF) method. The obtained results were compared with the measurements made by the Monte Carlo neutron transport code MCNP-4C with the ENDF/B-VII.1, CENDL-3.1 and JENDL-4.0 libraries. The results obtained from a 20cm-thick sample revealed that the calculation results with CENDL-3.1 and JENDL-4.0 libraries showed good agreements with the experiments conducted in the whole energy region. However, a large discrepancy of approximately 40% was observed below the 3MeV energy region with the ENDF/B-VII.1 library. For the 2cm-thick sample, the calculated results obtained from the abovementioned three libraries could not reproduce the experimental data in the energy range of 5-7MeV. The graphite data in CENDL-3.1 were verified for the first time and were proved to be reliable. Copyright © 2016 Elsevier Ltd. All rights reserved.

  1. Compatibility of the Radio Frequency Mass Gauge with Graphite-Epoxy Composite Tanks

    NASA Technical Reports Server (NTRS)

    Zimmerli, G. A.; Mueller, C. H.

    2015-01-01

    The radio frequency mass gauge (RFMG) is a low-gravity propellant quantity gauge being developed at NASA for possible use in long-duration space missions utilizing cryogenic propellants. As part of the RFMG technology development process, we evaluated the compatibility of the RFMG with a graphite-epoxy composite material used to construct propellant tanks. The key material property that can affect compatibility with the RFMG is the electrical conductivity. Using samples of 8552/IM7 graphite-epoxy composite, we characterized the resistivity and reflectivity over a range of frequencies. An RF impedance analyzer was used to characterize the out-of-plane electrical properties (along the sample thickness) in the frequency range 10 to 1800 MHZ. The resistivity value at 500 MHz was 4.8 ohm-cm. Microwave waveguide measurements of samples in the range 1.7 - 2.6 GHz, performed by inserting the samples into a WR-430 waveguide, showed reflectivity values above 98%. Together, these results suggested that a tank constructed from graphite/epoxy composite would produce good quality electromagnetic tank modes, which is needed for the RFMG. This was verified by room-temperature measurements of the electromagnetic modes of a 2.4 m diameter tank constructed by Boeing from similar graphite-epoxy composite material. The quality factor Q of the tank electromagnetic modes, measured via RF reflection measurements from an antenna mounted in the tank, was typically in the range 400 less than Q less than 3000. The good quality modes observed in the tank indicate that the RFMG is compatible with graphite-epoxy tanks, and thus the RFMG could be used as a low-gravity propellant quantity gauge in such tanks filled with cryogenic propellants.

  2. The Place for Thermoplastic Composites in Structural Components

    DTIC Science & Technology

    1987-12-01

    The molten tube is then squashed flat and consolidated into ribbon form by continuous opposed-belt laminating. Existing graphite-epoxy pultrusion...the solid form it must have a molecular weight that exceeds the critical entanglement value. Thus thermoplastic materials of commercial worth almost

  3. Supercooling of Hydrogen on Template Materials to Deterministically Seed Ignition-Quality Solid Fuel Layers

    DOE PAGES

    Shin, S. J.; Zepeda-Ruiz, L. A.; Lee, J. R. I.; ...

    2016-09-01

    In this study, we explored templating effects of various materials for hydrogen (H 2 and D 2) solidification by measuring the degree of supercooling required for liquid hydrogen to solidify below each triple point. The results show high supercooling (>100 mK) for most metallic, covalent, and ionic solids, and low supercooling (<100 mK) for van der Waals (vdW) solids. We attribute the low supercooling of vdW solids to the weak interaction of the substrate and hydrogen. Highly ordered pyrolytic graphite showed the lowest supercooling among materials that are solid at room temperature, but did not exhibit a templating effect withinmore » a fill-tube and capsule assembly.« less

  4. Applying the Coupled-Cluster Ansatz to Solids and Surfaces in the Thermodynamic Limit

    NASA Astrophysics Data System (ADS)

    Gruber, Thomas; Liao, Ke; Tsatsoulis, Theodoros; Hummel, Felix; Grüneis, Andreas

    2018-04-01

    Modern electronic structure theories can predict and simulate a wealth of phenomena in surface science and solid-state physics. In order to allow for a direct comparison with experiment, such ab initio predictions have to be made in the thermodynamic limit, substantially increasing the computational cost of many-electron wave-function theories. Here, we present a method that achieves thermodynamic limit results for solids and surfaces using the "gold standard" coupled cluster ansatz of quantum chemistry with unprecedented efficiency. We study the energy difference between carbon diamond and graphite crystals, adsorption energies of water on h -BN, as well as the cohesive energy of the Ne solid, demonstrating the increased efficiency and accuracy of coupled cluster theory for solids and surfaces.

  5. New developments in the Paris-Edinburgh cell program at HPCAT

    NASA Astrophysics Data System (ADS)

    Park, C.; Kenney-Benson, C.; Kono, Y.; Shen, G.; Yu, T.; Sakamaki, T.; Jing, Z.; Wang, Y.; Abd El Qader, M.; Baker, J.; Kumar, R.; Velisavljevic, N.

    2011-12-01

    The Paris-Edinburgh cell at HPCAT 16BM-B station is capable of maintaining sample pressure and temperature up to 7GPa and 2,300K for long durations more than 24 hrs for various types of materials in the molten state. Materials including rock forming minerals, metal alloys, semiconductors, and energetic organic compounds have been studied for their liquid structures and phase transition behaviors under these conditions. The sample volume ranges from 0.03 mm3 to 1.2 mm3 by adjusting the cylindrical sample diameter depending on x-ray attenuation, while the sample height available for x-ray scattering is limited to 0.4 mm due to the gap between the two co-axial WC anvils. The sample cell assembly has been optimized for x-ray transparency, chemical inertness, and thermal insulation using boron-epoxy composite gasket, hexagonal boron nitride or graphite crucible, and low density magnesia supporting the cylindrical graphite heater. For consistent measurements of liquid/amorphous and crystalline structures during melting and phase transitions, the energy-dispersive x-ray diffraction (EDXD) with multiple 2θ angles is applied, fully exploiting the bending magnet white beam spectrum provided by the Advanced Photon Source up to 120 keV energy. Fine collimation slits are applied for the diffracted beam to control the depth resolution at various diffraction angles and to minimize background scattering from the pressure media. A real-time radiography imaging system is also statically installed at the beamline for sample alignment and 2D projection volumetry applications. This combined setup is established as the routine PEC application at the station. Recently, a few new capabilities have been added: Ultrasonic velocity measurement for liquid samples having a disc shape (0.2-0.4 mm in thickness) has been successfully commissioned with the help of the radiography imaging system, which calibrates the acoustic travel distances through the sample cell assembly within 5 μm uncertainty. The white beam radiography also has been utilized in an in-situ thermoelectric property measurement for high-pressure solid phase. Electrical resistivity, thermoelectric coefficient (Seebeck coefficient), and thermal conductivity of solid phases can be simultaneously measured with a four-probe approach using inserted thermocouple wires. These new applications were made through substantial modifications of the sample assembly components as well as adding in-situ probing electrodes in- and outside of the PE anvils. These series of new instrumental developments at HPCAT opened new opportunities for in-situ studies of structure and property correlations for melts. New developments to extend the pressure and temperature capabilities while retaining the outstanding stability of the sample in molten state are ongoing.

  6. Lithium storage in structurally tunable carbon anode derived from sustainable source

    DOE PAGES

    Lim, Daw Gen; Kim, Kyungho; Razdan, Mayuri; ...

    2017-09-01

    Here, a meticulous solid state chemistry approach has been developed for the synthesis of carbon anode from a sustainable source. The reaction mechanism of carbon formation during pyrolysis of sustainable feed-stock was studied in situ by employing Raman microspectroscopy. No Raman spectral changes observed below 160°C (thermally stable precursor) followed by color change, however above 280°C characteristic D and G bands of graphitic carbon are recorded. Derived carbon particles exhibited high specific surface area with low structural ordering (active carbons) to low specific surface area with high graphitic ordering as a function of increasing reaction temperature. Carbons synthesized at 600°Cmore » demonstrated enhanced reversible lithiation capacity (390 mAh g -1), high charge-discharge rate capability, and stable cycle life. On the contrary, carbons synthesized at higher temperatures (>1200°C) produced more graphite-like structure yielding longer specific capacity retention with lower reversible capacity.« less

  7. Synthesis and characterization of CdS-based ternary composite for enhanced visible light-driven photocatalysis

    NASA Astrophysics Data System (ADS)

    Singh, Arvind; Sinha, A. S. K.

    2018-09-01

    Active ternary graphite and alumina-supported cadmium sulphide (CdS) composite was synthesized by impregnation method followed by high-temperature solid-gas reaction and characterized by X-ray diffraction (XRD), photoluminescence spectroscopy (PL), diffuse reflectance spectroscopy (DRS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDX) and X-ray photoelectron spectroscopy (XPS) techniques. The ternary CdS-graphite-alumina composite exhibited superior catalytic activity compared with the binary CdS-alumina composite due to its better visible-light absorption and higher charge separation. The ternary composite has a bed-type structure. It permits a greater interaction at the interface due to intimate contact between CdS and graphite in the ternary composite. This composite has a highly efficient visible light-driven photocatalytic activity for sustainable hydrogen production. It is also capable of degrading organic dyes in wastewater.

  8. Adhesion force interactions between cyclopentane hydrate and physically and chemically modified surfaces.

    PubMed

    Aman, Zachary M; Sloan, E Dendy; Sum, Amadeu K; Koh, Carolyn A

    2014-12-07

    Interfacial interactions between liquid-solid and solid-solid phases/surfaces are of fundamental importance to the formation of hydrate deposits in oil and gas pipelines. This work establishes the effect of five categories of physical and chemical modification to steel on clathrate hydrate adhesive force: oleamide, graphite, citric acid ester, nonanedithiol, and Rain-X anti-wetting agent. Hydrate adhesive forces were measured using a micromechanical force apparatus, under both dry and water-wet surface conditions. The results show that the graphite coating reduced hydrate-steel adhesion force by 79%, due to an increase in the water wetting angle from 42 ± 8° to 154 ± 7°. Two chemical surface coatings (nonanedithiol and the citric acid ester) induced rapid hydrate growth in the hydrate particles; nonanedithiol increased hydrate adhesive force by 49% from the baseline, while the citric acid ester coating reduced hydrate adhesion force by 98%. This result suggests that crystal growth may enable a strong adhesive pathway between hydrate and other crystalline structures, however this effect may be negated in cases where water-hydrocarbon interfacial tension is minimised. When a liquid water droplet was placed on the modified steel surfaces, the graphite and citric acid ester became less effective at reducing adhesive force. In pipelines containing a free water phase wetting the steel surface, chemical or physical surface modifications alone may be insufficient to eliminate hydrate deposition risk. In further tests, the citric acid ester reduced hydrate cohesive forces by 50%, suggesting mild activity as a hybrid anti-agglomerant suppressing both hydrate deposition and particle agglomeration. These results demonstrate a new capability to develop polyfunctional surfactants, which simultaneously limit the capability for hydrate particles to aggregate and deposit on the pipeline wall.

  9. Carbide coated fibers in graphites-aluminum composites. [(fabrication of metal matrix composites)

    NASA Technical Reports Server (NTRS)

    Imprescia, R. J.; Levinson, L. S.; Reiswig, R. D.; Wallace, T. C.; Williams, J. M.

    1976-01-01

    Research activities are described for a NASA-supported program at the Los Alamos Scientific Laboratory to develop graphite fiber-aluminum matrix composites. A chemical vapor deposition apparatus was constructed for continuously coating graphite fibers with TiC. As much as 150 meters of continuously coated fibers were produced. Deposition temperatures were varied from 1365 K to about 1750 K, and deposition time from 6 to 150 seconds. The 6 sec deposition time corresponded to a fiber feed rate of 2.54 m/min through the coater. Thin, uniform, adherent TiC coats, with thicknesses up to approximately 0.1 micrometer were produced on the individual fibers of Thornel 50 graphite yarns without affecting fiber strength. Although coat properties were fairly uniform throughout a given batch, more work is needed to improve the batch-to-batch reproducibility. Samples of TiC-coated Thornel 50 fibers were infiltrated with an aluminum alloy and hot-pressed in vacuum to produce small composite bars for flexure testing. Strengths as high as 90% of the rule-of-mixtures strength were achieved. Results of the examination of the fracture surfaces indicate that the bonding between the aluminum and the TiC-coated fibers is better than that achieved in a similar, commercially infiltrated material made with fibers having no observable surface coats. Several samples of Al-infiltrated, TiC-coated Thornel 50 graphite yarns, together with samples of the commercially infiltrated, uncoated fibers, were heated for 100 hours at temperatures near the alloy solidus. The TiC-coated samples appear to undergo less reaction than do the uncoated samples. Photomicrographs are shown.

  10. Local Magnetic Measurements of Trapped Flux Through a Permanent Current Path in Graphite

    NASA Astrophysics Data System (ADS)

    Stiller, Markus; Esquinazi, Pablo D.; Quiquia, José Barzola; Precker, Christian E.

    2018-04-01

    Temperature- and field-dependent measurements of the electrical resistance of different natural graphite samples suggest the existence of superconductivity at room temperature in some regions of the samples. To verify whether dissipationless electrical currents are responsible for the trapped magnetic flux inferred from electrical resistance measurements, we localized them using magnetic force microscopy on a natural graphite sample in remanent state after applying a magnetic field. The obtained evidence indicates that at room temperature a permanent current flows at the border of the trapped flux region. The current path vanishes at the same transition temperature T_c≈ 370 K as the one obtained from electrical resistance measurements on the same sample. This sudden decrease in the phase is different from what is expected for a ferromagnetic material. Time-dependent measurements of the signal show the typical behavior of flux creep of a permanent current flowing in a superconductor. The overall results support the existence of room-temperature superconductivity at certain regions in the graphite structure and indicate that magnetic force microscopy is suitable to localize them. Magnetic coupling is excluded as origin of the observed phase signal.

  11. Operation of the “Small” BioAMS spectrometers at CAMS: Past and future prospects

    DOE PAGES

    Ognibene, T. J.; Haack, K. W.; Bench, G.; ...

    2015-05-26

    A summary of results from the solid samples run on our compact 1 MV AMS system over its 13.5 years of operation is presented. On average 7065 samples per year were measured with that average dropping to 3278 samples per year following the deployment of our liquid sample capability. Although the dynamic range of our spectrometer is 4.5 orders in magnitude, most of the measured graphitic samples had 14C/C concentrations between 0.1 and 1 modern. Furthermore, the measurements of our ANU sucrose standard followed a Gaussian distribution with an average of 1.5082 ± 0.0134 modern. The LLNL biomedical AMS programmore » supported many different types of experiments, however, the large majority of samples measured were derived from animal model systems. We have transitioned all of our biomedical AMS measurements to the recently installed 250 kV SSAMS instrument with good agreement compared in measured 14C/C isotopic ratios between sample splits. We then present results from replacement of argon stripping gas with helium in the SSAMS with a 22% improvement in ion transmission through the accelerator and high-energy analyzing magnet.« less

  12. Operation of the “Small” BioAMS Spectrometers at CAMS: Past and Future Prospects

    PubMed Central

    Ognibene, T.J.; Haack, K.W.; Bench, G.; Brown, T.A.; Turteltaub, K.W.

    2015-01-01

    A summary of results from the solid samples run on our compact 1 MV AMS system over its 13.5 years of operation is presented. On average 7065 samples per year were measured with that average dropping to 3278 samples per year following the deployment of our liquid sample capability. Although the dynamic range of our spectrometer is 4.5 orders in magnitude, most of the measured graphitic samples had 14C/C concentrations between 0.1 and 1 modern. The measurements of our ANU sucrose standard followed a Gaussian distribution with an average of 1.5082 ± 0.0134 modern. The LLNL biomedical AMS program supported many different types of experiments, however, the large majority of samples measured were derived from animal model systems. We have transitioned all of our biomedical AMS measurements to the recently installed 250 kV SSAMS instrument with good agreement compared in measured 14C/C isotopic ratios between sample splits. Finally, we present results from replacement of argon stripping gas with helium in the SSAMS with a 22% improvement in ion transmission through the accelerator and high-energy analyzing magnet. PMID:26456990

  13. Simultaneous Enrichment of Polycyclic Aromatic Hydrocarbons and Cu(2+) in Water Using Tetraazacalix[2]arene[2]triazine as a Solid-Phase Extraction Selector.

    PubMed

    Zhao, Wenjie; Yang, Liu; He, Lijun; Zhang, Shusheng

    2016-08-10

    On the basis of the definite retention mechanism proven by the stationary phase for high-performance liquid chromatography, tetraazacalix[2]arene[2]triazine featuring multiple recognition sites was assessed as a solid-phase extraction (SPE) selector. The applicability of its silica support was used for the extraction of trace amounts of polycyclic aromatic hydrocarbons (PAHs) and Cu(2+) in aqueous samples, followed by high-performance liquid chromatography fluorometric and graphite furnace atomic absorption spectrometric determination. On the basis of the π-π interaction with PAHs and the chelating interaction with Cu(2+), the simultaneous extraction of PAHs and Cu(2+) and stepwise elution through tuning the eluent were successfully achieved, respectively. The SPE conditions affecting the extraction efficiency were optimized, including type and concentration of organic modifier, sample solution pH, flow rate, and volume. As a result of the special adsorption and desorption mechanism, high extraction efficiency was achieved with relative recoveries of 94.3-102.4% and relative standard deviations of less than 10.5%. The limits of detection were obtained with 0.4-3.1 ng L(-1) for PAHs and 15 ng L(-1) for Cu(2+), respectively. The method was applied to the analyses of PAHs and Cu(2+) in Xiliu Lake water samples collected in Zhengzhou, China.

  14. Efficient graphite ring heater suitable for diamond-anvil cells to 1300 K

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

    Du Zhixue; Amulele, George; Lee, Kanani K. M.

    In order to generate homogeneous high temperatures at high pressures, a ring-shaped graphite heater has been developed to resistively heat diamond-anvil cell (DAC) samples up to 1300 K. By putting the heater in direct contact with the diamond anvils, this graphite heater design features the following advantages: (1) efficient heating: sample can be heated to 1300 K while the DAC body temperature remains less than 800 K, eliminating the requirement of a special alloy for the DAC; (2) compact design: the sample can be analyzed with in situ measurements, e.g., x-ray, optical, and electrical probes are possible. In particular, themore » side access of the heater allows for radial x-ray diffraction (XRD) measurements in addition to traditional axial XRD.« less

  15. Calibrated work function mapping by Kelvin probe force microscopy

    NASA Astrophysics Data System (ADS)

    Fernández Garrillo, Pablo A.; Grévin, Benjamin; Chevalier, Nicolas; Borowik, Łukasz

    2018-04-01

    We propose and demonstrate the implementation of an alternative work function tip calibration procedure for Kelvin probe force microscopy under ultrahigh vacuum, using monocrystalline metallic materials with known crystallographic orientation as reference samples, instead of the often used highly oriented pyrolytic graphite calibration sample. The implementation of this protocol allows the acquisition of absolute and reproducible work function values, with an improved uncertainty with respect to unprepared highly oriented pyrolytic graphite-based protocols. The developed protocol allows the local investigation of absolute work function values over nanostructured samples and can be implemented in electronic structures and devices characterization as demonstrated over a nanostructured semiconductor sample presenting Al0.7Ga0.3As and GaAs layers with variable thickness. Additionally, using our protocol we find that the work function of annealed highly oriented pyrolytic graphite is equal to 4.6 ± 0.03 eV.

  16. On plate graphite supported sample processing for simultaneous lipid and protein identification by matrix assisted laser desorption ionization mass spectrometry.

    PubMed

    Calvano, Cosima Damiana; van der Werf, Inez Dorothé; Sabbatini, Luigia; Palmisano, Francesco

    2015-05-01

    The simultaneous identification of lipids and proteins by matrix assisted laser desorption ionization-mass spectrometry (MALDI-MS) after direct on-plate processing of micro-samples supported on colloidal graphite is demonstrated. Taking advantages of large surface area and thermal conductivity, graphite provided an ideal substrate for on-plate proteolysis and lipid extraction. Indeed proteins could be efficiently digested on-plate within 15 min, providing sequence coverages comparable to those obtained by conventional in-solution overnight digestion. Interestingly, detection of hydrophilic phosphorylated peptides could be easily achieved without any further enrichment step. Furthermore, lipids could be simultaneously extracted/identified without any additional treatment/processing step as demonstrated for model complex samples such as milk and egg. The present approach is simple, efficient, of large applicability and offers great promise for protein and lipid identification in very small samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  17. Rapid prototyping of carbon-based chemiresistive gas sensors on paper

    PubMed Central

    Mirica, Katherine A.; Azzarelli, Joseph M.; Weis, Jonathan G.; Schnorr, Jan M.; Swager, Timothy M.

    2013-01-01

    Chemically functionalized carbon nanotubes (CNTs) are promising materials for sensing of gases and volatile organic compounds. However, the poor solubility of carbon nanotubes hinders their chemical functionalization and the subsequent integration of these materials into devices. This manuscript describes a solvent-free procedure for rapid prototyping of selective chemiresistors from CNTs and graphite on the surface of paper. This procedure enables fabrication of functional gas sensors from commercially available starting materials in less than 15 min. The first step of this procedure involves the generation of solid composites of CNTs or graphite with small molecule selectors—designed to interact with specific classes of gaseous analytes—by solvent-free mechanical mixing in a ball mill and subsequent compression. The second step involves deposition of chemiresistive sensors by mechanical abrasion of these solid composites onto the surface of paper. Parallel fabrication of multiple chemiresistors from diverse composites rapidly generates cross-reactive arrays capable of sensing and differentiating gases and volatile organic compounds at part-per-million and part-per-thousand concentrations. PMID:23942132

  18. High-temperature friction and wear studies of Fe-Cu-Sn alloy with graphite as solid lubricant under dry sliding conditions

    NASA Astrophysics Data System (ADS)

    Mushtaq, Shuhaib; Wani, M. F.

    2018-02-01

    Solid lubricants are particularly used in the advanced mechanical motion systems with extreme conditions such as (high temperature, vacuum, radiation, extreme contact pressure, etc). The main focus of this paper is to study the dry sliding friction and wear behavior of Fe-Cu-Sn alloy with varying wt% of graphite at high temperature up to 423 K. The influence of temperature, sliding distance and load on friction and wear behavior of Fe-Cu-Sn alloy against EN8 steel was studied using ball (EN8) on disc (Fe-Cu-Sn alloy). Lower wear and lower friction of Fe-Cu-Sn alloy were observed at high temperature, as compared to room temperature. Surface morphological and surface analytical studies of fresh and worn surfaces were carried out using optical microscopy, 3D profilometer, scanning electron microscope, energy dispersive x-ray spectroscopy, XRD, and Raman spectroscopy to understand the friction and wear behavior.

  19. Controlling Self-Assembly of Engineered Peptides on Graphite by Rational Mutation

    PubMed Central

    So, Christopher R.; Hayamizu, Yuhei; Yazici, Hilal; Gresswell, Carolyn; Khatayevich, Dmitriy; Tamerler, Candan; Sarikaya, Mehmet

    2012-01-01

    Self-assembly of proteins on surfaces is utilized in many fields to integrate intricate biological structures and diverse functions with engineered materials. Controlling proteins at bio-solid interfaces relies on establishing key correlations between their primary sequences and resulting spatial organizations on substrates. Protein self-assembly, however, remains an engineering challenge. As a novel approach, we demonstrate here that short dodecapeptides selected by phage display are capable of self-assembly on graphite and form long-range ordered biomolecular nanostructures. Using atomic force microscopy and contact angle studies, we identify three amino-acid domains along the primary sequence that steer peptide ordering and lead to nanostructures with uniformly displayed residues. The peptides are further engineered via simple mutations to control fundamental interfacial processes, including initial binding, surface aggregation and growth kinetics, and intermolecular interactions. Tailoring short peptides via their primary sequence offers versatile control over molecular self-assembly, resulting in well-defined surface properties essential in building engineered, chemically rich, bio-solid interfaces. PMID:22233341

  20. Proposal of simple and novel method of capacity fading analysis using pseudo-reference electrode in lithium ion cells: Application to solvent-free lithium ion polymer batteries

    NASA Astrophysics Data System (ADS)

    Shono, Kumi; Kobayashi, Takeshi; Tabuchi, Masato; Ohno, Yasutaka; Miyashiro, Hajime; Kobayashi, Yo

    2014-02-01

    We propose a simple procedure for introducing a pseudo-reference electrode (PRE) to lithium ion batteries using isometric lithium metal placed between the cathode and anode, and we successfully obtained the cathode and anode voltage profiles, individual interfacial impedances, and the misalignment of the operation range between the cathode and anode after cycle operation. The proposed procedure is applicable to lithium ion battery systems using a solid electrolyte to prepare two cells with a lithium counter electrode. We determined the capacity decrease of a solvent-free lithium ion polymer battery consisting of a LiNi1/3Mn1/3Co1/3O2 (NMC), a polyether-based solid polymer electrolyte (SPE), and a graphite (Gr) with the proposed PRE over 1000 cycles. The capacity retention of the [Gr|SPE|NMC] cell reached 50% at the 1000th cycle upon the optimization of cell preparation, and we found that the main factor of the capacity decrease was the continuous irreversible loss of active lithium at the graphite anode, not the oxidation of the SPE. Our findings suggest that we should reconsider combining a polyether-based SPE with a conventionally used 4 V class cathode and a graphite anode to develop an innovative, safe, and low-cost battery for the expected large lithium ion battery systems for stationary use.

  1. Graphitization of Coke and Its Interaction with Slag in the Hearth of a Blast Furnace

    NASA Astrophysics Data System (ADS)

    Li, Kejiang; Zhang, Jianliang; Liu, Yanxiang; Barati, Mansoor; Liu, Zhengjian; Zhong, Jianbo; Su, Buxin; Wei, Mengfang; Wang, Guangwei; Yang, Tianjun

    2016-04-01

    Coke reaction behavior in the blast furnace hearth has yet to be fully understood due to limited access to the high temperature zone. The graphitization of coke and its interaction with slag in the hearth of blast furnace were investigated with samples obtained from the center of the deadman of a blast furnace during its overhaul period. All hearth coke samples from fines to lumps were confirmed to be highly graphitized, and the graphitization of coke in the high temperature zone was convinced to start from the coke surface and lead to the formation of coke fines. It will be essential to perform further comprehensive investigations on graphite formation and its evolution in a coke as well as its multi-effect on blast furnace performance. The porous hearth cokes were found to be filled up with final slag. Further research is required about the capability of coke to fill final slag and the attack of final slag on the hearth bottom refractories since this might be a new degradation mechanism of refractories located in the hearth bottom.

  2. Multiresidue method for the determination of 227 pesticides in hot pepper (Capsicum annuum L.) by liquid chromatography with tandem mass spectrometry.

    PubMed

    Zhu, Yong-Zhe; Zhao, Mei-Ai; Nan Feng, Ya; Han Kim, Jeong

    2014-10-01

    A high-throughput, rapid, and efficient modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method with a simple cleanup procedure has been developed for simultaneously determining 227 pesticides in pepper samples by liquid chromatography with tandem mass spectrometry (running time: 10 min). Pesticide residues were extracted/partitioned with an acetonitrile/DisQuE QuEChERS pouch, and the resulting samples were cleaned up with different methods: dispersive solid-phase extraction with primary secondary amines or multiwalled carbon nanotubes and graphitized carbon solid mini cartridge column. The results indicated that multiwalled carbon nanotubes dispersive sorbents achieved the best recoveries and had less matrix interference. The numbers of pesticides with a recovery in the range of 70-120% were 199 at a spiked level of 40 μg/kg. The correlation coefficients (r(2)) for 227 pesticides were above 0.99, while the limits of quantitation of pesticides in pepper samples ranged from 0.13 to 13.51 μg/kg (S/N = 10), and the limits of detection ranged from 0.04 to 4.05 μg/kg (S/N = 3). The relative standard deviations of approximately 197 pesticides were below 20% at spiked levels of 40 μg/kg. Based on these results, the proposed method was chosen as the most suitable cleanup procedure for the determination of multiresidue pesticides in pepper samples. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Application of Chitosan-Zinc Oxide Nanoparticles for Lead Extraction From Water Samples by Combining Ant Colony Optimization with Artificial Neural Network

    NASA Astrophysics Data System (ADS)

    Khajeh, M.; Pourkarami, A.; Arefnejad, E.; Bohlooli, M.; Khatibi, A.; Ghaffari-Moghaddam, M.; Zareian-Jahromi, S.

    2017-09-01

    Chitosan-zinc oxide nanoparticles (CZPs) were developed for solid-phase extraction. Combined artificial neural network-ant colony optimization (ANN-ACO) was used for the simultaneous preconcentration and determination of lead (Pb2+) ions in water samples prior to graphite furnace atomic absorption spectrometry (GF AAS). The solution pH, mass of adsorbent CZPs, amount of 1-(2-pyridylazo)-2-naphthol (PAN), which was used as a complexing agent, eluent volume, eluent concentration, and flow rates of sample and eluent were used as input parameters of the ANN model, and the percentage of extracted Pb2+ ions was used as the output variable of the model. A multilayer perception network with a back-propagation learning algorithm was used to fit the experimental data. The optimum conditions were obtained based on the ACO. Under the optimized conditions, the limit of detection for Pb2+ ions was found to be 0.078 μg/L. This procedure was also successfully used to determine the amounts of Pb2+ ions in various natural water samples.

  4. Irradiation Creep in Graphite

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

    Ubic, Rick; Butt, Darryl; Windes, William

    2014-03-13

    An understanding of the underlying mechanisms of irradiation creep in graphite material is required to correctly interpret experimental data, explain micromechanical modeling results, and predict whole-core behavior. This project will focus on experimental microscopic data to demonstrate the mechanism of irradiation creep. High-resolution transmission electron microscopy should be able to image both the dislocations in graphite and the irradiation-induced interstitial clusters that pin those dislocations. The team will first prepare and characterize nanoscale samples of virgin nuclear graphite in a transmission electron microscope. Additional samples will be irradiated to varying degrees at the Advanced Test Reactor (ATR) facility and similarlymore » characterized. Researchers will record microstructures and crystal defects and suggest a mechanism for irradiation creep based on the results. In addition, the purchase of a tensile holder for a transmission electron microscope will allow, for the first time, in situ observation of creep behavior on the microstructure and crystallographic defects.« less

  5. LASER APPLICATIONS AND OTHER TOPICS IN QUANTUM ELECTRONICS: On the possibility of studying the temporal evolution of a surface relief directly during exposure to high-power radiation

    NASA Astrophysics Data System (ADS)

    Abramov, D. V.; Arakelyan, S. M.; Galkin, A. F.; Klimovskii, Ivan I.; Kucherik, A. O.; Prokoshev, V. G.

    2006-06-01

    The video image of the graphite surface exposed to focused laser radiation is obtained with the help of a laser monitor. A bright ring moving over the heated surface was observed. A method for reconstructing the surface relief from the video image is proposed and realised. The method is based on the measurement of the angular distribution of the light intensity scattered by the graphite sample surface. The surface relief of the graphite sample changing in time is reconstructed. The relative change in the relief height during laser excitation is measured. The statistical characteristics of the reconstructed graphite surface shape and their variation during laser irradiation are studied. It is found that a circular convexity appears within the bright ring. The formation mechanism of this convexity requires further investigations.

  6. Development of a Muon Rotating Target for J-PARC/MUSE

    NASA Astrophysics Data System (ADS)

    Makimura, Shunsuke; Kobayashi, Yasuo; Miyake, Yasuhiro; Kawamura, Naritoshi; Strasser, Patrick; Koda, Akihiro; Shimomura, Koichiro; Fujimori, Hiroshi; Nishiyama, Kusuo; Kato, Mineo; Kojima, Kenji; Higemoto, Wataru; Ito, Takashi; Shimizu, Ryou; Kadono, Ryosuke

    At the J-PARC muon science facility (J-PARC/MUSE), a graphite target with a thickness of 20 mm has been used in vacuum to obtain an intense pulsed muon beam from the RCS 3-GeV proton beam [1], [2]. In the current design, the target frame is constructed using copper with a stainless steel tube embedded for water cooling. The energy deposited by the proton beam at 1 MW is evaluated to be 3.3 kW on the graphite target and 600 W on the copper frame by a Monte-Carlo simulation code, PHITS [3]. Graphite materials are known to lose their crystal structure and can be shrunk under intense proton beam irradiation. Consequently, the lifetime of the muon target is essentially determined by the radiation damage in graphite, and is evaluated to be half a year [4]. Hence, we are planning to distribute the radiation damage by rotating a graphite wheel. Although the lifetime of graphite in this case will be more than 10 years, the design of the bearing must be carefully considered. Because the bearing in JPARC/MUSE is utilized in vacuum, under high radiation, and at high temperature, an inorganic and solid lubricant must be applied to the bearing. Simultaneously, the temperature of the bearing must also be decreased to extend the lifetime. In 2009, a mock-up of the Muon Rotating Target, which could heat up and rotate a graphite wheel, was fabricated. Then several tests were started to select the lubricant and to determine the structure of the Muon Rotating Target, the control system and so on. In this report, the present status of the Muon Rotating Target for J-PARC/MUSE, especially the development of a rotation system in vacuum, is described.

  7. Mono- and multilayers of molecular spoked carbazole wheels on graphite

    PubMed Central

    Aggarwal, A Vikas; Kalle, Daniel; Höger, Sigurd

    2014-01-01

    Summary Self-assembled monolayers of a molecular spoked wheel (a shape-persistent macrocycle with an intraannular spoke/hub system) and its synthetic precursor are investigated by scanning tunneling microscopy (STM) at the liquid/solid interface of 1-octanoic acid and highly oriented pyrolytic graphite. The submolecularly resolved STM images reveal that the molecules indeed behave as more or less rigid objects of certain sizes and shapes – depending on their chemical structures. In addition, the images provide insight into the multilayer growth of the molecular spoked wheels (MSWs), where the first adlayer acts as a template for the commensurate adsorption of molecules in the second layer. PMID:25550744

  8. Mono- and multilayers of molecular spoked carbazole wheels on graphite.

    PubMed

    Jester, Stefan-S; Aggarwal, A Vikas; Kalle, Daniel; Höger, Sigurd

    2014-01-01

    Self-assembled monolayers of a molecular spoked wheel (a shape-persistent macrocycle with an intraannular spoke/hub system) and its synthetic precursor are investigated by scanning tunneling microscopy (STM) at the liquid/solid interface of 1-octanoic acid and highly oriented pyrolytic graphite. The submolecularly resolved STM images reveal that the molecules indeed behave as more or less rigid objects of certain sizes and shapes - depending on their chemical structures. In addition, the images provide insight into the multilayer growth of the molecular spoked wheels (MSWs), where the first adlayer acts as a template for the commensurate adsorption of molecules in the second layer.

  9. Investigating the effects of proton exchange membrane fuel cell conditions on carbon supported platinum electrocatalyst composition and performance

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

    Patel, Anant; Artyushkova, Kateryna; Atanassov, Plamen

    2011-12-01

    Changes that carbon-supported platinum electrocatalysts undergo in a proton exchange membrane fuel cell environment were simulated by ex situ heat treatment of catalyst powder samples at 150 C and 100% relative humidity. In order to study modifications that are introduced to chemistry, morphology, and performance of electrocatalysts, XPS, HREELS and three-electrode rotating disk electrode experiments were performed. Before heat treatment, graphitic content varied by 20% among samples with different types of carbon supports, with distinct differences between bulk and surface compositions within each sample. Following the aging protocol, the bulk and surface chemistry of the samples were similar, with graphitemore » content increasing or remaining constant and Pt-carbide decreasing for all samples. From the correlation of changes in chemical composition and losses in performance of the electrocatalysts, we conclude that relative distribution of Pt particles on graphitic and amorphous carbon is as important for electrocatalytic activity as the absolute amount of graphitic carbon present« less

  10. Determination of Pb in Biological Samples by Graphite Furnace Atomic Absorption Spectrophotometry: An Exercise in Common Interferences and Fundamental Practices in Trace Element Determination

    ERIC Educational Resources Information Center

    Spudich, Thomas M.; Herrmann, Jennifer K.; Fietkau, Ronald; Edwards, Grant A.

    2004-01-01

    An experiment is conducted to ascertain trace-level Pb in samples of bovine liver or muscle by applying graphite furnace atomic absorption spectrophotometry (GFAAS). The primary objective is to display the effects of physical and spectral intrusions in determining trace elements, and project the usual methods employed to minimize accuracy errors…

  11. Atomic resolution images of graphite in air

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

    Grigg, D.A.; Shedd, G.M.; Griffis, D.

    One sample used for proof of operation for atomic resolution in STM is highly oriented pyrolytic graphite (HOPG). This sample has been imaged with many different STM`s obtaining similar results. Atomic resolution images of HOPG have now been obtained using an STM designed and built at the Precision Engineering Center. This paper discusses the theoretical predictions and experimental results obtained in imaging of HOPG.

  12. Electrostatic force microscopy on oriented graphite surfaces: coexistence of insulating and conducting behaviors.

    PubMed

    Lu, Yonghua; Muñoz, M; Steplecaru, C S; Hao, Cheng; Bai, Ming; Garcia, N; Schindler, K; Esquinazi, P

    2006-08-18

    We present measurements of the electric potential fluctuations on the surface of highly oriented pyrolytic graphite using electrostatic force and atomic force microscopy. Micrometric domainlike potential distributions are observed even when the sample is grounded. Such potential distributions are unexpected given the good metallic conductivity of graphite because the surface should be an equipotential. Our results indicate the coexistence of regions with "metalliclike" and "insulatinglike" behaviors showing large potential fluctuations of the order of 0.25 V. In lower quality graphite, this effect is not observed. Experiments are performed in Ar and air atmospheres.

  13. Carbide coated fibers in graphite-aluminum composites

    NASA Technical Reports Server (NTRS)

    Imprescia, R. J.; Levinson, L. S.; Reiswig, R. D.; Wallace, T. C.; Williams, J. M.

    1975-01-01

    Thin, uniform coats of titanium carbide, deposited on graphite fibers by chemical vapor deposition with thicknesses up to approximately 0.1 microns were shown to improve fiber strength significantly. For greater thicknesses, strength was degraded. The coats promote wetting of the fibers and infiltration of the fiber yarns with aluminum alloys, and act as protective barriers to inhibit reaction between the fibers and the alloys. Chemical vapor deposition was used to produce silicon carbide coats on graphite fibers. In general, the coats were nonuniform and were characterized by numerous surface irregularities. Despite these irregularities, infiltration of these fibers with aluminum alloys was good. Small graphite-aluminum composite samples were produced by vacuum hot-pressing of aluminum-infiltrated graphite yarn at temperatures above the metal liquidus.

  14. Comparison of the tribological properties of fluorinated cokes and graphites

    NASA Technical Reports Server (NTRS)

    Fusaro, Robert L.

    1988-01-01

    The friction, wear, endurance life, and surface morphology of rubbed (burnished) fluorinated graphite and fluorinated coke materials were studied. Two different coke powders, a graphitic carbon powder, and a graphite powder were fluorinated and then tribologically investigated. In addition, one of the coke powders was reduced in size before fluorinating to evaluate the effect of a finer particle size on the tribological properties. For comparison, graphite and coke powders which were not fluorinated were also tribologically evaluated. Elemental analysis by emission spectroscopy was performed on each sample to determine the impurity content and X-ray diffraction analysis was performed to determine the crystallinity. Coke was found to have very little lubricating ability, but fluorinated coke did possess good lubricating properties. However, the fluorinated graphite and fluorinated graphitic carbon (which gave equivalent results) gave superior results to those obtained with the fluorinated cokes. No tribological benefit was found for using small versus a larger particle size of coke, at least when evaluated as a rubbed film.

  15. Comparison of the tribological properties of fluorinated cokes and graphites

    NASA Technical Reports Server (NTRS)

    Fusaro, Robert L.

    1987-01-01

    The friction, wear, endurance life, and surface morphology of rubbed (burnished) fluorinated graphite and fluorinated coke materials were studied. Two different coke powders, a graphitic carbon powder, and a graphite powder were fluorinated and then tribologically investigated. In addition, one of the coke powders was reduced in size before fluorinating to evaluate the effect of a finer particle size on the tribological properties. For comparison, graphite and coke powders which were not fluorinated were also tribologically evaluated. Elemental analysis by emission spectroscopy was performed on each sample to determine the impurity content and X-ray diffraction analysis was performed to determine the crystallinity. Coke was found to have very little lubricating ability, but fluorinated coke did possess good lubricating properties. However, the fluorinated graphite and fluorinated graphitic carbon (which gave equivalent results) gave superior results to those obtained with the fluorinated cokes. No tribological benefit was found for using small versus a larger particle size of coke, at least when evaluated as a rubbed film.

  16. Effect of High Energy Radiation on Mechanical Properties of Graphite Fiber Reinforced Composites. M.S. Thesis

    NASA Technical Reports Server (NTRS)

    Naranong, N.

    1980-01-01

    The flexural strength and average modulus of graphite fiber reinforced composites were tested before and after exposure to 0.5 Mev electron radiation and 1.33 Mev gamma radiation by using a three point bending test (ASTM D-790). The irradiation was conducted on vacuum treated samples. Graphite fiber/epoxy (T300/5208), graphite fiber/polyimide (C6000/PMR 15) and graphite fiber/polysulfone (C6000/P1700) composites after being irradiated with 0.5 Mev electron radiation in vacuum up to 5000 Mrad, show increases in stress and modulus of approximately 12% compared with the controls. Graphite fiber/epoxy (T300/5208 and AS/3501-6), after being irradiated with 1.33 Mev gamma radiation up to 360 Mrads, show increases in stress and modulus of approximately 6% at 167 Mrad compared with the controls. Results suggest that the graphite fiber composites studied should withstand the high energy radiation in a space environment for a considerable time, e.g., over 30 years.

  17. Inertial impaction air sampling device

    DOEpatents

    Dewhurst, Katharine H.

    1990-01-01

    An inertial impactor to be used in an air sampling device for collection of respirable size particles in ambient air which may include a graphite furnace as the impaction substrate in a small-size, portable, direct analysis structure that gives immediate results and is totally self-contained allowing for remote and/or personal sampling. The graphite furnace collects suspended particles transported through the housing by means of the air flow system, and these particles may be analyzed for elements, quantitatively and qualitatively, by atomic absorption spectrophotometry.

  18. Inertial impaction air sampling device

    DOEpatents

    Dewhurst, K.H.

    1987-12-10

    An inertial impactor to be used in an air sampling device for collection of respirable size particles in ambient air which may include a graphite furnace as the impaction substrate in a small-size, portable, direct analysis structure that gives immediate results and is totally self-contained allowing for remote and/or personal sampling. The graphite furnace collects suspended particles transported through the housing by means of the air flow system, and these particles may be analyzed for elements, quantitatively and qualitatively, by atomic absorption spectrophotometry. 3 figs.

  19. Increasing the wear resistance of ultra-high molecular weight polyethylene by adding solid lubricating fillers

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

    Panin, S. V., E-mail: svp@ispms.tsc.ru; Kornienko, L. A.; Poltaranin, M. A.

    2014-11-14

    In order to compare effectiveness of adding solid lubricating fillers for polymeric composites based on ultra-high molecular weight polyethylene (UHMWPE) with graphite, molybdenum disulfide and polytetrafluoroethylene, their tribotechnical characteristics under dry friction, boundary lubrication and abrasive wearing were investigated. The optimal weight fractions of fillers in terms of improving wear resistance have been determined. The supramolecular structure and topography of wear track surfaces of UHMWPE-based composites with different content of fillers have been studied.

  20. Comparison of several solid-phase extraction sorbents for continuous determination of amines in water by gas chromatography-mass spectrometry.

    PubMed

    Jurado-Sánchez, Beatriz; Ballesteros, Evaristo; Gallego, Mercedes

    2009-08-15

    A semiautomatic method has been proposed for the determination of different types of amines in water samples including anilines, chloroanilines, N-nitrosamines and aliphatic amines. The analytes were retained on a solid-phase extraction sorbent column and after elution, 1 microL of the extract was analysed by gas chromatography coupled with electron impact ionization mass spectrometry. A systematic overview is given of the advantages and disadvantages of several sorbents (LiChrolut EN, Oasis HLB, RP-C(18), graphitized carbon black, fullerenes and nanotubes) in the retention of amine compounds and based on sensitivity, selectivity and reliability. The retention efficiency for the studied amines was higher (ca. 100%) with LiChrolut EN and Oasis HLB than it was with RP-C(18) and fullerenes (53 and 62%, respectively, on average). Detection limits of 0.5-16 ng L(-1) for the 27 amines studied were obtained when using a sorbent column containing 75 mg of LiChrolut EN for 100mL of sample, the RSD being lower than 6.5%. The method was applied with good accuracy and precision in the determination of amines in various types of water including river, pond, tap, well, drinking, swimming pool and waste.

  1. Nanodiamond infiltration into porous silicon through etching of solid carbon produced at different graphitization temperatures

    NASA Astrophysics Data System (ADS)

    Miranda, C. R. B.; Baldan, M. R.; Beloto, A. F.; Ferreira, N. G.

    2011-09-01

    Nanocrystalline diamond (NCD) was grown on the porous silicon (PS) substrate using Reticulated Vitreous Carbon (RVC) as an additional solid carbon source. RVC was produced at different heat treatment temperatures of 1300, 1500, and 2000 °C, resulting in samples with different turbostratic carbon organizations. The PS substrate was produced by an electrochemical method. NCD film was obtained by the chemical vapor infiltration/deposition process where a RVC piece was positioned just below the PS substrate. The PS and NCD samples were characterized by Field Emission Gun-Scanning Electron Microscopy (FEG-SEM). NCD films presented faceted nanograins with uniform surface texture covering all the pores resulting in an apparent micro honeycomb structure. Raman's spectra showed the D and G bands, as well as, the typical two shoulders at 1,150 and 1,490 cm-1 attributed to NCD. X-ray diffraction analyses showed the predominant (111) diamond orientation as well as the (220) and (311) peaks. The structural organization and the heteroatom presence on the RVC surface, analyzed from X-ray photoelectron spectroscopy, showed their significant influence on the NCD growth process. The hydrogen etching released, from RVC surface, associated to carbon and/or oxygen/nitrogen amounts led to different contributions for NCD growth.

  2. A direct solid sampling analysis method for the detection of silver nanoparticles in biological matrices.

    PubMed

    Feichtmeier, Nadine S; Ruchter, Nadine; Zimmermann, Sonja; Sures, Bernd; Leopold, Kerstin

    2016-01-01

    Engineered silver nanoparticles (AgNPs) are implemented in food contact materials due to their powerful antimicrobial properties and so may enter the human food chain. Hence, it is desirable to develop easy, sensitive and fast analytical screening methods for the determination of AgNPs in complex biological matrices. This study describes such a method using solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry (GFAAS). A recently reported novel evaluation strategy uses the atomization delay of the respective GFAAS signal as significant indicator for AgNPs and thereby allows discrimination of AgNPs from ionic silver (Ag(+)) in the samples without elaborate sample pre-treatment. This approach was further developed and applied to a variety of biological samples. Its suitability was approved by investigation of eight different food samples (parsley, apple, pepper, cheese, onion, pasta, maize meal and wheat flour) spiked with ionic silver or AgNPs. Furthermore, the migration of AgNPs from silver-impregnated polypropylene food storage boxes to fresh pepper was observed and a mussel sample obtained from a laboratory exposure study with silver was investigated. The differences in the atomization delays (Δt(ad)) between silver ions and 20-nm AgNPs vary in a range from -2.01 ± 1.38 s for maize meal to +2.06 ± 1.08 s for mussel tissue. However, the differences were significant in all investigated matrices and so indicative of the presence/absence of AgNPs. Moreover, investigation of model matrices (cellulose, gelatine and water) gives the first indication of matrix-dependent trends. Reproducibility and homogeneity tests confirm the applicability of the method.

  3. Thermal expansion behavior of LDEF metal matrix composites

    NASA Technical Reports Server (NTRS)

    Le, T. D.; Steckel, G. L.

    1992-01-01

    The effects of the space environment on the thermal expansion stability of metal matrix composites (graphite/Al and graphite/Mg) will be presented. A sample from each category of metal matrix composites mounted on the leading and trailing edge was chosen for analysis of the temperature-time-thermal strain histories. Typical thermal expansion curves over the same range of temperature were selected at the beginning, mid, and end of the recording duration. The thermal expansion of selected post-flight LDEF samples were measured over the same range of temperature in the laboratory using a Michelson laser interferometer. The thermal strains were monitored concurrently with a laser interferometer and a mounted strain gage.

  4. Chemical Characterization and Removal of Carbon-14 from Irradiated Graphite II - 13023

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

    Dunzik-Gougar, Mary Lou; Cleaver, James; LaBrier, Daniel

    2013-07-01

    Approximately 250,000 tonnes of irradiated graphite waste exists worldwide and that quantity is expected to increase with decommissioning of Generation II reactors and deployment of Generation IV gas-cooled, graphite moderated reactors. This situation indicates the need for a graphite waste management strategy. Of greatest concern for long-term disposal of irradiated graphite is carbon-14 (C-14), with a half-life of 5730 years. Study of irradiated graphite from some nuclear reactors indicates C-14 is concentrated on the outer 5 mm of the graphite structure. The aim of the research presented last year and updated here is to identify the chemical form of C-14more » in irradiated graphite and develop a practical method by which C-14 can be removed. A nuclear-grade graphite, NBG-18, and a high-surface-area graphite foam, POCOFoam{sup R}, were exposed to liquid nitrogen (to increase the quantity of C-14 precursor) and neutron-irradiated (10{sup 13} neutrons/cm{sup 2}/s). Finer grained NBG-25 was not exposed to liquid nitrogen prior to irradiation at a neutron flux on the order of 10{sup 14} /cm{sup 2}/s. Characterization of pre- and post-irradiation graphite was conducted to determine the chemical environment and quantity of C-14 and its precursors via the use of surface sensitive characterization techniques. Scanning Electron Microscopy (SEM) was used to evaluate the morphological features of graphite samples. The concentration, chemical composition, and bonding characteristics of C-14 and its precursors were determined through X-ray Photoelectron Spectroscopy (XPS), Time-of-Flight Secondary Ion Mass Spectrometry (SIMS), and Energy Dispersive X-ray Analysis Spectroscopy (EDX). Results of post-irradiation characterization of these materials indicate a variety of surface functional groups containing carbon, oxygen, nitrogen and hydrogen. During thermal treatment, irradiated graphite samples are heated in the presence of an inert carrier gas (with or without oxidant gas), which carries off gaseous products released during treatment. Graphite gasification occurs via interaction with adsorbed oxygen complexes. Experiments in argon were performed at 900 deg. C and 1400 deg. C to evaluate the selective removal of C-14. Thermal treatment also was performed with the addition of 3 and 5 volume % oxygen at temperatures 700 deg. C and 1400 deg. C. Thermal treatment experiments were evaluated for the effective selective removal of C-14. Lower temperatures and oxygen levels correlated to more efficient C-14 removal. (authors)« less

  5. Influence of graphite and serpentine minerals along landslide failure surfaces

    NASA Astrophysics Data System (ADS)

    Alberti, Stefano; Battista Crosta, Giovanni; Wang, Gonghui; Dattola, Giuseppe; Bertolo, Davide

    2017-04-01

    Landslides and deep-seated gravitational slope deformation (DSGSD) often are concentrated in sedimentary and metasedimentary rocks (e.g. Ambrosi and Crosta, 2006) and in carbonaceous materials (CM), where weaker slip surfaces can be generated more easily, with a behaviour similar to that of fault zone (e.g. Zulauf et al., 1990; Craw, 2002; Oohashi et al., 2011, Nakamura et al., 2015). Among the carbonaceous minerals, graphite (grouped with other silicate sheet minerals) acts as a "solid lubrificant" and plays a key role on frictional properties of the slip surface (Yamasaki et al., 2015). These minerals have one key characteristic in common: the presence of weak bonding along (001) planes. Graphite also has one of the weakest bonding in the crystal structure, and it is characterized by a markedly low coefficient of friction (ca 0.1). A similar behaviour is found in serpentine minerals series and chlorite. We performed these tests on different samples derived from Mont de La Saxe landslide and Chervaz landslide. The first one is located in the upper Aosta Valley, the second in the central part of the Aosta Valley. Both these landslides are characterized by metasedimentary sequences. The undisturbed samples derived by core recovery surveys. We performed a petrographic characterization by XRD (X-Ray Diffraction), XRF (X-Ray Refraction) and SEM (Scansion Electron Microscope) with microprobe in addition to laboratory tests on samples from shear zones. Along these shear zones grains are crushed, their size and shapes are changed and these changes necessarily affect pore-water pressure due to volume change in the shear zone. We performed tests using a dynamic-loading ring-shear apparatus (DPRI-5, Sassa et al., 1997). This apparatus allows to simulate the entire process of failure, from initial static or dynamic loading, through shear failure, pore-pressure changes and possible liquefaction, to large-displacement, steady-state shear movement. It is also possible to simulate the formation of the shear zone and the post-failure mobility of high-speed landslides, monitoring pore-pressure generation, and mobilized shear resistance together with shear displacement. Reference List: Ambrosi, C., & Crosta, G. B. (2006). Large sackung along major tectonic features in the Central Italian Alps. Engineering Geology, 83(1), 183-200. Craw, D. (2002). Geochemistry of late metamorphic hydrothermal alteration and graphitisation of host rock, Macraes gold mine, Otago Schist, New Zealand. Chemical Geology, 191(4), 257-275. Nakamura, Y., Oohashi, K., Toyoshima, T., Satish-Kumar, M., & Akai, J. (2015). Strain-induced amorphization of graphite in fault zones of the Hidaka metamorphic belt, Hokkaido, Japan. Journal of Structural Geology, 72, 142-161. Sassa K, Fukuoka H, Wang FW (1997) Mechanism and risk assessment of landslide- triggered-debris flows: lesson from the 1996.12.6 Otari debris flow disaster, Nagano, Japan. In: Cruden DM, Fell R (eds) Landslide risk assessment, proceedings of the international workshop on landslide risk assessment. Honolulu, 19-21 February, pp 347-356 Zulauf, G., Kleinschmidt, G., & Oncken, O. (1990). Brittle deformation and graphitic cataclasites in the pilot research well KTB-VB (Oberpfalz, FRG). Geological Society, London, Special Publications, 54(1), 97-103. Yamasaki, S., Chigira, M., & Petley, D. N. (2016). The role of graphite layers in gravitational deformation of pelitic schist. Engineering Geology, 208, 29-38.

  6. Dose measurement in heterogeneous phantoms with an extrapolation chamber

    NASA Astrophysics Data System (ADS)

    Deblois, Francois

    A hybrid phantom-embedded extrapolation chamber (PEEC) made of Solid Water(TM) and bone-equivalent material was used for determining absolute dose in a bone-equivalent phantom irradiated with clinical radiation beams (cobalt-60 gamma rays; 6 and 18 MV x-rays; and 9 and 15 MeV electrons). The dose was determined with the Spencer-Attix cavity theory, using ionization gradient measurements and an indirect determination of the chamber air-mass through measurements of chamber capacitance. The air gaps used were between 2 and 3 mm and the sensitive air volume of the extrapolation chamber was remotely controlled through the motion of the motorized piston with a precision of +/-0.0025 mm. The collected charge was corrected for ionic recombination and diffusion in the chamber air volume following the standard two-voltage technique. Due to the hybrid chamber design, correction factors accounting for scatter deficit and electrode composition were determined and applied in the dose equation to obtain dose data for the equivalent homogeneous bone phantom. Correction factors for graphite electrodes were calculated with Monte Carlo techniques and the calculated results were verified through relative air cavity dose measurements for three different polarizing electrode materials: graphite, steel, and brass in conjunction with a graphite collecting electrode. Scatter deficit, due mainly to loss of lateral scatter in the hybrid chamber, reduces the dose to the air cavity in the hybrid PEEC in comparison with full bone PEEC from 0.7 to ˜2% depending on beam quality and energy. In megavoltage photon and electron beams, graphite electrodes do not affect the dose measurement in the Solid Water(TM) PEEC but decrease the cavity dose by up to 5% in the bone-equivalent PEEC even for very thin graphite electrodes (<0.0025 cm). The collecting electrode material in comparison with the polarizing electrode material has a larger effect on the electrode correction factor; the thickness of thin electrodes, on the other hand, has a negligible effect on dose determination. The uncalibrated hybrid PEEC is an accurate and absolute device for measuring the dose directly in bone material in conjunction with appropriate correction factors determined with Monte Carlo techniques.

  7. A new carbon-based magnetic material for the dispersive solid-phase extraction of UV filters from water samples before liquid chromatography-tandem mass spectrometry analysis.

    PubMed

    Piovesana, Susy; Capriotti, Anna Laura; Cavaliere, Chiara; La Barbera, Giorgia; Samperi, Roberto; Zenezini Chiozzi, Riccardo; Laganà, Aldo

    2017-07-01

    Magnetic solid-phase extraction is one of the most promising new extraction methods for liquid samples before ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis. Several types of materials, including carbonaceous ones, have been prepared for this purpose. In this paper, for the first time, the preparation, characterization, and sorption capability of Fe 3 O 4 -graphitized carbon black (mGCB) composite toward some compounds of environmental interest were investigated. The synthesized mGCB consisted of micrometric GCB particles with 55 m 2  g -1 surface area bearing some carbonyl and hydroxyl functionalities and the surface partially decorated by Fe 3 O 4 microparticles. The prepared mGCB was firstly tested as an adsorbent for the extraction from surface water of 50 pollutants, including estrogens, perfluoroalkyl compounds, UV filters, and quinolones. The material showed good affinity to many of the tested compounds, except carboxylates and glucoronates; however, some compounds were difficult to desorb. Ten UV filters belonging to the chemical classes of benzophenones and p-aminobenzoates were selected, and parameters were optimized for the extraction of these compounds from surface water before UHPLC-MS/MS determination. Then, the method was validated in terms of linearity, trueness, intra-laboratory precision, and detection and quantification limits. In summary, the method performance (trueness, expressed as analytical recovery, 85-114%; RSD 5-15%) appears suitable for the determination of the selected compounds at the level of 10-100 ng L -1 , with detection limits in the range of 1-5 ng L -1 . Finally, the new method was compared with a published one, based on conventional solid-phase extraction with GCB, showing similar performance in real sample analysis. Graphical Abstract Workflow of the analytical method based on magnetic solid-phase extraction followed by LC-MS/MS determination.

  8. Braze Development of Graphite Fiber for Use in Phase Change Material Heat Sinks

    NASA Technical Reports Server (NTRS)

    Quinn, Gregory; Beringer, Woody; Gleason, Brian; Stephan, Ryan

    2011-01-01

    Hamilton Sundstrand (HS), together with NASA Johnson Space Center, developed methods to metallurgically join graphite fiber to aluminum. The goal of the effort was to demonstrate improved thermal conductance, tensile strength and manufacturability compared to existing epoxy bonded techniques. These improvements have the potential to increase the performance and robustness of phase change material heat sinks that use graphite fibers as an interstitial material. Initial work focused on evaluating joining techniques from four suppliers, each consisting of a metallization step followed by brazing or soldering of one inch square blocks of Fibercore graphite fiber material to aluminum end sheets. Results matched the strength and thermal conductance of the epoxy bonded control samples, so two suppliers were down-selected for a second round of braze development. The second round of braze samples had up to a 300% increase in strength and up to a 132% increase in thermal conductance over the bonded samples. However, scalability and repeatability proved to be significant hurdles with the metallization approach. An alternative approach was pursued which used a nickel braze allow to prepare the carbon fibers for joining with aluminum. Initial results on sample blocks indicate that this approach should be repeatable and scalable with good strength and thermal conductance when compared with epoxy bonding.

  9. Diamonds in detonation soot

    NASA Technical Reports Server (NTRS)

    Greiner, N. Roy; Phillips, Dave; Johnson, J. D.; Volk, Fred

    1990-01-01

    Diamonds 4 to 7 nm in diameter have been identified and partially isolated from soot formed in detonations of carbon-forming composite explosives. The morphology of the soot has been examined by transmission electron microscopy (TEM), and the identity of the diamond has been established by the electron diffraction pattern of the TEM samples and by the X-ray diffraction (XRD) pattern of the isolated solid. Graphite is also present in the form of ribbons of turbostatic structure with a thickness of 2 to 4 nm. A fraction, about 25 percent of the soot by weight, was recovered from the crude soot after oxidation of the graphite with fuming perchloric acid. This fraction showed a distinct XRD pattern of diamond and the diffuse band of amorphous carbon. The IR spectrum of these diamonds closely matches that of diamonds recovered from meteorites (Lewis et al., 1987), perhaps indicating similar surface properties after the oxidation. If these diamonds are produced in the detonation itself or during the initial expansion, they exhibit a phenomenal crystal growth rate (5 nm/0.00001 s equal 1.8 m/hr) in a medium with a very low hydrogen/carbon ratio. Because the diamonds will be carried along with the expanding gases, they will be accelerated to velocities approaching 8 km/s.

  10. 49 CFR 173.453 - Fissile materials-exceptions.

    Code of Federal Regulations, 2014 CFR

    2014-10-01

    ... noted. (a) An individual package containing 2 grams or less of fissile material. (b) An individual or bulk packaging containing 15 grams or less of fissile material provided the package has at least 200 grams of solid nonfissile material for every gram of fissile material. Lead, beryllium, graphite, and...

  11. 49 CFR 173.453 - Fissile materials-exceptions.

    Code of Federal Regulations, 2010 CFR

    2010-10-01

    ... noted. (a) An individual package containing 2 grams or less of fissile material. (b) An individual or bulk packaging containing 15 grams or less of fissile material provided the package has at least 200 grams of solid nonfissile material for every gram of fissile material. Lead, beryllium, graphite, and...

  12. 49 CFR 173.453 - Fissile materials-exceptions.

    Code of Federal Regulations, 2012 CFR

    2012-10-01

    ... noted. (a) An individual package containing 2 grams or less of fissile material. (b) An individual or bulk packaging containing 15 grams or less of fissile material provided the package has at least 200 grams of solid nonfissile material for every gram of fissile material. Lead, beryllium, graphite, and...

  13. 49 CFR 173.453 - Fissile materials-exceptions.

    Code of Federal Regulations, 2013 CFR

    2013-10-01

    ... noted. (a) An individual package containing 2 grams or less of fissile material. (b) An individual or bulk packaging containing 15 grams or less of fissile material provided the package has at least 200 grams of solid nonfissile material for every gram of fissile material. Lead, beryllium, graphite, and...

  14. 49 CFR 173.453 - Fissile materials-exceptions.

    Code of Federal Regulations, 2011 CFR

    2011-10-01

    ... noted. (a) An individual package containing 2 grams or less of fissile material. (b) An individual or bulk packaging containing 15 grams or less of fissile material provided the package has at least 200 grams of solid nonfissile material for every gram of fissile material. Lead, beryllium, graphite, and...

  15. The Treatment of PPCP-Containing Sewage in an Anoxic/Aerobic Reactor Coupled with a Novel Design of Solid Plain Graphite-Plates Microbial Fuel Cell

    PubMed Central

    Chang, Yi-Tang; Yang, Chu-Wen; Chang, Yu-Jie; Chang, Ting-Chieh; Wei, Da-Jiun

    2014-01-01

    Synthetic sewage containing high concentrations of pharmaceuticals and personal care products (PPCPs, mg/L level) was treated using an anoxic/aerobic (A/O) reactor coupled with a microbial fuel cell (MFC) at hydraulic retention time (HRT) of 8 h. A novel design of solid plain graphite plates (SPGRPs) was used for the high surface area biodegradation of the PPCP-containing sewage and for the generation of electricity. The average CODCr and total nitrogen removal efficiencies achieved were 97.20% and 83.75%, respectively. High removal efficiencies of pharmaceuticals, including acetaminophen, ibuprofen, and sulfamethoxazole, were also obtained and ranged from 98.21% to 99.89%. A maximum power density of 532.61 mW/cm2 and a maximum coulombic efficiency of 25.20% were measured for the SPGRP MFC at the anode. Distinct differences in the bacterial community were presented at various locations including the mixed liquor suspended solids and biofilms. The bacterial groups involved in PPCP biodegradation were identified as Dechloromonas spp., Sphingomonas sp., and Pseudomonas aeruginosa. This design, which couples an A/O reactor with a novel design of SPGRP MFC, allows the simultaneous removal of PPCPs and successful electricity production. PMID:25197659

  16. INSTRUMENTS AND METHODS OF INVESTIGATION: Experimental investigation of the thermal properties of carbon at high temperatures and moderate pressures

    NASA Astrophysics Data System (ADS)

    Asinovskii, Erik I.; Kirillin, Alexander V.; Kostanovskii, Alexander V.

    2002-08-01

    A consistent procedure for plotting the carbon melting and boiling coexistence curves based on published data and the authors' experimental results is proposed. The parameters of a triple point are predicted to differ markedly from the currently accepted values: pt approx1 bar and Tt approx 4000 K. Two types of experimental facilities were used, with laser heating of samples in one and direct ohmic heating in the other. The existence of a carbyne region (a stable linear polymer consisting of carbon atoms) in the carbon phase diagram is discussed. Results on the direct solid-phase graphite - carbyne transition are presented, and this is shown to occur under certain conditions in the form of a thermal explosion.

  17. Tip-induced local strain on Mo S 2 / graphite detected by inelastic electron tunneling spectroscopy

    DOE PAGES

    Ko, Wonhee; Hus, Saban M.; Li, Xufan; ...

    2018-03-02

    We report the detection of tip-induced local strain applied to the monolayer MoS 2 grown on a graphite substrate by scanning tunneling microscope. Monolayer MoS 2 behaves as both mechanical and tunneling barriers that prevent the tip from contacting the graphite while maintaining the tunneling current. Inelastic tunneling electron spectroscopy (IETS) is utilized to probe the phonon modes in graphite. As the tip pushes the sample, IETS reveals a continuous phonon softening in graphite, corroborated by a downward shift of the phonon energy as calculated by density-functional theory. Finally, our results demonstrate a way to apply local mechanical strain andmore » simultaneously detect the induced change in phonon modes by unitizing IETS with two-dimensional materials as a tunneling barrier.« less

  18. Tip-induced local strain on Mo S 2 / graphite detected by inelastic electron tunneling spectroscopy

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

    Ko, Wonhee; Hus, Saban M.; Li, Xufan

    We report the detection of tip-induced local strain applied to the monolayer MoS 2 grown on a graphite substrate by scanning tunneling microscope. Monolayer MoS 2 behaves as both mechanical and tunneling barriers that prevent the tip from contacting the graphite while maintaining the tunneling current. Inelastic tunneling electron spectroscopy (IETS) is utilized to probe the phonon modes in graphite. As the tip pushes the sample, IETS reveals a continuous phonon softening in graphite, corroborated by a downward shift of the phonon energy as calculated by density-functional theory. Finally, our results demonstrate a way to apply local mechanical strain andmore » simultaneously detect the induced change in phonon modes by unitizing IETS with two-dimensional materials as a tunneling barrier.« less

  19. Tip-induced local strain on Mo S2/graphite detected by inelastic electron tunneling spectroscopy

    NASA Astrophysics Data System (ADS)

    Ko, Wonhee; Hus, Saban M.; Li, Xufan; Berlijn, Tom; Nguyen, Giang D.; Xiao, Kai; Li, An-Ping

    2018-03-01

    We report the detection of tip-induced local strain applied to the monolayer Mo S2 grown on a graphite substrate by scanning tunneling microscope. Monolayer Mo S2 behaves as both mechanical and tunneling barriers that prevent the tip from contacting the graphite while maintaining the tunneling current. Inelastic tunneling electron spectroscopy (IETS) is utilized to probe the phonon modes in graphite. As the tip pushes the sample, IETS reveals a continuous phonon softening in graphite, corroborated by a downward shift of the phonon energy as calculated by density-functional theory. Our results demonstrate a way to apply local mechanical strain and simultaneously detect the induced change in phonon modes by unitizing IETS with two-dimensional materials as a tunneling barrier.

  20. Quantitative Analysis of Heavy Metals in Water Based on LIBS with an Automatic Device for Sample Preparation

    NASA Astrophysics Data System (ADS)

    Hu, Li; Zhao, Nanjing; Liu, Wenqing; Meng, Deshuo; Fang, Li; Wang, Yin; Yu, Yang; Ma, Mingjun

    2015-08-01

    Heavy metals in water can be deposited on graphite flakes, which can be used as an enrichment method for laser-induced breakdown spectroscopy (LIBS) and is studied in this paper. The graphite samples were prepared with an automatic device, which was composed of a loading and unloading module, a quantitatively adding solution module, a rapid heating and drying module and a precise rotating module. The experimental results showed that the sample preparation methods had no significant effect on sample distribution and the LIBS signal accumulated in 20 pulses was stable and repeatable. With an increasing amount of the sample solution on the graphite flake, the peak intensity at Cu I 324.75 nm accorded with the exponential function with a correlation coefficient of 0.9963 and the background intensity remained unchanged. The limit of detection (LOD) was calculated through linear fitting of the peak intensity versus the concentration. The LOD decreased rapidly with an increasing amount of sample solution until the amount exceeded 20 mL and the correlation coefficient of exponential function fitting was 0.991. The LOD of Pb, Ni, Cd, Cr and Zn after evaporating different amounts of sample solution on the graphite flakes was measured and the variation tendency of their LOD with sample solution amounts was similar to the tendency for Cu. The experimental data and conclusions could provide a reference for automatic sample preparation and heavy metal in situ detection. supported by National Natural Science Foundation of China (No. 60908018), National High Technology Research and Development Program of China (No. 2013AA065502) and Anhui Province Outstanding Youth Science Fund of China (No. 1108085J19)

  1. A (13)C NMR analysis of the effects of electron radiation on graphite/polyetherimide composites

    NASA Technical Reports Server (NTRS)

    Ferguson, Milton W.

    1989-01-01

    Initial investigations have been made into the use of high resolution nuclear magnetic resonance (NMR) for the characterization of radiation effects in graphite and Kevlar fibers, polymers, and the fiber/matrix interface in graphite/polyetherimide composites. Sample preparation techniques were refined. Essential equipment has been procured. A new NMR probe was constructed to increase the proton signal-to-noise ratio. Problem areas have been identified and plans developed to resolve them.

  2. Fundamental studies of graphene/graphite and graphene-based Schottky photovoltaic devices

    NASA Astrophysics Data System (ADS)

    Miao, Xiaochang

    In the carbon allotropes family, graphene is one of the most versatile members and has been extensively studied since 2004. The goal of this dissertation is not only to investigate the novel fundamental science of graphene and its three-dimensional sibling, graphite, but also to explore graphene's promising potential in modern electronic and optoelectronic devices. The first two chapters provide a concise introduction to the fundamental solid state physics of graphene (as well as graphite) and the physics at the metal/semiconductor interfaces. In the third chapter, we demonstrate the formation of Schottky junctions at the interfaces of graphene (semimetal) and various inorganic semiconductors that play dominating roles in today's semiconductor technology, such as Si, SiC, GaAs and GaN. As shown from their current-voltage (I -V) and capacitance-voltage (C-V) characteristics, the interface physics can be well described within the framework of the Schottky-Mott model. The results are also well consist with that from our previous studies on graphite based Schottky diodes. In the fourth chapter, as an extension of graphene based Schottky work, we investigate the photovoltaic (PV) effect of graphene/Si junctions after chemically doped with an organic polymer (TFSA). The power conversion efficiency of the solar cell improves from 1.9% to 8.6% after TFSA doping, which is the record in all graphene based PVs. The I -V, C-V and external quantum efficiency measurements suggest 12 that such a significant enhancement in the device performance can be attributed to a doping-induced decrease in the series resistance and a simultaneous increase in the built-in potential. In the fifth chapter, we investigate for the first time the effect of uniaxial strains on magneto-transport properties of graphene. We find that low-temperature weak localization effect in monolayer graphene is gradually suppressed under increasing strains, which is due to a strain-induced decreased intervalley-scattering rate. In chapter 6, we study the high vacuum thermal annealing effect on an unconventional ferromagnetism (FM) in highly oriented pyrolytic graphite (HOPG). The FM diminishes and eventually disappears in annealed samples accompanied by improved electrical transport properties and crystallinity. Our results indicate that the FM is mainly coming from the lattice imperfections.

  3. Correlated XANES, TEM, and NanoSIMS of presolar graphite grains

    NASA Astrophysics Data System (ADS)

    Groopman, Evan E.; Nittler, Larry R.

    2018-01-01

    We report correlated XANES, TEM, and NanoSIMS measurements of twelve presolar graphite grains extracted from primitive meteorites and for which isotopic data indicate predominantly Type-II supernovae origins. We find continued evidence for isotopic heterogeneities in presolar graphite grains, including the first observation of a radial gradient in the inferred initial 26Al/27Al within a presolar graphite grain. The XANES spectra of these samples show a variety of minor absorbances near the C K-edge, attributable to vinyl-keto, aliphatic, carboxyl, and carbonate molecules, as well as possible damage during sample preparation. Each sample exhibits homogeneous C K-edge XANES spectra within the graphite, however, showing no correlation with isotopic heterogeneities. Gradients in the isotope ratios of C, N, O, and Al could be due to both processes during condensation, e.g., mixing in stellar ejecta and granular transport, and post-condensation effects, such as isotope dilution and exchange with isotopically normal material in the early Solar System or laboratory, the latter of which is a significant issue for high-density presolar graphite grains. It remains unknown whether the mechanisms behind isotope exchange would also affect the local chemistry and therefore the XANES spectra. Ti L-edge XANES from most Ti-rich subgrains match standard spectra for TiC and potentially TiCN. A rare rutile (TiO2) subgrain has been identified, though it lacks the lowest energy L3 peak typically seen in standard spectra. Ca has also been identified by EDXS in TiC subgrains, likely due to the decay of live 44Ti at the time of formation. Future NanoSIMS measurements will determine the variability of initial 44Ti in TiC subgrains, an important constraint on mixing in the ejecta of the grains' parent supernovae.

  4. Anode performance of boron-doped graphites prepared from shot and sponge cokes

    NASA Astrophysics Data System (ADS)

    Liu, Tao; Luo, Ruiying; Yoon, Seong-Ho; Mochida, Isao

    The structures and anode performances of graphitized pristine and boron-doped shot and sponge cokes have been comparatively studied by means of scanning electron microscope (SEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and galvanostatic measurement. The results show that high degree of graphitization can be obtained by the substituted boron atom in the carbon lattice, and boron in the resultant boron-doped graphites mainly exist in the form of boron carbide and boron substituted in the carbon lattice. Both of boron-doped graphites from shot and sponge cokes obtain discharge capacity of 350 mAh g -1 and coulombic efficiency above 90%. Apart from commonly observed discharge plateau for graphite, boron-doped samples in this study also show a small plateau at ca. 0.06 V. This phenomenon can be explained that Li ion stores in the site to be void-like spaces that are produced by "molecular bridging" between the edge sites of graphene layer stack with a release of boron atoms substituted at the edge of graphene layer. The effect of the amount of boron dopant and graphitization temperature on the anode performance of boron-doped graphite are also investigated in this paper.

  5. Direct determination of Pb in raw milk by graphite furnace atomic absorption spectrometry (GF AAS) with electrothermal atomization sampling from slurries.

    PubMed

    de Oliveira, Tatiane Milão; Augusto Peres, Jayme; Lurdes Felsner, Maria; Cristiane Justi, Karin

    2017-08-15

    Milk is an important food in the human diet due to its physico-chemical composition; therefore, it is necessary to monitor contamination by toxic metals such as Pb. Milk sample slurries were prepared using Triton X-100 and nitric acid for direct analysis of Pb using graphite furnace atomic absorption spectrometry - GF AAS. After dilution of the slurries, 10.00µl were directly introduced into the pyrolytic graphite tube without use of a chemical modifier, which acts as an advantage considering this type of matrix. The limits of detection and quantification were 0.64 and 2.14µgl -1 , respectively. The figures of merit studied showed that the proposed methodology without pretreatment of the raw milk sample and using external standard calibration is suitable. The methodology was applied in milk samples from the Guarapuava region, in Paraná State (Brazil) and Pb concentrations ranged from 2.12 to 37.36µgl -1 . Copyright © 2017 Elsevier Ltd. All rights reserved.

  6. Comparison between the Strength Levels of Baseline Nuclear-Grade Graphite and Graphite Irradiated in AGC-2

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

    Carroll, Mark Christopher

    2015-07-01

    This report details the initial comparison of mechanical strength properties between the cylindrical nuclear-grade graphite specimens irradiated in the second Advanced Graphite Creep (AGC-2) experiment with the established baseline, or unirradiated, mechanical properties compiled in the Baseline Graphite Characterization program. The overall comparative analysis will describe the development of an appropriate test protocol for irradiated specimens, the execution of the mechanical tests on the AGC-2 sample population, and will further discuss the data in terms of developing an accurate irradiated property distribution in the limited amount of irradiated data by leveraging the considerably larger property datasets being captured in themore » Baseline Graphite Characterization program. Integrating information on the inherent variability in nuclear-grade graphite with more complete datasets is one of the goals of the VHTR Graphite Materials program. Between “sister” specimens, or specimens with the same geometry machined from the same sub-block of graphite from which the irradiated AGC specimens were extracted, and the Baseline datasets, a comprehensive body of data will exist that can provide both a direct and indirect indication of the full irradiated property distributions that can be expected of irradiated nuclear-grade graphite while in service in a VHTR system. While the most critical data will remain the actual irradiated property measurements, expansion of this data into accurate distributions based on the inherent variability in graphite properties will be a crucial step in qualifying graphite for nuclear use as a structural material in a VHTR environment.« less

  7. Physical aging in graphite/epoxy composites

    NASA Technical Reports Server (NTRS)

    Kong, E. S. W.

    1983-01-01

    Sub-Tg annealing has been found to affect the properties of graphite/epoxy composites. The network epoxy studied was based on the chemistry of tetraglycidyl 4,4'-diamino-diphenyl methane (TGDDM) crosslinked by 4,4'-diamino-diphenyl sulfone (DDS). Differential scanning calorimetry, thermal mechanical analysis, and solid-state cross-polarized magic-angle-spinning nuclear magnetic resonance spectroscopy have been utilized in order to characterize this process of recovery towards thermodynamic equilibrium. The volume and enthalpy recovery as well as the 'thermoreversibility' aspects of the physical aging are discussed. This nonequilibrium and time-dependent behavior of network epoxies are considered in view of the increasingly wide applications of TGDDM-DDS epoxies as matrix materials of structural composites in the aerospace industry.

  8. NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR EXTRACTION OF METALS FROM SOIL, DUST, AIR FILTER, AND SURFACE AND DERMAL SAMPLES FOR AA (GRAPHITE FURNACE OR FLAME) OR ICP-AES ANALYSIS (BCO-L-3.1)

    EPA Science Inventory

    The purpose of this SOP is to describe the acid digestion of soil, house dust, air filter, and surface or dermal wipe samples for analysis using inductively coupled plasma atomic emissions spectrometry (ICP-AES) and/or graphite furnace atomic absorption spectrometry (GFAAS) or fl...

  9. Inertial impaction air sampling device

    DOEpatents

    Dewhurst, K.H.

    1990-05-22

    An inertial impactor is designed which is to be used in an air sampling device for collection of respirable size particles in ambient air. The device may include a graphite furnace as the impaction substrate in a small-size, portable, direct analysis structure that gives immediate results and is totally self-contained allowing for remote and/or personal sampling. The graphite furnace collects suspended particles transported through the housing by means of the air flow system, and these particles may be analyzed for elements, quantitatively and qualitatively, by atomic absorption spectrophotometry. 3 figs.

  10. Determination of gold and cobalt dopants in advanced materials based on tin oxide by slurry sampling high-resolution continuum source graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Filatova, Daria G.; Eskina, Vasilina V.; Baranovskaya, Vasilisa B.; Vladimirova, Svetlana A.; Gaskov, Alexander M.; Rumyantseva, Marina N.; Karpov, Yuri A.

    2018-02-01

    A novel approach is developed for the determination of Co and Au dopants in advanced materials based on tin oxide using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS GFAAS) with direct slurry sampling. Sodium carboxylmethylcellulose (Na-CMC) is an effective stabilizer for diluted suspensions. Use Na-CMC allows to transfer the analytes into graphite furnace completely and reproducibly. The relative standard deviation obtained by HR CS GFAAS was not higher than 4%. Accuracy was proven by means inductively coupled plasma mass spectrometry (ICP-MS) in solutions after decomposition as a comparative technique. To determine Au and Co in the volume of SnO2, the acid decomposition conditions (HCl, HF) of the samples were suggested by means of an autoclave in a microwave oven.

  11. In situ observation of quasimelting of diamond and reversible graphite-diamond phase transformations.

    PubMed

    Huang, J Y

    2007-08-01

    Because of technique difficulties in achieving the extreme high-pressure and high-temperature (HPHT) simultaneously, direct observation of the structures of carbon at extreme HPHT conditions has not been possible. Banhart and Ajayan discovered remarkably that carbon onions can act as nanoscopic pressure cells to generate high pressures. By heating carbon onions to approximately 700 degrees C and under electron beam irradiation, the graphite-to-diamond transformation was observed in situ by transmission electron microscopy (TEM). However, the highest achievable temperature in a TEM heating holder is less than 1000 degrees C. Here we report that, by using carbon nanotubes as heaters and carbon onions as high-pressure cells, temperatures higher than 2000 degrees C and pressures higher than 40 GPa were achieved simultaneously in carbon onions. At such HPHT conditions and facilitated by electron beam irradiation, the diamond formed in the carbon onion cores frequently changed its shape, size, orientation, and internal structure and moved like a fluid, implying that it was in a quasimelting state. The fluctuation between the solid phase of diamond and the fluid/amorphous phase of diamond-like carbon, and the changes of the shape, size, and orientation of the solid diamond, were attributed to the dynamic crystallization of diamond crystal from the quasimolten state and the dynamic graphite-diamond phase transformations. Our discovery offers unprecedented opportunities to studying the nanostructures of carbon at extreme conditions in situ and at an atomic scale.

  12. Electrochemical characterisation of CaCl2 deficient LiCl-KCl-CaCl2 eutectic melt and electro-deoxidation of solid UO2

    NASA Astrophysics Data System (ADS)

    Sri Maha Vishnu, D.; Sanil, N.; Mohandas, K. S.; Nagarajan, K.

    2016-03-01

    The CaCl2 deficient ternary eutectic melt LiCl-KCl-CaCl2 (50.5: 44.2: 5.3 mol %) was electrochemically characterised by cyclic voltammetry and polarization techniques in the context of its probable use as the electrolyte in the electrochemical reduction of solid UO2 to uranium metal. Tungsten (cathodic polarization) and graphite (anodic polarization) working electrodes were used in these studies carried out in the temperature range 623 K-923 K. The cathodic limit of the melt was observed to be set by the deposition of Ca2+ ions followed by Li+ ions on the tungsten electrode and the anodic limit by oxidation of chloride ions on the graphite electrode (chlorine evolution). The difference between the onset potential of deposition of Ca2+ and Li+ was found to be 0.241 V at a scan rate of 20 mV/s at 623 K and the difference decreased with increase in temperature and vanished at 923 K. Polarization measurements with stainless steel (SS) cathode and graphite anode at 673 K showed the possibility of low-energy reactions occurring on the UO2 electrode in the melt. UO2 pellets were cathodically polarized at 3.9 V for 25 h to test the feasibility of electro-reduction to uranium in the melt. The surface of the pellets was found reduced to U metal.

  13. Raman Scattering in a New Carbon Material

    NASA Technical Reports Server (NTRS)

    Voronov, O. A.; Street, K. W., Jr.

    2010-01-01

    Samples of a new carbon material, Diamonite-B, were fabricated under high pressure from a commercial carbon black--identified as mixed fullerenes. The new material is neither graphite-like nor diamond-like, but exhibits electrical properties close to graphite and mechanical properties close to diamond. The use of Raman spectroscopy to investigate the vibrational dynamics of this new carbon material and to provide structural characterization of its short-, medium- and long-range order is reported. We also provide the results of investigations of these samples by high-resolution electron microscopy and X-ray diffraction. Hardness, electrical conductivity, thermal conductivity and other properties of this new material are compared with synthetic graphite-like and diamond-like materials, two other phases of synthetic bulk carbon.

  14. Synthesis of Graphite Oxide with Different Surface Oxygen Contents Assisted Microwave Radiation

    PubMed Central

    Ibarra-Hernández, Adriana

    2018-01-01

    Graphite oxide is synthesized via oxidation reaction using oxidant compounds that have lattice defects by the incorporation of unlike functional groups. Herein, we report the synthesis of the graphite oxide with diverse surface oxygen content through three (B, C, D) different modified versions of the Hummers method assisted microwave radiation compared with the conventional graphite oxide sample obtained by Hummers method (A). These methods allow not only the production of graphite oxide but also reduced graphene oxide, without undergoing chemical, thermal, or mechanical reduction steps. The values obtained of C/O ratio were ~2, 3.4, and ~8.5 for methodologies C, B, and D, respectively, indicating the presence of graphite oxide and reduced graphene oxide, according to X-ray photoelectron spectroscopy. Raman spectroscopy of method D shows the fewest structural defects compared to the other methodologies. The results obtained suggest that the permanganate ion produces reducing species during graphite oxidation. The generation of these species is attributed to a reversible reaction between the permanganate ion with π electrons, ions, and radicals produced after treatment with microwave radiation. PMID:29438280

  15. Performance and Surface Integrity of Ti6Al4V After Sinking EDM with Special Graphite Electrodes

    NASA Astrophysics Data System (ADS)

    Amorim, Fred L.; Stedile, Leandro J.; Torres, Ricardo D.; Soares, Paulo C.; Henning Laurindo, Carlos A.

    2014-04-01

    Titanium and its alloys have high chemical reactivity with most of the cutting tools. This makes it difficult to work with these alloys using conventional machining processes. Electrical discharge machining (EDM) emerges as an alternative technique to machining these materials. In this work, it is investigated the performance of three special grades of graphite as electrodes when ED-Machining Ti6Al4V samples under three different regimes. The main influences of electrical parameters are discussed for the samples material removal rate, volumetric relative wear and surface roughness. The samples surfaces were evaluated using SEM images, microhardness measurements, and x-ray diffraction. It was found that the best results for samples material removal rate, surface roughness, and volumetric relative wear were obtained for the graphite electrode with 10-μm particle size and negative polarity. For all samples machined by EDM and characterized by x-ray (XRD), it was identified the presence of titanium carbides. For the finish EDM regimes, the recast layer presents an increased amount of titanium carbides compared to semi-finish and rough regimes.

  16. Methods of analysis by the U.S. Geological Survey Organic Geochemistry Research Group : determination of triazine and phenylurea herbicides and their degradation products in water using solid-phase extraction and liquid chromatography/mass spectrometry

    USGS Publications Warehouse

    Lee, Edward Alan; Strahan, Alex P.; Thurman, Earl Michael

    2002-01-01

    An analytical method for the determination of 7 triazine and phenylurea herbicides and 12 of their degradation products in natural water samples using solid-phase extraction and liquid chromatography/mass spectrometry is presented in this report. Special consideration was given during the development of the method to prevent the formation of degradation products during the analysis. Filtered water samples were analyzed using 0.5 gram graphitized carbon as the solid-phase extraction media followed by liquid chromatography/mass spectrometry. Three different water-sample matrices?ground-water, surface-water, and reagent-water samples?spiked at 0.2 and 2.0 micrograms per liter were analyzed. Method detection limits ranged from 0.013 to 0.168 microgram per liter for the parent triazine herbicides and the triazine degradation products. Method detection limits ranged from 0.042 to 0.141 microgram per liter for the parent phenylurea herbicides and their degradation products. Mean recoveries for the triazine compounds in the ground- and surface-water samples generally ranged from 72.6 to 117.5 percent, but deethyl-cyanazine amide was recovered at 140.5 percent. Mean recoveries from the ground- and surface-water samples for the phenylurea compounds spiked at the 2.0-micrograms-per-liter level ranged from 82.1 to 114.4 percent. The mean recoveries for the phenylureas spiked at 0.2-microgram per liter were less consistent, ranging from 87.0 to 136.0 percent. Mean recoveries from reagent-water samples ranged from 87.0 to 109.5 percent for all compounds. The triazine compounds and their degradation products are reported in concentrations ranging from 0.05 to 2.0 micrograms per liter, with the exception of deethylcyanazine and deethylcyanazine amide which are reported at 0.20 to 2.0 micrograms per liter. The phenylurea compounds and their degradation products are reported in concentrations ranging from 0.20 to 2.0 micrograms per liter. The upper concentration limit was 2.0 micrograms per liter for all compounds without dilution.

  17. Biotin determination in food supplements by an electrochemical magneto biosensor.

    PubMed

    Kergaravat, Silvina V; Gómez, Gabriel A; Fabiano, Silvia N; Laube Chávez, Tamara I; Pividori, María I; Hernández, Silvia R

    2012-08-15

    An electrochemical magneto biosensor for the rapid determination of biotin in food samples is reported. The affinity reaction was performed on streptavidin-modified magnetic microbeads as a solid support in a direct competitive format. The biotinylated horseradish peroxidase enzyme (biotin-HRP) competes with free biotin in the sample for the binding sites of streptavidin on the magnetic microbeads. The modified magnetic beads were then easily captured by a magneto graphite-epoxy composite electrode and the electrochemical signal was based on the enzymatic activity of the HRP enzyme under the addition of H(2)O(2) as the substrate and o-phenilendiamine as cosubstrate. The response was electrochemically detected by square wave voltammetry. The limit of detection was 8.4×10(-8) mol L(--1) of biotin (20 μg L(--1)) with a dynamic range from 0.94 to 2.4×10(-7) mol L(--1). Biotin-fortified commercial dietary supplement and infant formula samples were evaluated obtaining good performances in the results. Total time of analysis was 40 min per 20 assays. Copyright © 2012 Elsevier B.V. All rights reserved.

  18. Dynamic Finite Element Predictions for Mars Sample Return Cellular Impact Test #4

    NASA Technical Reports Server (NTRS)

    Fasanella, Edwin L.; Billings, Marcus D.

    2001-01-01

    The nonlinear, transient dynamic finite element code, MSC.Dytran, was used to simulate an impact test of an energy absorbing Earth Entry Vehicle (EEV) that will impact without a parachute. EEVOs are designed to return materials from asteroids, comets, or planets for laboratory analysis on Earth. The EEV concept uses an energy absorbing cellular structure designed to contain and limit the acceleration of space exploration samples during Earth impact. The spherical shaped cellular structure is composed of solid hexagonal and pentagonal foam-filled cells with hybrid graphite-epoxy/Kevlar cell walls. Space samples fit inside a smaller sphere at the center of the EEVOs cellular structure. Pre-test analytical predictions were compared with the test results from a bungee accelerator. The model used to represent the foam and the proper failure criteria for the cell walls were critical in predicting the impact loads of the cellular structure. It was determined that a FOAM1 model for the foam and a 20% failure strain criteria for the cell walls gave an accurate prediction of the acceleration pulse for cellular impact.

  19. Rheological characterization of addition polyimide matrix resins and prepregs

    NASA Technical Reports Server (NTRS)

    Maximovich, M. G.; Galeos, R. M.

    1984-01-01

    Although graphite-reinforced polyimide matrix composites offer outstanding specific strength and stiffness, together with high thermal oxidative stability, processing problems connected with their rheological behavior remain to be addressed. The present rheological studies on neat polyimide resin systems encountered outgassing during cure. A staging technique has been developed which can successfully handle polyimide samples, and novel methods were applied to generate rheological curves for graphite-reinforced prepregs. The commercial graphite/polyimide systems studied were PRM 15, LARC 160, and V378A.

  20. Ultrasound assisted combustion synthesis of TiC in Al-Ti-C system.

    PubMed

    Liu, Zhiwei; Rakita, Milan; Xu, Wilson; Wang, Xiaoming; Han, Qingyou

    2015-11-01

    This research investigated the effects of high-intensity ultrasound on the combustion synthesis of TiC particles in Al-Ti-C system. The process involved that high-intensity ultrasound was applied on the surface of a compacted Al-Ti-C pellet directly through a Nb probe during the thermal explosion reaction. By comparing with the sample without ultrasonic treatment, it was found that the thermal explosion reaction for synthesizing TiC phase could take place thoroughly in the ultrasonically treated sample. During the process of synthesizing TiC phase, the dissolution of solid graphite particles into the Al-Ti melt, as well as the nucleation and growth of TiC particles could be promoted effectively due to the effects of ultrasound, leading to an enhancement of the formation of TiC particles. Ultrasound assisted combustion synthesis as a simple and effective approach was proposed for synthesizing materials in this research. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Impact Test and Simulation of Energy Absorbing Concepts for Earth Entry Vehicles

    NASA Technical Reports Server (NTRS)

    Billings, Marcus D.; Fasanella, Edwin L.; Kellas, Sotiris

    2001-01-01

    Nonlinear dynamic finite element simulations have been performed to aid in the design of an energy absorbing concept for a highly reliable passive Earth Entry Vehicle (EEV) that will directly impact the Earth without a parachute. EEV's are designed to return materials from asteroids, comets, or planets for laboratory analysis on Earth. The EEV concept uses an energy absorbing cellular structure designed to contain and limit the acceleration of space exploration samples during Earth impact. The spherical shaped cellular structure is composed of solid hexagonal and pentagonal foam-filled cells with hybrid graphite- epoxy/Kevlar cell walls. Space samples fit inside a smaller sphere at the center of the EEV's cellular structure. Comparisons of analytical predictions using MSC,Dytran with test results obtained from impact tests performed at NASA Langley Research Center were made for three impact velocities ranging from 32 to 40 m/s. Acceleration and deformation results compared well with the test results. These finite element models will be useful for parametric studies of off-nominal impact conditions.

  2. Macrosegregation and Grain Formation Caused by Convection Associated with Directional Solidification Through Cross-Section Increase

    NASA Technical Reports Server (NTRS)

    Ghods, Masoud; Lauer, Mark; Tewari, Surendra; Poirier, David; Grugel, Richard

    2016-01-01

    Cylindrical Al-7 wt% Silicon, Al-19 wt% Copper and Lead-6 wt% Antimony alloy samples were directionally solidified (DS) with liquid above, solid below, and gravity pointing down, in graphite crucibles having an abrupt cross-sectional increase. These alloys have similar solidification shrinkage but are expected to have different degrees of thermosolutal convection during solidification. Microstructures in the DS samples in the vicinity of the section change have been studied in order to examine the effect of convection associated with the combined influence of thermosolutal effects and solidification shrinkage. Extensive radial and axial macrosegregation associated with cross-section change is observed. It also appears that steepling and local primary alpha-phase remelting resulting from convection are responsible for stray grain formation at the reentrant corners. Preliminary results from a numerical model, which includes solidification shrinkage and thermosolutal convection in the mushy zone, indicate that these regions are prone to solutal remelting of dendrites.

  3. Hybridized polymer matrix composites

    NASA Technical Reports Server (NTRS)

    London, A.

    1981-01-01

    Design approaches and materials are described from which are fabricated pyrostatic graphite/epoxy (Gr/Ep) laminates that show improved retention of graphite particulates when subjected to burning. Sixteen hybridized plus two standard Gr/Ep laminates were designed, fabricated, and tested in an effort to eliminate the release of carbon (graphite) fiber particles from burned/burning, mechanically disturbed samples. The term pyrostatic is defined as meaning mechanically intact in the presence of fire. Graphite particulate retentive laminates were constructed whose constituent materials, cost of fabrication, and physical and mechanical properties were not significantly different from existing Gr/Ep composites. All but one laminate (a Celion graphite/bis-maleimide polyimide) were based on an off-the-shelf Gr/Ep, the AS-1/3501-5A system. Of the 16 candidates studied, four thin (10-ply) and four thick (50-ply) hybridized composites are recommended.

  4. Compatibility of the Radio Frequency Mass Gauge with Composite Tanks

    NASA Technical Reports Server (NTRS)

    Zimmerli, Greg; Mueller, Carl

    2015-01-01

    The radio frequency mass gauge (RFMG) is a low-gravity propellant quantity gauge being developed at NASA for possible use in long-duration space missions utilizing cryogenic propellants. As part of the RFMG technology development process, we evaluated the compatibility of the RFMG with a graphite-epoxy composite material used to construct propellant tanks. The key material property that can affect compatibility with the RFMG is the electrical conductivity. Using samples of 8552IM7 graphite-epoxy composite, we characterized the resistivity and reflectivity over a range of frequencies. An RF impedance analyzer was used to characterize the out-of-plane electrical properties (along the sample thickness) in the frequency range 10 to 1800 MHZ. The resistivity value at 500 MHz was 4.8 ohm-cm. Microwave waveguide measurements of samples in the range 1.7 2.6 GHz, performed by inserting the samples into a WR-430 waveguide, showed reflectivity values above 98. Together, these results suggested that a tank constructed from graphite-epoxy composite would produce good quality electromagnetic tank modes, which is needed for the RFMG. This was verified by room-temperature measurements of the electromagnetic modes of a 2.4 m diameter tank constructed by Boeing from similar graphite-epoxy composite material. The quality factor Q of the tank electromagnetic modes, measured via RF reflection measurements from an antenna mounted in the tank, was typically in the range 400 Q 3000. The good quality modes observed in the tank indicate that the RFMG is compatible with graphite-epoxy tanks, and thus the RFMG could be used as a low-gravity propellant quantity gauge in such tanks filled with cryogenic propellants.

  5. Determination of acetanilide herbicides in cereal crops using accelerated solvent extraction, solid-phase extraction and gas chromatography-electron capture detector.

    PubMed

    Zhang, Yaping; Yang, Jun; Shi, Ronghua; Su, Qingde; Yao, Li; Li, Panpan

    2011-07-01

    A method was developed to determine eight acetanilide herbicides from cereal crops based on accelerated solvent extraction (ASE) and solid-phase extraction (SPE) followed by gas chromatography-electron capture detector (GC-ECD) analysis. During the ASE process, the effect of four parameters (temperature, static time, static cycles and solvent) on the extraction efficiency was considered and compared with shake-flask extraction method. After extraction with ASE, four SPE tubes (graphitic carbon black/primary secondary amine (GCB/PSA), GCB, Florisil and alumina-N) were assayed for comparison to obtain the best clean-up efficiency. The results show that GCB/PSA cartridge gave the best recoveries and cleanest chromatograms. The analytical process was validated by the analysis of spiked blank samples. Performance characteristics such as linearity, limit of detection (LOD), limit of quantitation (LOQ), precision and recovery were studied. At 0.05 mg/kg spiked level, recoveries and precision values for rice, wheat and maize were 82.3-115.8 and 1.1-13.6%, respectively. For all the herbicides, LOD and LOQ ranged from 0.8 to 1.7 μg/kg and from 2.4 to 5.3 μg/kg, respectively. The proposed analytical methodology was applied for the analysis of the targets in samples; only three herbicides, propyzamid, metolachlor and diflufenican, were detected in two samples. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Temperature and flow fields in samples heated in monoellipsoidal mirror furnaces

    NASA Astrophysics Data System (ADS)

    Rivas, D.; Haya, R.

    The temperature field in samples heated in monoellipsoidal mirror furnaces will be analyzed. The radiation heat exchange between the sample and the mirror is formulated analytically, taking into account multiple reflections at the mirror. It will be shown that the effect of these multiple reflections in the heating process is quite important, and, as a consequence, the effect of the mirror reflectance in the temperature field is quite strong. The conduction-radiation model will be used to simulate the heating process in the floating-zone technique in microgravity conditions; important parameters like the Marangoni number (that drives the thermocapillary flow in the melt), and the temperature gradient at the melt-crystal interface will be estimated. The model will be validated comparing with experimental data. The case of samples mounted in a wall-free configuration (as in the MAXUS-4 programme) will be also considered. Application to the case of compound samples (graphite-silicon-graphite) will be made; the melting of the silicon part and the surface temperature distribution in the melt will be analyzed. Of special interest is the temperature difference between the two graphite rods that hold the silicon part, since it drives the thermocapillary flow in the melt. This thermocapillary flow will be studied, after coupling the previous model with the convective effects. The possibility of counterbalancing this flow by the controlled vibration of the graphite rods will be studied as well. Numerical results show that suppressing the thermocapillary flow can be accomplished quite effectively.

  7. Pretreatment of lubricated surfaces with sputtered cadmium oxide

    NASA Technical Reports Server (NTRS)

    Fusaro, Robert L. (Inventor)

    1991-01-01

    Cadmium oxide is used with a dry solid lubricant on a surface to improve wear resistance. The surface topography is first altered by photochemical etching to a predetermined pattern. The cadmium oxide is then sputtered onto the altered surface to form an intermediate layer to more tightly hold the dry lubricant, such as graphite.

  8. Levitation of water and organic substances in high static magnetic fields

    NASA Astrophysics Data System (ADS)

    Beaugnon, E.; Tournier, R.

    1991-08-01

    The levitation of various diamagnetic liquid and solid substances such as water, ethanol, acetone, bismuth, antimony, graphite, wood and plastic has been achieved at room temperature in a strong inhomogeneous static magnetic field. These experiments were performed in the hybrid magnet at the Service National des Champs Intenses (CNRS, Grenoble). These findings show that high field superconducting magnets could be used to provide a contactless, low gravity environment for the elaboration of a wide range of materials. En utilisant les forts champs magnétiques produits par la bobine hybride du Service National des Champs Intenses (CNRS, Grenoble), nous avons obtenu àtempérature ambiante la lévitation de substances diamagnétiques solides ou liquides telles que l'eau, l'alcool, l'acétone, le bismuth, l'antimoine, le graphite, le bois et le plastique. Ces résultats montrent que les bobines supraconductrices peuvent être utilisées pour l'élaboration de nombreux matériaux en gravité réduite, sans contact avec un contenant.

  9. Nanosecond formation of diamond and lonsdaleite by shock compression of graphite.

    PubMed

    Kraus, D; Ravasio, A; Gauthier, M; Gericke, D O; Vorberger, J; Frydrych, S; Helfrich, J; Fletcher, L B; Schaumann, G; Nagler, B; Barbrel, B; Bachmann, B; Gamboa, E J; Göde, S; Granados, E; Gregori, G; Lee, H J; Neumayer, P; Schumaker, W; Döppner, T; Falcone, R W; Glenzer, S H; Roth, M

    2016-03-14

    The shock-induced transition from graphite to diamond has been of great scientific and technological interest since the discovery of microscopic diamonds in remnants of explosively driven graphite. Furthermore, shock synthesis of diamond and lonsdaleite, a speculative hexagonal carbon polymorph with unique hardness, is expected to happen during violent meteor impacts. Here, we show unprecedented in situ X-ray diffraction measurements of diamond formation on nanosecond timescales by shock compression of pyrolytic as well as polycrystalline graphite to pressures from 19 GPa up to 228 GPa. While we observe the transition to diamond starting at 50 GPa for both pyrolytic and polycrystalline graphite, we also record the direct formation of lonsdaleite above 170 GPa for pyrolytic samples only. Our experiment provides new insights into the processes of the shock-induced transition from graphite to diamond and uniquely resolves the dynamics that explain the main natural occurrence of the lonsdaleite crystal structure being close to meteor impact sites.

  10. Change of properties after oxidation of IG-11 graphite by air and CO 2 gas

    NASA Astrophysics Data System (ADS)

    Lim, Yun-Soo; Chi, Se-Hwan; Cho, Kwang-Yun

    2008-02-01

    Artificial graphite is typically manufactured by carbonization of a shaped body of a kneaded mixture using granular cokes as a filler and pitch as a binder. It undergoes a pitch impregnation process if necessary and finally applying graphitization heat treatment. The effect of thermal oxidation in air or a CO 2 atmosphere on IG-11 graphite samples is investigated in this study. The results show a localized oxidation process that progressively reveals the large coke particles with increasing level of overall weight loss in air. The surface of the graphite was peeled off and no change was found in the specific gravity after air oxidation. However, the specific gravity of graphite was continuously decreased by CO 2 oxidation. The decrease in the specific gravity by CO 2 oxidation was due to CO 2 gas that progressed from the surface to the interior. The pore shape after CO 2 oxidation differed from that under air oxidation.

  11. Nanosecond formation of diamond and lonsdaleite by shock compression of graphite

    DOE PAGES

    Kraus, D.; Ravasio, A.; Gauthier, M.; ...

    2016-03-14

    The shock-induced transition from graphite to diamond has been of great scientific and technological interest since the discovery of microscopic diamonds in remnants of explosively driven graphite. Furthermore, shock synthesis of diamond and lonsdaleite, a speculative hexagonal carbon polymorph with unique hardness, is expected to happen during violent meteor impacts. Here, we show unprecedented in situ X-ray diffraction measurements of diamond formation on nanosecond timescales by shock compression of pyrolytic as well as polycrystalline graphite to pressures from 19 GPa up to 228 GPa. While we observe the transition to diamond starting at 50 GPa for both pyrolytic and polycrystallinemore » graphite, we also record the direct formation of lonsdaleite above 170 GPa for pyrolytic samples only. In conclusion, our experiment provides new insights into the processes of the shock-induced transition from graphite to diamond and uniquely resolves the dynamics that explain the main natural occurrence of the lonsdaleite crystal structure being close to meteor impact sites.« less

  12. Highly selective dopamine electrochemical sensor based on electrochemically pretreated graphite and nafion composite modified screen printed carbon electrode.

    PubMed

    Ku, Shuhao; Palanisamy, Selvakumar; Chen, Shen-Ming

    2013-12-01

    Herein, we report a highly selective dopamine electrochemical sensor based on electrochemically pretreated graphite/nafion composite modified screen printed carbon (SPC) electrode. Electrochemically activated graphite/nafion composite was prepared by using a simple electrochemical method. Scanning electron microscope (SEM) used to characterize the surface morphology of the fabricated composite electrode. The SEM result clearly indicates that the graphitic basal planes were totally disturbed and leads to the formation of graphite nanosheets. The composite modified electrode showed an enhanced electrocatalytic activity toward the oxidation of DA when compared with either electrochemical pretreated graphite or nafion SPC electrodes. The fabricated composite electrode exhibits a good electrocatalytic oxidation toward DA in the linear response range from 0.5 to 70 μM with the detection limit of 0.023 μM. The proposed sensor also exhibits very good selectivity and stability, with the appreciable sensitivity. In addition, the proposed sensor showed satisfactory recovery results toward the commercial pharmaceutical DA samples. Copyright © 2013 Elsevier Inc. All rights reserved.

  13. Ti-doped isotropic graphite: A promising armour material for plasma-facing components

    NASA Astrophysics Data System (ADS)

    García-Rosales, C.; López-Galilea, I.; Ordás, N.; Adelhelm, C.; Balden, M.; Pintsuk, G.; Grattarola, M.; Gualco, C.

    2009-04-01

    Finely dispersed Ti-doped isotropic graphites with 4 at.% Ti have been manufactured using synthetic mesophase pitch 'AR' as raw material. These new materials show a thermal conductivity at room temperature of ˜200 W/mK and flexural strength close to 100 MPa. Measurement of the total erosion yield by deuterium bombardment at ion energies and sample temperatures for which pure carbon shows maximum values, resulted in a reduction of at least a factor of 4, mainly due to dopant enrichment at the surface caused by preferential erosion of carbon. In addition, ITER relevant thermal shock loads were applied with an energetic electron beam at the JUDITH facility. The results demonstrated a significantly improved performance of Ti-doped graphite compared to pure graphite. Finally, Ti-doped graphite was successfully brazed to a CuCrZr block using a Mo interlayer. These results let assume that Ti-doped graphite can be a promising armour material for divertor plasma-facing components.

  14. Nanosecond formation of diamond and lonsdaleite by shock compression of graphite

    PubMed Central

    Kraus, D.; Ravasio, A.; Gauthier, M.; Gericke, D. O.; Vorberger, J.; Frydrych, S.; Helfrich, J.; Fletcher, L. B.; Schaumann, G.; Nagler, B.; Barbrel, B.; Bachmann, B.; Gamboa, E. J.; Göde, S.; Granados, E.; Gregori, G.; Lee, H. J.; Neumayer, P.; Schumaker, W.; Döppner, T.; Falcone, R. W.; Glenzer, S. H.; Roth, M.

    2016-01-01

    The shock-induced transition from graphite to diamond has been of great scientific and technological interest since the discovery of microscopic diamonds in remnants of explosively driven graphite. Furthermore, shock synthesis of diamond and lonsdaleite, a speculative hexagonal carbon polymorph with unique hardness, is expected to happen during violent meteor impacts. Here, we show unprecedented in situ X-ray diffraction measurements of diamond formation on nanosecond timescales by shock compression of pyrolytic as well as polycrystalline graphite to pressures from 19 GPa up to 228 GPa. While we observe the transition to diamond starting at 50 GPa for both pyrolytic and polycrystalline graphite, we also record the direct formation of lonsdaleite above 170 GPa for pyrolytic samples only. Our experiment provides new insights into the processes of the shock-induced transition from graphite to diamond and uniquely resolves the dynamics that explain the main natural occurrence of the lonsdaleite crystal structure being close to meteor impact sites. PMID:26972122

  15. Transparent, flexible supercapacitors from nano-engineered carbon films.

    PubMed

    Jung, Hyun Young; Karimi, Majid B; Hahm, Myung Gwan; Ajayan, Pulickel M; Jung, Yung Joon

    2012-01-01

    Here we construct mechanically flexible and optically transparent thin film solid state supercapacitors by assembling nano-engineered carbon electrodes, prepared in porous templates, with morphology of interconnected arrays of complex shapes and porosity. The highly textured graphitic films act as electrode and current collector and integrated with solid polymer electrolyte, function as thin film supercapacitors. The nanostructured electrode morphology and the conformal electrolyte packaging provide enough energy and power density for the devices in addition to excellent mechanical flexibility and optical transparency, making it a unique design in various power delivery applications.

  16. Transparent, flexible supercapacitors from nano-engineered carbon films

    PubMed Central

    Jung, Hyun Young; Karimi, Majid B.; Hahm, Myung Gwan; Ajayan, Pulickel M.; Jung, Yung Joon

    2012-01-01

    Here we construct mechanically flexible and optically transparent thin film solid state supercapacitors by assembling nano-engineered carbon electrodes, prepared in porous templates, with morphology of interconnected arrays of complex shapes and porosity. The highly textured graphitic films act as electrode and current collector and integrated with solid polymer electrolyte, function as thin film supercapacitors. The nanostructured electrode morphology and the conformal electrolyte packaging provide enough energy and power density for the devices in addition to excellent mechanical flexibility and optical transparency, making it a unique design in various power delivery applications. PMID:23105970

  17. Transparent, flexible supercapacitors from nano-engineered carbon films

    NASA Astrophysics Data System (ADS)

    Jung, Hyun Young; Karimi, Majid B.; Hahm, Myung Gwan; Ajayan, Pulickel M.; Jung, Yung Joon

    2012-10-01

    Here we construct mechanically flexible and optically transparent thin film solid state supercapacitors by assembling nano-engineered carbon electrodes, prepared in porous templates, with morphology of interconnected arrays of complex shapes and porosity. The highly textured graphitic films act as electrode and current collector and integrated with solid polymer electrolyte, function as thin film supercapacitors. The nanostructured electrode morphology and the conformal electrolyte packaging provide enough energy and power density for the devices in addition to excellent mechanical flexibility and optical transparency, making it a unique design in various power delivery applications.

  18. Cleanup Verification Package for the 118-F-1 Burial Ground

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

    E. J. Farris and H. M. Sulloway

    2008-01-10

    This cleanup verification package documents completion of remedial action for the 118-F-1 Burial Ground on the Hanford Site. This burial ground is a combination of two locations formerly called Minor Construction Burial Ground No. 2 and Solid Waste Burial Ground No. 2. This waste site received radioactive equipment and other miscellaneous waste from 105-F Reactor operations, including dummy elements and irradiated process tubing; gun barrel tips, steel sleeves, and metal chips removed from the reactor; filter boxes containing reactor graphite chips; and miscellaneous construction solid waste.

  19. METHOD FOR PREPARING URANIUM MONOCARBIDE-PLUTONIUM MONOCARBIDE SOLID SOLUTION

    DOEpatents

    Ogard, A.E.; Leary, J.A.; Maraman, W.J.

    1963-03-19

    A method is given for preparing solid solutions of uranium monocarbide- plutonium monocarbide. In this method, the powder form of uranium dioxide, plutonium dioxide, and graphite are mixed in a ratio determined by the equation: xUO/sub 2/ + yPuO/sub 2/ + (2+z)C yields UxPu/sub y/C/sub z/ +2CO, where x + y equ al 1.0 and z is greater than 0.9 but less than 1.0. The resulting mixture is compacted and heated in a vacuum at a temperature of 1850 deg C. (AEC)

  20. Closed tubes preparation of graphite for high-precision AMS radiocarbon analysis

    NASA Astrophysics Data System (ADS)

    Hajdas, I.; Michczynska, D.; Bonani, G.; Maurer, M.; Wacker, L.

    2009-04-01

    Radiocarbon dating is an established tool applied in Geochronology. Technical developments of Accelerator Mass Spectrometry AMS, which allow measurements of samples containing less than 1 mg of carbon, opened opportunities for new applications. Moreover, high resolution records of the past changes require high-resolution chronologies i.e. sampling for 14C dating. In result, the field of applications is rapidly expanding and number of radiocarbon analysis is growing rapidly. Nowadays dedicated 14C AMS machines have great capacity for analysis but in order to keep up with the demand for analysis and provide the results as fast as possible a very efficient way of sample preparation is required. Sample preparation for 14C AMS analysis consists of two steps: separation of relevant carbon from the sample material (removing contamination) and preparation of graphite for AMS analysis. The last step usually involves reaction of CO2 with H2, in the presence of metal catalyst (Fe or Co) of specific mesh size heated to 550-625°C, as originally suggested by Vogel et al. (1984). Various graphitization systems have been built in order to fulfil the requirement of sample quality needed for high-precision radiocarbon data. In the early 90ties another method has been proposed (Vogel 1992) and applied by few laboratories mainly for environmental or biomedical samples. This method uses TiH2 as a source of H2 and can be easily and flexibly applied to produce graphite. Sample of CO2 is frozen in to the tube containing pre-conditioned Zn/TiH2 and Fe catalyst. Torch sealed tubes are then placed in the stepwise heated oven at 500/550°C and left to react for several hours. The greatest problem is the lack of control of the reaction completeness and considerable fractionation. However, recently reported results (Xu et al. 2007) suggest that high precision dating using graphite produced in closed tubes might be possible. We will present results of radiocarbon dating of the set of standards and secondary IAEA standards to demonstrate to what level this method can be used for high precision radiocarbon dating. References Vogel JS. 1992. Rapid Production of Graphite without Contamination for Biomedical Ams. Radiocarbon 34: 344-350. Vogel JS, Southon JR, Nelson DE, and Brown TA. 1984. Performance of Catalytically Condensed Carbon for Use in Accelerator Mass-Spectrometry. Nuclear Instruments & Methods in Physics Research Section B-Beam Interactions with Materials and Atoms 233: 289-293. Xu X, Trumbore SE, Zheng S, Southon JR, McDuffee KE, Luttgen M, and Liu JC. 2007. Modifying a sealed tube zinc reduction method for preparation of AMS graphite targets: Reducing background and attaining high precision. Nuclear Instruments and Methods in Physics Research Section B: Beam Interactions with Materials and Atoms Accelerator Mass Spectrometry - Proceedings of the Tenth International Conference on Accelerator Mass Spectrometry 259: 320-329.

  1. Study of blended conductive graft copolymer with graphite oxide thin films deposited using spin coating method for gas sensing and photovoltaic applications

    NASA Astrophysics Data System (ADS)

    KałuŻyński, P.; Procek, M.; Stolarczyk, Agnieszka; Maciak, E.

    2017-08-01

    This work presents an investigation on conductive graft comb copolymer like SILPEG CH9 with carbon materials like graphite oxide or reduced graphite oxide. Morphology and optical properties like sample roughness, graphite oxide particles distribution, optical transmittance were measured of obtained thin films deposited on glass substrate using spin coating method. The study showed that obtained thin films are repeatable, convenient to process, and their parameters can be easy changed by the spin rate regulation during the deposition. Given results shows the possibility of using such polymer blend in the implementation of organic photovoltaic cells and different optoelectronics applications.

  2. Comparison of the morphology, chemical composition and microstructure of cryptocrystalline graphite and carbon black

    NASA Astrophysics Data System (ADS)

    Quan, Ying; Liu, Qinfu; Zhang, Shilong; Zhang, Shuai

    2018-07-01

    The structures of cryptocrystalline graphite (CG) and carbon black (CB) have been analyzed using scanning electron microscopy (SEM), transmission electron microscopy (TEM), organic elemental analysis (OEA), X-ray diffraction (XRD), RAMAN and high-resolution transmission electron microscopy (HRTEM). These results indicate that CG has the same elemental composition as CB, with carbon being the major element present. SL sample (CG with low graphitization degree) and CB exhibit similar microcrystalline structures. CG was shown to contain a layered graphitic structure that was significantly different to the primary spherical particles present in CB. It is proposed that these CG sheets may potentially be reduced and delaminated to afford multilayer graphene structures with improved material properties.

  3. U.S.-MEXICO BORDER PROGRAM ARIZONA BORDER STUDY--STANDARD OPERATING PROCEDURE FOR EXTRACTION OF METALS FROM SOIL, DUST, AIR FILTER, AND SURFACE AND DERMAL WIPE SAMPLES FOR AA (GRAPHITE FURNACE OR FLAME) OR ICP-AES ANALYSIS (BCO-L-3.1)

    EPA Science Inventory

    The purpose of this SOP is to describe the acid digestion of soil, house dust, air filter, and surface or dermal wipe samples for analysis using inductively coupled plasma atomic emissions spectrometry (ICP-AES) and/or graphite furnace atomic absorption spectrometry (GFAAS) or fl...

  4. Method for electrostatic deposition of graphene on a substrate

    NASA Technical Reports Server (NTRS)

    Sumanasekera, Gamini (Inventor); Sidorov, Anton N. (Inventor); Ouseph, P. John (Inventor); Yazdanpanah, Mehdi M. (Inventor); Cohn, Robert W. (Inventor); Jalilian, Romaneh (Inventor)

    2010-01-01

    A method for electrostatic deposition of graphene on a substrate comprises the steps of securing a graphite sample to a first electrode; electrically connecting the first electrode to a positive terminal of a power source; electrically connecting a second electrode to a ground terminal of the power source; placing the substrate over the second electrode; and using the power source to apply a voltage, such that graphene is removed from the graphite sample and deposited on the substrate.

  5. Liquid-phase pulsed laser ablation synthesis of graphitized carbon-encapsulated palladium core-shell nanospheres for catalytic reduction of nitrobenzene to aniline

    NASA Astrophysics Data System (ADS)

    Kim, Yu-jin; Ma, Rory; Reddy, D. Amaranatha; Kim, Tae Kyu

    2015-12-01

    Graphitized carbon-encapsulated palladium (Pd) core-shell nanospheres were produced via pulsed laser ablation of a solid Pd foil target submerged in acetonitrile. The microstructural features and optical properties of these nanospheres were characterized via high resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and UV-visible spectroscopy. Microstructural analysis indicated that the core-shell nanostructures consisted of single-crystalline cubic metallic Pd spheres that serve as the core material, over which graphitized carbon was anchored as a heterogeneous shell. The absorbance spectrum of the synthesized nanostructures exhibited a broad (absorption) band at ∼264 nm; this band corresponded to the typical inter-band transition of a metallic system and resulted possibly from the absorbance of the ionic Pd2+. The catalytic properties of the Pd and Pd@C core-shell nanostructures were investigated using the reduction of nitrobenzene to aniline by an excess amount of NaBH4 in an aqueous solution at room temperature, as a model reaction. Owing to the graphitized carbon-layered structure and the high specific surface area, the resulting Pd@C nanostructures exhibited higher conversion efficiencies than their bare Pd counterparts. In fact, the layered structure provided access to the surface of the Pd nanostructures for the hydrogenation reaction, owing to the synergistic effect between graphitized carbon and the nanostructures. Their unique structure and excellent catalytic performance render Pd@C core-shell nanostructures highly promising candidates for catalysis applications.

  6. Mars Mission Analysis Trades Based on Legacy and Future Nuclear Propulsion Options

    NASA Astrophysics Data System (ADS)

    Joyner, Russell; Lentati, Andrea; Cichon, Jaclyn

    2007-01-01

    The purpose of this paper is to discuss the results of mission-based system trades when using a nuclear thermal propulsion (NTP) system for Solar System exploration. The results are based on comparing reactor designs that use a ceramic-metallic (CERMET), graphite matrix, graphite composite matrix, or carbide matrix fuel element designs. The composite graphite matrix and CERMET designs have been examined for providing power as well as propulsion. Approaches to the design of the NTP to be discussed will include an examination of graphite, composite, carbide, and CERMET core designs and the attributes of each in regards to performance and power generation capability. The focus is on NTP approaches based on tested fuel materials within a prismatic fuel form per the Argonne National Laboratory testing and the ROVER/NERVA program. NTP concepts have been examined for several years at Pratt & Whitney Rocketdyne for use as the primary propulsion for human missions beyond earth. Recently, an approach was taken to examine the design trades between specific NTP concepts; NERVA-based (UC)C-Graphite, (UC,ZrC)C-Composite, (U,Zr)C-Solid Carbide and UO2-W CERMET. Using Pratt & Whitney Rocketdyne's multidisciplinary design analysis capability, a detailed mission and vehicle model has been used to examine how several of these NTP designs impact a human Mars mission. Trends for the propulsion system mass as a function of power level (i.e. thrust size) for the graphite-carbide and CERMET designs were established and correlated against data created over the past forty years. These were used for the mission trade study. The resulting mission trades presented in this paper used a comprehensive modeling approach that captures the mission, vehicle subsystems, and NTP sizing.

  7. Schnellverfahren zur flammenlosen AAS-Bestimmung von Spurenelementen in geologischen Proben

    NASA Astrophysics Data System (ADS)

    Schrön, W.; Bombach, G.; Beuge, P.

    This paper reports experience with direct quantitative trace element determinations in powdered geological samples by nameless atomic absorption spectroscopy. Two methods were explored. The first one is based on the production of a sample aerosol by laser radiation in a specifically designed sample chamber and the subsequent transport of the aerosol into a graphite tube, which has been preheated to a stable temperature. This technique is suited for a large range of concentration and is relatively free from matrix interferences. The technique was tested for the elements Ag, As, Bi, Cd, Co, Mn, Ni, Pb, Sb, Se, Sr and Tl. The described sample chamber can be also used in combination with other spcctroscopic techniques. The second method explored permits the quantitative determination of trace elements at very low concentrations. Essentially an accurately weighed amount of sample is placed on a graphite rod and introduced into a graphite furnace by inserting the rod through the sample injection port. Atomization takes place also under stable temperature conditions. Using this technique detection limits were found to be 10 -11 g for Ag, 2 × 10 -11 g for Cd and 10 -10 g for Sb in silicate materials.

  8. Degradation Mechanisms of Electrochemically Cycled Graphite Anodes in Lithium-ion Cells

    NASA Astrophysics Data System (ADS)

    Bhattacharya, Sandeep

    This research is aimed at developing advanced characterization methods for studying the surface and subsurface damage in Li-ion battery anodes made of polycrystalline graphite and identifying the degradation mechanisms that cause loss of electrochemical capacity. Understanding microstructural aspects of the graphite electrode degradation mechanisms during charging and discharging of Li-ion batteries is of key importance in order to design durable anodes with high capacity. An in-situ system was constructed using an electrochemical cell with an observation window, a large depth-of-field digital microscope and a micro-Raman spectrometer. It was revealed that electrode damage by removal of the surface graphite fragments of 5-10 mum size is the most intense during the first cycle that led to a drastic capacity drop. Once a solid electrolyte interphase (SEI) layer covered the electrode surface, the rate of graphite particle loss decreased. Yet, a gradual loss of capacity continued by the formation of interlayer cracks adjacent to SEI/graphite interfaces. Deposition of co-intercalation compounds, LiC6, Li2CO3 and Li2O, near the crack tips caused partial closure of propagating graphite cracks during cycling and reduced the crack growth rate. Bridging of crack faces by delaminated graphite layers also retarded crack propagation. The microstructure of the SEI layer, formed by electrochemical reduction of the ethylene carbonate based electrolyte, consisted of ˜5-20 nm sized crystalline domains (containing Li2CO3, Li2O 2 and nano-sized graphite fragments) dispersed in an amorphous matrix. During the SEI formation, two regimes of Li-ion diffusion were identified at the electrode/electrolyte interface depending on the applied voltage scan rate (dV/dt). A low Li-ion diffusion coefficient ( DLi+) at dV/dt < 0.05 mVs-1 produced a tubular SEI that uniformly covered the graphite surface and prevented damage at 25°C. At 60°C, a high D Li+ formed a Li2CO3-enriched SEI and ensued a 28% increase in the battery capacity at 25°C. On correlating the microscopic information to the electrochemical performance, novel Li2CO3-coated electrodes were fabricated that were durable. The SEI formed on pre-treated electrodes reduced the strain in the graphite lattice from 0.4% (for uncoated electrodes) to 0.1%, facilitated Li-ion diffusion and hence improved the capacity retention of Li-ion batteries during long-term cycling.

  9. A new oxidation based technique for artifact free TEM specimen preparation of nuclear graphite

    NASA Astrophysics Data System (ADS)

    Johns, Steve; Shin, Wontak; Kane, Joshua J.; Windes, William E.; Ubic, Rick; Karthik, Chinnathambi

    2018-07-01

    Graphite is a key component in designs of current and future nuclear reactors whose in-service lifetimes are dependent upon the mechanical performance of the graphite. Irradiation damage from fast neutrons creates lattice defects which have a dynamic effect on the microstructure and mechanical properties of graphite. Transmission electron microscopy (TEM) can offer real-time monitoring of the dynamic atomic-level response of graphite subjected to irradiation; however, conventional TEM specimen-preparation techniques, such as argon ion milling itself, damage the graphite specimen and introduce lattice defects. It is impossible to distinguish these defects from the ones created by electron or neutron irradiation. To ensure that TEM specimens are artifact-free, a new oxidation-based technique has been developed. Bulk nuclear grades of graphite (IG-110 and NBG-18) and highly oriented pyrolytic graphite (HOPG) were initially mechanically thinned to ∼60 μm. Discs 3 mm in diameter were then oxidized at temperatures between 575 °C and 625 °C in oxidizing gasses using a new jet-polisher-like set-up in order to achieve optimal oxidation conditions to create self-supporting electron-transparent TEM specimens. The quality of these oxidized specimens were established using optical and electron microscopy. Samples oxidized at 575 °C exhibited large areas of electron transparency and the corresponding lattice imaging showed no apparent damage to the graphite lattice.

  10. A new oxidation based technique for artifact free TEM specimen preparation of nuclear graphite

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

    Johns, Steve; Shin, Wontak; Kane, Joshua J.

    Graphite is a key component in designs of current and future nuclear reactors whose in-service lifetimes are dependent upon the mechanical performance of the graphite. Irradiation damage from fast neutrons creates lattice defects which have a dynamic effect on the microstructure and mechanical properties of graphite. Transmission electron microscopy (TEM) can offer real-time monitoring of the dynamic atomic-level response of graphite subjected to irradiation; however, conventional TEM specimen-preparation techniques, such as argon ion milling itself, damage the graphite specimen and introduce lattice defects. It is impossible to distinguish these defects from the ones created by electron or neutron irradiation. Thus,tomore » ensure that TEM specimens are artifact-free, a new oxidation-based technique has been developed. Bulk nuclear grades of graphite (IG-110 and NBG-18) and highly oriented pyrolytic graphite (HOPG) were initially mechanically thinned to ~60μm. Discs 3mm in diameter were then oxidized at temperatures between 575°C and 625°C in oxidizing gasses using a new jet-polisher-like set-up in order to achieve optimal oxidation conditions to create self-supporting electron-transparent TEM specimens. The quality of these oxidized specimens were established using optical and electron microscopy. Samples oxidized at 575°C exhibited large areas of electron transparency and the corresponding lattice imaging showed no apparent damage to the graphite lattice.« less

  11. Carbon isotope geochemistry of graphite vein deposits from New Hampshire, U.S.A.

    NASA Astrophysics Data System (ADS)

    Rumble, Douglas, III; Hoering, Thomas C.

    1986-06-01

    Graphite veins of hydrothermal origin occur throughout central New Hampshire. Veins truncate sillimanite-grade, metasedimentary rocks of Early Devonian-Silurian age and range in size from microscopic to meters in thickness. In addition to graphite, veins may contain quartz, tourmaline, ilmenite, rutile, sillimanite, muscovite or chlorite. Vein mineralogy is generally compatible with wall rock mineral assemblages. Mineralization structures include wall-rock alteration zones, coxcomb graphite crystals on vein walls, and botryoidal, concentrically layered graphite-silicate nodules. The δ13C values of graphite in 14 deposits studied range from - 28%. (PDB) to - 9%. Veins whose textures give evidence of a single stage of mineralization have a narrow range of δ13C values (± 0.2%.). Other veins record successive episodes of graphite precipitation and have ranges of 3-6%. In one sample, adjacent layers of graphite differ by 3%. The wide range of δ13C may be explained by mixing carbon from two crustal reservoirs: biogenic, reduced carbon and carbonate. Precipitation of graphite results from mixing two or more aqueous fluids with different CO 2/CH 4 ratios. Parental fluids are produced by devolatilization during metamorphism. Water-rich fluids with CH4 > CO2 and low δ13C are derived from pelites that contained organic matter; whereas fluids with CO2 > CH4 and high δ13C come from siliceous carbonates.

  12. A new oxidation based technique for artifact free TEM specimen preparation of nuclear graphite

    DOE PAGES

    Johns, Steve; Shin, Wontak; Kane, Joshua J.; ...

    2018-04-03

    Graphite is a key component in designs of current and future nuclear reactors whose in-service lifetimes are dependent upon the mechanical performance of the graphite. Irradiation damage from fast neutrons creates lattice defects which have a dynamic effect on the microstructure and mechanical properties of graphite. Transmission electron microscopy (TEM) can offer real-time monitoring of the dynamic atomic-level response of graphite subjected to irradiation; however, conventional TEM specimen-preparation techniques, such as argon ion milling itself, damage the graphite specimen and introduce lattice defects. It is impossible to distinguish these defects from the ones created by electron or neutron irradiation. Thus,tomore » ensure that TEM specimens are artifact-free, a new oxidation-based technique has been developed. Bulk nuclear grades of graphite (IG-110 and NBG-18) and highly oriented pyrolytic graphite (HOPG) were initially mechanically thinned to ~60μm. Discs 3mm in diameter were then oxidized at temperatures between 575°C and 625°C in oxidizing gasses using a new jet-polisher-like set-up in order to achieve optimal oxidation conditions to create self-supporting electron-transparent TEM specimens. The quality of these oxidized specimens were established using optical and electron microscopy. Samples oxidized at 575°C exhibited large areas of electron transparency and the corresponding lattice imaging showed no apparent damage to the graphite lattice.« less

  13. NEUTRONIC REACTOR AND FUEL ELEMENT THEREFOR

    DOEpatents

    Szilard, L.; Young, G.J.

    1958-03-01

    This patent relates to a reactor design of the type which employs solid fuel elements disposed in channels within the moderator through which channels and around the fuel elements is conveyed a coolant fiuid. The coolant channels are comprised of aluminum tubes extending through a solid moderator such as graphite and the fuel elements are comprised of an elongated solid body of natural uranium jacketed in an aluminum jacket with the ends thereof closed by aluminum caps of substantially greater thickness than the jacket was and in good thermal contact with the fuel material to facilitate the conduction of heat from the central portion of said ends to the coolant surrounding the fuel element to prevent overheating of said central portion.

  14. Decoupling of Solid 4He Layers under the Superfluid Overlayer

    NASA Astrophysics Data System (ADS)

    Ishibashi, Kenji; Hiraide, Jo; Taniguchi, Junko; Suzuki, Masaru

    2018-03-01

    It has been reported that in a large oscillation amplitude, the mass decoupling of multilayer 4He films adsorbed on graphite results from the depinning of the second solid atomic layer. This decoupling suddenly vanishes below a certain low temperature TD due to the cancellation of mass decoupling by the superfluid counterflow of the the overylayer. We studied the relaxation of the depinned state at various temperatures, after reduction of oscillation amplitude below TD . It was found that above the superfluid transition temperature the mass decoupling revives with a relaxation time of several 100 s. It strongly supports that the depinned state of the second solid atomic layer remains underneath the superfluid overlayer.

  15. High-resolution transmission electron microscopy studies of graphite materials prepared by high-temperature treatment of unburned carbon concentrates from combustion fly ashes

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

    Miguel Cabielles; Jean-Nol Rouzaud; Ana B. Garcia

    2009-01-15

    High-resolution transmission electron microscopy (HRTEM) has been used in this work to study the microstructural (structure and microtexture) changes occurring during the high-temperature treatment of the unburned carbon concentrates from coal combustion fly ashes. Emphasis was placed on two aspects: (i) the development of graphitic carbon structures and (ii) the disordered carbon forms remaining in the graphitized samples. In addition, by coupling HRTEM with energy-dispersive spectroscopy, the transformations with the temperature of the inorganic matter (mainly iron- and silicon-based phases) of the unburned carbon concentrates were evidenced. The HRTEM results were compared to the averaged structural order of the materialsmore » as evaluated by X-ray diffraction (XRD) and Raman spectroscopy. As indicated by XRD and Raman parameters, more-ordered materials were obtained from the unburned carbon concentrates with higher mineral/inorganic matter, thus inferring the catalytic effect of some of their components. However, the average character of the information provided by these instrumental techniques seems to be inconclusive in discriminating between carbon structures with different degrees of order (stricto sensu graphite, graphitic, turbostratic, etc.) in a given graphitized unburned carbon. Unlike XRD and Raman, HRTEM is a useful tool for imaging directly the profile of the polyaromatic layers (graphene planes), thus allowing the sample heterogeneity to be looked at, specifically the presence of disordered carbon phases. 49 refs., 9 figs., 3 tabs.« less

  16. Relation between acid dissolution time in the vacuum test tube and time required for graphitization for AMS target preparation

    NASA Astrophysics Data System (ADS)

    Yokoyama, Yusuke; Miyairi, Yousuke; Matsuzaki, Hiroyuki; Tsunomori, Fumiaki

    2007-06-01

    Availability of an effective graphitization system is essential for the successful operation of an AMS laboratory for radiocarbon measurements. We have set up a graphitization system consisting of metal vacuum lines for cleaning CO2 sample gas which is then converted to graphite. CO2 gas from a carbonate sample is produced in vacuum in a test tube by injecting concentrated phosphoric acid. The tube is placed into a heated metal block to accelerate dissolution. However, we have observed systematic differences in the time required to convert the CO2 gas to graphite under a hydrogen atmosphere, from less than 3 h to over 10 h. We have conducted a series of experiments including background measurements and yield measurements to monitor secondary carbon contamination and changes in isotopic fractionation. All of the tests show that the carbon isotope ratios remain unaffected by the duration of the process. We also used a quadrupole mass spectrometer (QMS) to identify possible contaminant gases. Contaminant peaks were identified at high mass (larger than 60) only for long duration experiments. This suggests a possible reaction between the rubber cap and acid fumes producing a contaminant gas that impeded the reduction of CO2.

  17. Wettability of graphitic-carbon and silicon surfaces: MD modeling and theoretical analysis

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

    Ramos-Alvarado, Bladimir; Kumar, Satish; Peterson, G. P.

    2015-07-28

    The wettability of graphitic carbon and silicon surfaces was numerically and theoretically investigated. A multi-response method has been developed for the analysis of conventional molecular dynamics (MD) simulations of droplets wettability. The contact angle and indicators of the quality of the computations are tracked as a function of the data sets analyzed over time. This method of analysis allows accurate calculations of the contact angle obtained from the MD simulations. Analytical models were also developed for the calculation of the work of adhesion using the mean-field theory, accounting for the interfacial entropy changes. A calibration method is proposed to providemore » better predictions of the respective contact angles under different solid-liquid interaction potentials. Estimations of the binding energy between a water monomer and graphite match those previously reported. In addition, a breakdown in the relationship between the binding energy and the contact angle was observed. The macroscopic contact angles obtained from the MD simulations were found to match those predicted by the mean-field model for graphite under different wettability conditions, as well as the contact angles of Si(100) and Si(111) surfaces. Finally, an assessment of the effect of the Lennard-Jones cutoff radius was conducted to provide guidelines for future comparisons between numerical simulations and analytical models of wettability.« less

  18. Gas Evolution in Operating Lithium-Ion Batteries Studied In Situ by Neutron Imaging

    PubMed Central

    Michalak, Barbara; Sommer, Heino; Mannes, David; Kaestner, Anders; Brezesinski, Torsten; Janek, Jürgen

    2015-01-01

    Gas generation as a result of electrolyte decomposition is one of the major issues of high-performance rechargeable batteries. Here, we report the direct observation of gassing in operating lithium-ion batteries using neutron imaging. This technique can be used to obtain qualitative as well as quantitative information by applying a new analysis approach. Special emphasis is placed on high voltage LiNi0.5Mn1.5O4/graphite pouch cells. Continuous gassing due to oxidation and reduction of electrolyte solvents is observed. To separate gas evolution reactions occurring on the anode from those associated with the cathode interface and to gain more insight into the gassing behavior of LiNi0.5Mn1.5O4/graphite cells, neutron experiments were also conducted systematically on other cathode/anode combinations, including LiFePO4/graphite, LiNi0.5Mn1.5O4/Li4Ti5O12 and LiFePO4/Li4Ti5O12. In addition, the data were supported by gas pressure measurements. The results suggest that metal dissolution in the electrolyte and decomposition products resulting from the high potentials adversely affect the gas generation, particularly in the first charge cycle (i.e., during graphite solid-electrolyte interface layer formation). PMID:26496823

  19. Graphite intercalated polyaniline composite with superior anticorrosive and hydrophobic properties, as protective coating material on steel surfaces

    NASA Astrophysics Data System (ADS)

    Rathnayake, R. M. N. M.; Mantilaka, M. M. M. G. P. G.; Hara, Masanori; Huang, Hsin-Hui; Wijayasinghe, H. W. M. A. C.; Yoshimura, Masamichi; Pitawala, H. M. T. G. A.

    2017-07-01

    Solid polymer composite systems are widely being used for potential technological applications in secondary energy sources and electrochromic devices. In this study, we synthesized and characterized a composite material composed of polyaniline (PANI) and natural needle platy (NPG) vein graphite. Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), cyclic voltammetry (CV), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), micro-Raman analysis, thermogravimetric and differential thermal analysis (TGA/DTA), transmission electron microscopy (TEM) were used to study the structural and electrochemical properties of the prepared PANI/NPG graphite composite. XPS, FTIR, and micro-Raman analysis confirmed the existence of relevant functional groups and bonding in the prepared PANI/NPG composite material. The composite shows a very low corrosion rate, approximately 29 μm per year, and high hydrophobicity on steel surfaces, which helps to prevent the corrosion due to O2 penetration towards the metal surface. It indicates that the composite can be used as a high potential surface coating material to anticorrosion. The specific capacitance of PANI/NPG composite is 833.3 F g-1, which is higher than that of PANI. This synergistic electrical performance result proves the prepared PANI/NPG graphite composite as a suitable protective coating material for steel surfaces.

  20. Graphite as a Biomarker in Rocks of the 3.8 Ga Isua Supracrustal Belt

    NASA Astrophysics Data System (ADS)

    Lepland, A.; van Zuilen, M.; Layne, G. D.; Arrhenius, G.

    2002-12-01

    Recent petrographic and isotopic studies of graphite and apatite in supracrustal rocks from the 3.8 Ga Isua belt (ISB) in southern West Greenland [1, 2] have shown inconsistencies in interpreting traces of life in the earliest terrestrial sediment record. Isotopically light graphitic carbon, suggestive of a bioorganic origin, has been previously reported from the carbonate-rich Isua rocks [3, 4] that at the time were recognized as sedimentary deposits. However, these carbonate-rich rocks, that provided the basis for original biologic interpretations, have been shown to have a metasomatic origin [5] not sedimentary as previously believed. This protolith reinterpretation has highlighted the need for assessment of graphite genesis and related isotopic systematics when using graphite as an ancient biomarker. We have, for this purpose, studied graphite in a suite of samples from the ISB including metacarbonates, turbidites, cherts and banded iron formations (BIFs). Graphite is relatively abundant (0.1-2 wt. %) in metacarbonate samples, while the abundances of reduced carbon in metasedimentary BIFs and metacherts are below 100 ppm. Petrographic analyses show that graphite in metacarbonates typically associates with Fe-bearing carbonate and magnetite. This mineral association indicates graphite formation in Isua metacarbonates by thermal-metamorphic reduction of carbonate ion, in which the carbonate ion is reduced to form graphite and ferrous iron is oxidized to form magnetite. Carbon isotopic compositions of graphite (δ13C ca. -2 per mil) and associated Fe-carbonate (δ13C ca. -6 per mil) indicate isotopic equilibrium between these two phases at ca. 500 C, consistent with the metamorphic history of the ISB. Stepped-combustion experiments undertaken on Isua BIFs and metacherts reveal that these sediments contain virtually no graphite, and the small amount of reduced carbon found there represents recent organic contamination. Our stepped-combustion-mass-spectrometry data demonstrate that previous isotopic results on graphite deficient Isua rocks obtained by single step combustion are unreliable. The proposed biologic significance of graphite occurring as inclusions in apatite [4] in Isua rocks is not supported by our findings because such graphite-apatite association can only be found in biologically irrelevant metacarbonate rocks. The isotopic systematics of the epigenetic processes responsible for formation of isotopically light graphite enclosed in apatite crystals [4] will be discussed, integrating new ion microprobe isotope data on graphite in apatite and other mineral phases occurring in Isua metacarbonates. References: [1] van Zuilen, M., Lepland, A. and Arrhenius, G., 2002. Reassessing the evidence for the earliest traces of life. Nature 418: 627-630. [2] Lepland, A., Arrhenius, G. and Cornell, D. in press. Apatite in early Archean Isua supracrustal rocks, southern West Greenland: its origin, association with graphite and potential as a biomarker. Precam. Res. [3] Schidlowski, M., 1988. A 3,800-million-year isotopic record of life from carbon in sedimentary rocks. Nature 333: 313-318. [4] Mojzsis, S.J., Arrhenius, G., McKeegan, K.D., Harrison, T.M., Nutman, A.P. and Friend, C.R.L., 1996. Evidence for life on Earth before 3800 million years ago. Nature 384: 55-59. [5] Rosing, M.T., Rose, N.M., Bridgwater, D. and Thomsen, H.S., 1996. Earliest part of Earth's stratigraphic record: a reappraisal of the >3.7 Ga Isua (Greenland) supracrustal sequence. Geol. 24: 43-46.

  1. Frictional Characteristics of graphene

    NASA Astrophysics Data System (ADS)

    Lee, Changgu; Carpick, Robert; Hone, James

    2009-03-01

    The frictional characteristics of graphene were characterized using friction force microscopy (FFM). The frictional force for monolayer graphene is more than twice that of bulk graphite, with 2,3, and 4 layer samples showing a monotonic decrease in friction with increasing sample thickness. Measurements on suspended graphene membranes show identical results, ruling out substrate effects as the cause of the observed variation. Likewise, the adhesion force is identical for all samples. The frictional force is independent of load within experimental uncertainty, consistent with previous measurements on graphite. We consider several possible explanations for the origin of the observed thickness dependence.

  2. Laser processing for manufacturing nanocarbon materials

    NASA Astrophysics Data System (ADS)

    Van, Hai Hoang

    CNTs have been considered as the excellent candidate to revolutionize a broad range of applications. There have been many method developed to manipulate the chemistry and the structure of CNTs. Laser with non-contact treatment capability exhibits many processing advantages, including solid-state treatment, extremely fast processing rate, and high processing resolution. In addition, the outstanding monochromatic, coherent, and directional beam generates the powerful energy absorption and the resultant extreme processing conditions. In my research, a unique laser scanning method was developed to process CNTs, controlling the oxidation and the graphitization. The achieved controllability of this method was applied to address the important issues of the current CNT processing methods for three applications. The controllable oxidation of CNTs by laser scanning method was applied to cut CNT films to produce high-performance cathodes for FE devices. The production method includes two important self-developed techniques to produce the cold cathodes: the production of highly oriented and uniformly distributed CNT sheets and the precise laser trimming process. Laser cutting is the unique method to produce the cathodes with remarkable features, including ultrathin freestanding structure (~200 nm), greatly high aspect ratio, hybrid CNT-GNR emitter arrays, even emitter separation, and directional emitter alignment. This unique cathode structure was unachievable by other methods. The developed FE devices successfully solved the screening effect issue encounter by current FE devices. The laser-control oxidation method was further developed to sequentially remove graphitic walls of CNTs. The laser oxidation process was directed to occur along the CNT axes by the laser scanning direction. Additionally, the oxidation was further assisted by the curvature stress and the thermal expansion of the graphitic nanotubes, ultimately opening (namely unzipping) the tubular structure to produce GNRs. Therefore the developed laser scanning method optimally exploited the thermal laser-CNT interaction, successfully transforming CNTs into 2D GNRs. The solid-state laser unzipping process effectively addressed the issues of contamination and scalability encountered by the current unzipping methods. Additionally, the produced GNRs were uniquely featured with the freestanding structure and the smooth surfaces. If the scanning process was performed in an inert environment without the appearance of oxygen, the oxidation of CNTs would not happen. Instead, the greatly mobile carbon atoms of the heated CNTs would reorganize the crystal structure, inducing the graphitization process to improve the crystallinity. Many observations showing the structural improvement of CNTs under laser irradiation has been reported, confirming the capability of laser to heal graphitic defects. Laser methods were more time-efficient and energy-efficient than other annealing methods because laser can quickly heat CNTs to generate graphitization in less than one second. This subsecond heating process of laser irradiation was more effective than other heating methods because it avoided the undesired coalescence of CNTs. In my research, the laser scanning method was applied to generate the graphitization, healing the structural defects of CNTs. Different from the reported laser methods, the laser scanning directed the locally annealed areas to move along the CNT axes, migrating and coalescencing the graphitic defects to achieve better healing results. The critical information describing the CNT structural transformation caused by the moving laser irradiation was explored from the successful applications of the developed laser method. This knowledge inspires an important method to modifiy the general graphitic structure for important applications, such as carbon fiber production, CNT self-assembly process and CNT welding. This method will be effective, facile, versatile, and adaptable for laboratory and industrial facilities.

  3. Ag induced electromagnetic interference shielding of Ag-graphite/PVDF flexible nanocomposites thinfilms

    NASA Astrophysics Data System (ADS)

    Kumaran, R.; Alagar, M.; Dinesh Kumar, S.; Subramanian, V.; Dinakaran, K.

    2015-09-01

    We report Ag nanoparticle induced Electromagnetic Interference (EMI) shielding in a flexible composite films of Ag nanoparticles incorporated graphite/poly-vinylidene difluoride (PVDF). PVDF nanocomposite thin-films were synthesized by intercalating Ag in Graphite (GIC) followed by dispersing GIC in PVDF. The X-ray diffraction analysis and the high-resolution transmission electron microscope clearly dictate the microstructure of silver nanoparticles in graphite intercalated composite of PVDF matrix. The conductivity values of nanocomposites are increased upto 2.5 times when compared to neat PVDF having a value of 2.70 S/cm at 1 MHz. The presence of Ag broadly enhanced the dielectric constant and lowers the dielectric loss of PVDF matrix proportional to Ag content. The EMI shielding effectiveness of the composites is 29.1 dB at 12.4 GHz for the sample having 5 wt. % Ag and 10 wt. % graphite in PVDF.

  4. Theoretical investigation of magnetic properties in interfaces of magnetic nanoparticles and amorphous carbons

    NASA Astrophysics Data System (ADS)

    Sun, Shih-Jye; Hsu, Hua-Shu; Ovchinnikov, Sergei; Chen, Guan-Long

    2017-06-01

    Based on the experimental finding of the exchange bias in amorphous carbon samples with embedded Co nanoparticles and on the graphited character of the amorphous carbon interface confirmed by molecular dynamics simulations we have proposed the interface of graphited carbon to be antiferromagnetic. A theoretical model, which comprises the Kondo interactions in the interfaces of Co nanoparticles and the induced antiferromagnetic interactions in the graphited carbons, is employed to evaluate the ferromagnetism of the interfaces of Co nanoparticles. We have shown that the ferromagnetism of interfaces of Co nanoparticles will be enhanced by the increase of antiferromagnetic interaction as well as the increase of electron density in the graphited carbons. In particular, we found that the antiferromagnetic interactions in graphited carbons will change the spin-wave excitation in interfaces of Co nanoparticles from the quasiacoustic mode to the quasioptical one.

  5. On the Application of Lithium Additives in the Electrolytic Production of Primary Aluminum

    NASA Astrophysics Data System (ADS)

    Saitov, A. V.; Bazhin, V. Yu.; Povarov, V. G.

    2017-12-01

    The behavior of carbon-graphite subjected to treatment in the lithium carbonate Li2CO3 melt without cryolite and alkali-metal fluorides is studied to reliably estimate the influence of lithium on the surface layers of a carbon-containing cathode lining. The chemical composition and the structure of the carbon-graphite material after its interaction with lithium in the Li2CO3 melt have been studied. The high-temperature interaction of the system components in the melt is found to be accompanied by fracture of the operating surface of the carbon-graphite material, while the carbon-graphite surface does not failed upon interacting with lithium vapors. Based on the obtained data, a model for the formation of lithium ions during the reduction of lithium and its interaction with a carbon-graphite sample during the electrolysis of lithium carbonate is proposed.

  6. New Experimental Technique for Nodularity and Mg Fading Control in Compacted Graphite Iron Production on Laboratory Scale

    NASA Astrophysics Data System (ADS)

    Hernando, Juan Carlos; Domeij, Björn; González, Daniel; Amieva, José Manuel; Diószegi, Attila

    2017-11-01

    The narrow production window for compacted graphite iron material (CGI) drastically reduces the possibilities to produce it in small batches outside an industrial environment. This fact hinders laboratory-scale investigations on CGI solidification. This work presents a solution to that issue by introducing an experimental technique to produce graphitic cast iron of the main three families. Samples of a base hypereutectic spheroidal graphite iron (SGI) were re-melted in a resistance furnace under Ar atmosphere. Varying the holding time at 1723 K (1450 °C), graphitic irons ranging from spheroidal to lamellar were produced. Characterization of the graphite morphology evolution, in terms of nodularity as a function of holding time, is presented. The nodularity decay for the SGI region suggests a linear correlation with the holding time. In the CGI region, nodularity deterioration shows a slower rate, concluding with the sudden appearance of lamellar graphite. The fading process of magnesium, showing agreement with previous researchers, is described by means of empirical relations as a function of holding time and nodularity. The results on nodularity fade and number of nodules per unit area fade suggest that both phenomena occur simultaneously during the fading process of magnesium.

  7. Molecular dynamics simulations of shock compressed heterogeneous materials. II. The graphite/diamond transition case for astrophysics applications

    NASA Astrophysics Data System (ADS)

    Pineau, N.; Soulard, L.; Colombet, L.; Carrard, T.; Pellé, A.; Gillet, Ph.; Clérouin, J.

    2015-03-01

    We present a series of molecular dynamics simulations of the shock compression of copper matrices containing a single graphite inclusion: these model systems can be related to some specific carbon-rich rocks which, after a meteoritic impact, are found to contain small fractions of nanodiamonds embedded in graphite in the vicinity of high impedance minerals. We show that the graphite to diamond transformation occurs readily for nanometer-sized graphite inclusions, via a shock accumulation process, provided the pressure threshold of the bulk graphite/diamond transition is overcome, independently of the shape or size of the inclusion. Although high diamond yields (˜80%) are found after a few picoseconds in all cases, the transition is non-isotropic and depends substantially on the relative orientation of the graphite stack with respect to the shock propagation, leading to distinct nucleation processes and size-distributions of the diamond grains. A substantial regraphitization process occurs upon release and only inclusions with favorable orientations likely lead to the preservation of a fraction of this diamond phase. These results agree qualitatively well with the recent experimental observations of meteoritic impact samples.

  8. Braze Development of Graphite Fiber for Use in Phase Change Material Heat Sinks

    NASA Technical Reports Server (NTRS)

    Quinn, Gregory; Gleason, Brian; Beringer, Woody; Stephen, Ryan

    2010-01-01

    Hamilton Sundstrand (HS), together with NASA Johnson Space Center, developed methods to metallurgically join graphite fiber to aluminum. The goal of the effort was to demonstrate improved thermal conductance, tensile strength and manufacturability compared to existing epoxy bonded techniques. These improvements have the potential to increase the performance and robustness of phase change material heat sinks that use graphite fibers as an interstitial material. Initial work focused on evaluating joining techniques from 4 suppliers, each consisting of a metallization step followed by brazing or soldering of one inch square blocks of Fibercore graphite fiber material to aluminum end sheets. Results matched the strength and thermal conductance of the epoxy bonded control samples, so two suppliers were down-selected for a second round of braze development. The second round of braze samples had up to a 300% increase in strength and up to a 132% increase in thermal conductance over the bonded samples. However, scalability and repeatability proved to be significant hurdles with the metallization approach. An alternative approach was pursued which used nickel and active braze allows to prepare the carbon fibers for joining with aluminum. This approach was repeatable and scalable with improved strength and thermal conductance when compared with epoxy bonding.

  9. In-situ pre-concentration through repeated sampling and pyrolysis for ultrasensitive determination of thallium in drinking water by electrothermal atomic absorption spectrometry.

    PubMed

    Liu, Liwei; Zheng, Huaili; Xu, Bincheng; Xiao, Lang; Chigan, Yong; Zhangluo, Yilan

    2018-03-01

    In this paper, a procedure for in-situ pre-concentration in graphite furnace by repeated sampling and pyrolysis is proposed for the determination of ultra-trace thallium in drinking water by graphite furnace atomic absorption spectrometry (GF-AAS). Without any other laborious enrichment processes that routinely result in analyte loss and contamination, thallium was directly concentrated in the graphite furnace automatically and subsequently subject to analysis. The effects of several key factors, such as the temperature for pyrolysis and atomization, the chemical modifier, and the repeated sampling times were investigated. Under the optimized conditions, a limit of detection of 0.01µgL -1 was obtained, which fulfilled thallium determination in drinking water by GB 5749-2006 regulated by China. Successful analysis of thallium in certified water samples and drinking water samples was demonstrated, with analytical results in good agreement with the certified values and those by inductively coupled plasma mass spectrometry (ICP-MS), respectively. Routine spike-recovery tests with randomly selected drinking water samples showed satisfactory results of 80-96%. The proposed method is simple and sensitive for screening of ultra-trace thallium in drinking water samples. Copyright © 2017. Published by Elsevier B.V.

  10. Burn/Blast Tests of Miscellaneous Graphite Composite Parts.

    DTIC Science & Technology

    1979-11-01

    accommodate the size of the test fixture sample holder. The QCSEE fan blade consisted of various layers of KEVLAR (polyaramid fiber), S-glass, AS graphite...panel tested was a 14-ply laminate of W-134 graphite and MXG 6070 modified phenolic resin. This was an experimental formulation pro- posed as an...166/X-130 T-Section T-300/5209 epoxy 17 x 26 20 1122 skin-to-spar ST-163/X-127 QCSEE Kevlar /AS/Glass/B/PR 24 x 29 20 1204 fan blade BT-164/X-128 Le1C

  11. Mechanosynthesis of Precursors for TiC-Cu Cermets

    NASA Astrophysics Data System (ADS)

    Eremina, M. A.; Lomaeva, S. F.; Burnyshev, I. N.; Kalyuzhnyi, D. G.

    2018-04-01

    The structural and phase state of the samples obtained by co-grinding of Ti and Cu powders under different conditions (with graphite, in petroleum ether, and in xylene) is investigated. It is demonstrated that after thermal treatment of powders obtained by milling of titanium, copper, and graphite in petroleum ether, both cubic titanium carbide and hexagonal titanium carbohydride are formed, whereas by milling without graphite, only hexagonal carbohydride possessing high thermal stability is formed. CuTi and CuTi2 intermetallic phases are formed under all examined conditions of mechanosynthesis.

  12. Determination of As in tobacco by using electrochemical hydride generation at a Nafion® solid polymer electrolyte cell hyphenated with atomic fluorescence spectrometry

    NASA Astrophysics Data System (ADS)

    Yang, Qinghua; Gan, Wuer; Deng, Yun; Sun, Huihui

    2011-11-01

    In the present work, a novel solid polymer electrolyte hydride generation (SPE-HG) cell was developed. The home-made SPE-HG cell, mainly composed of three components (Nafion®117 membrane for separating and H + exchanging, a soft graphite felt cathode and a Ti mesh modified by Ir anode), was employed for detecting As by coupling to atomic fluorescence spectrometry (AFS). The H + generated by electrolysis of pure water in anode chamber transferred to cathode chamber through SPE, and immediately reacted with As 3 + to generate AsH 3. The relative mechanisms and operation conditions for hydride generation of As were investigated in detail. The developed cell employed water as an alternative of acid anolyte, with virtues of low-cost, more than 6 months lifetime and environment friendly compared with the conventional cell. Under the optimized conditions, the limit of determination of As 3 + for sample blank solution was 0.12 μg L - 1 , the RSD was 2.9% for 10 consecutive measurements of 5 μg L - 1 As 3 + standard solution. The accuracy of the method was verified by the determination of As in the reference Tea (GBW07605) and the developed method was successfully applied to determine trace amounts of As in tobacco samples with recovery from 97% to 103%.

  13. Ionic liquid-assisted multiwalled carbon nanotube-dispersive micro-solid phase extraction for sensitive determination of inorganic As species in garlic samples by electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Grijalba, Alexander Castro; Escudero, Leticia B.; Wuilloud, Rodolfo G.

    2015-08-01

    A highly sensitive dispersive micro-solid phase extraction (D-μ-SPE) method combining an ionic liquid (IL) and multi-walled carbon nanotubes (MWCNTs) for inorganic As species (As(III) and As(V)) species separation and determination in garlic samples by electrothermal atomic absorption spectrometry (ETAAS) was developed. Trihexyl(tetradecil)phosphonium chloride IL was used to form an ion pair with the arsenomolybdate complex obtained by reaction of As(V) with molybdate ion. Afterwards, 1.0 mg of MWCNTs was dispersed for As(V) extraction and the supernatant was separated by centrifugation. MWCNTs were re-dispersed with tetradecyltrimethylammonium bromide surfactant and ultrasound followed by direct injection into the graphite furnace of ETAAS for As determination. Pyrolysis and atomization conditions were carefully studied for complete decomposition of MWCNTs and IL matrices. Under optimum conditions, an extraction efficiency of 100% and a preconcentration factor of 70 were obtained with 5 mL of garlic extract. The detection limit was 7.1 ng L- 1 and the relative standard deviations (RSDs) for six replicate measurements at 5 μg L- 1 of As were 5.4% and 4.8% for As(III) and As(V), respectively. The proposed D-μ-SPE method allowed the efficient separation and determination of inorganic As species in a complex matrix such as garlic extract.

  14. [Determination of perfluoroalkyl acids in lamb liver by high performance liquid chromatography- tandem mass spectrometry combined with dispersive solid phase extraction].

    PubMed

    Zhu, Pingping; Yue, Zhenfeng; Zheng, Zongkun; Zhang, Yi; Li, Wenyin; Zhao, Fengjuan; Xiao Chengui; Bai, Runye; Lin, Wei

    2015-05-01

    A method was developed for the determination of 19 perfluoroalkyl acids (PFAs) in lamb liver by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/ MS) combined with dispersive solid phase extraction. The sample was extracted with acidified acetonitrile, and then cleaned-up by a mixture of N-propylethylenediamine (PSA), C18 and graphitized carbon black (GCB) sorbents. The 19 PFAs were analyzed by HPLC-MS/MS with a C18 chromatographic column, adopting the multiple reaction monitoring (MRM) mode with negative electrospray ionization. The effects of the dosages of hydrochloric acid and the sorbents on the recoveries of the 19 PFAs were studied. For accurate quantitative analysis, the isotope internal standard method was used. The calibration curves were linear with the correlation coefficients over 0.998 in the range of 0.05-20 µg/kg for the 19 PFAs. The limits of detection were 0.004-0.111 µg/kg. The limits of quantification were 0.012-0.370 µg/kg. The mean recoveries of the 19 PFAs at spiked levels of 0.5, 1.0, 2.0 µg/kg were in the range from 80% to 128% with the relative standard deviations of 0.31%-11.1%. The developed method is rapid, simple, accurate. It is suitable for the determination of the 19 PFAs in large quantities of lamb liver samples.

  15. Characterization of Austempered Ferritic Ductile Iron

    NASA Astrophysics Data System (ADS)

    Dakre, Vinayak S.; Peshwe, D. R.; Pathak, S. U.; Likhite, A. A.

    2018-04-01

    The ductile iron (DI) has graphite nodules enclose in ferrite envelop in pearlitic matrix. The pearlitic matrix in DI was converted to ferritic matrix through heat treatment. This heat treatment includes austenitization of DI at 900°C for 1h, followed by furnace cooling to 750°C & hold for 1h, then again furnace cooling to 690°C hold for 2h, then samples were allowed to cool in furnace. The new heat treated DI has graphite nodules in ferritic matrix and called as ferritic ductile iron (FDI). Both DIs were austenitized at 900°C for 1h and then quenched into salt bath at 325°C. The samples were soaked in salt bath for 60, 120, 180, 240 and 300 min followed by air cooling. The austempered samples were characterized with help of optical microscopy, SEM and X-ray diffraction analysis. Austempering of ferritic ductile iron resulted in finer ausferrite matrix as compared to ADI. Area fraction of graphite, ferrite and austenite were determining using AXIOVISION-SE64 software. Area fraction of graphite was more in FDI than that of as cast DI. The area fraction of graphite remains unaffected due to austempering heat treatment. Ausferritic matrix coarsened (feathered) with increasing in austempering time for both DI and FDI. Bulk hardness test was carried on Rockwell Hardness Tester with load of 150 kgf and diamond indenter. Hardness obtained in as cast DI is 28 HRC which decreased to 6 HRC in FDI due conversion of pearlitic matrix to ferritic matrix. Hardness is improved by austempering process.

  16. Progress Towards Microwave Ignition of Explosives

    NASA Astrophysics Data System (ADS)

    Curling, Mark; Collins, Adam; Dima, Gabriel; Proud, William

    2009-06-01

    Microwaves could provide a method of propellant ignition that does away with a traditional primer, making ammunition safer and suitable for Insensitive Munitions (IM) applications. By embedding a suitable material inside a propellant, it is postulated that microwaves could be used to stimulate hotspots, through direct heating or electrostatic discharge (arcing) across the energetic material. This paper reports on progress in finding these suitable materials. Graphite rod, magnetite cubes and powders of graphite, aluminium, copper oxide, and iron were irradiated in a conventional microwave oven. Temperature measurements were made using a shielded thermocouple and thermal paints. Only graphite rod and magnetite showed significant heating upon microwave exposure. The light output from arcing of iron, steel, iron pyrite, magnetite and graphite was measured in the same microwave oven as above. Sample mass and shape were correlated with arcing intensity. A strategy is proposed to create a homogeneous igniter material by embedding arcing materials within an insulator, Polymethylpentene (TPX). External discharges were transmitted through TPX, however no embedded samples were successful in generating an electrical breakdown suitable for propellant ignition.

  17. Determination of Chlorine in Milk via Molecular Absorption of SrCl Using High-Resolution Continuum Source Graphite Furnace Atomic Absorption Spectrometry.

    PubMed

    Ozbek, Nil; Akman, Suleyman

    2016-07-20

    Total chlorine in milk was determined via the molecular absorption of diatomic strontium monochloride at 635.862 nm using high-resolution continuum source graphite furnace atomic absorption spectrometry. The effects of coating the graphite furnace, using different modifiers, amount of molecule-forming element, and different calibrants were investigated and optimized. Chlorine concentrations in milk samples were determined in a Zr-coated graphite furnace using 25 μg of Sr as the molecule-forming reagent and applying a pyrolysis temperature of 600 °C and a molecule-forming temperature of 2300 °C. Linearity was maintained up to 500 μg mL(-1) of Cl. The method was tested by analyzing a certified reference wastewater. The results were in the uncertainty limits of the certified value. The limit of detection of the method was 1.76 μg mL(-1). The chlorine concentrations in various cow milk samples taken from the market were found in the range of 588-1472 mg L(-1).

  18. Swift heavy ion-induced radiation damage in isotropic graphite studied by micro-indentation and in-situ electrical resistivity

    NASA Astrophysics Data System (ADS)

    Hubert, Christian; Voss, Kay Obbe; Bender, Markus; Kupka, Katharina; Romanenko, Anton; Severin, Daniel; Trautmann, Christina; Tomut, Marilena

    2015-12-01

    Due to its excellent thermo-physical properties and radiation hardness, isotropic graphite is presently the most promising material candidate for new high-power ion accelerators which will provide highest beam intensities and energies. Under these extreme conditions, specific accelerator components including production targets and beam protection modules are facing the risk of degradation due to radiation damage. Ion-beam induced damage effects were tested by irradiating polycrystalline, isotropic graphite samples at the UNILAC (GSI, Darmstadt) with 4.8 MeV per nucleon 132Xe, 150Sm, 197Au, and 238U ions applying fluences between 1 × 1011 and 1 × 1014 ions/cm2. The overall damage accumulation and its dependence on energy loss of the ions were studied by in situ 4-point resistivity measurements. With increasing fluence, the electric resistivity increases due to disordering of the graphitic structure. Irradiated samples were also analyzed off-line by means of micro-indentation in order to characterize mesoscale effects such as beam-induced hardening and stress fields within the specimen. With increasing fluence and energy loss, hardening becomes more pronounced.

  19. SEM/XPS analysis of fractured adhesively bonded graphite fibre-reinforced polyimide composites

    NASA Technical Reports Server (NTRS)

    Devilbiss, T. A.; Messick, D. L.; Wightman, J. P.; Progar, D. J.

    1985-01-01

    The surfaces of the graphite fiber-reinforced polyimide composites presently pretreated prior to bonding with polyimide adhesive contained variable amounts of a fluoropolymer, as determined by X-ray photoelectron spectroscopy. Lap shear strengths were determined for unaged samples and for those aged over 500- and 1000-hour periods at 177 and 232 C. Unaged sample lap strengths, which were the highest obtained, exhibited no variation with surface pretreatment, but a significant decrease is noted with increasing aging temperature. These thermally aged samples, however, had increased surface fluorine concentration, while a minimal concentration was found in unaged samples. SEM demonstrated a progressive shift from cohesive to adhesive failure for elevated temperature-aged composites.

  20. Investigation of Pristine Graphite Oxide as Room-Temperature Chemiresistive Ammonia Gas Sensing Material.

    PubMed

    Bannov, Alexander G; Prášek, Jan; Jašek, Ondřej; Zajíčková, Lenka

    2017-02-09

    Graphite oxide has been investigated as a possible room-temperature chemiresistive sensor of ammonia in a gas phase. Graphite oxide was synthesized from high purity graphite using the modified Hummers method. The graphite oxide sample was investigated using scanning electron microscopy, energy dispersive X-ray spectroscopy, X-ray diffraction, thermogravimetry and differential scanning calorimetry. Sensing properties were tested in a wide range of ammonia concentrations in air (10-1000 ppm) and under different relative humidity levels (3%-65%). It was concluded that the graphite oxide-based sensor possessed a good response to NH₃ in dry synthetic air (ΔR/R₀ ranged from 2.5% to 7.4% for concentrations of 100-500 ppm and 3% relative humidity) with negligible cross-sensitivity towards H₂ and CH₄. It was determined that the sensor recovery rate was improved with ammonia concentration growth. Increasing the ambient relative humidity led to an increase of the sensor response. The highest response of 22.2% for 100 ppm of ammonia was achieved at a 65% relative humidity level.

  1. Heterogeneous photo-Fenton processes using graphite carbon coating hollow CuFe2O4 spheres for the degradation of methylene blue

    NASA Astrophysics Data System (ADS)

    Guo, Xiaojun; Wang, Kebai; Li, Dai; Qin, Jiabin

    2017-10-01

    The novel graphite carbon coating hollow CuFe2O4 spheres were fabricated through solvothermal method and characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Raman spectra, etc. The catalytic performance of the graphite carbon coating hollow CuFe2O4 spheres was evaluated in photo-Fenton-like degradation of methylene blue (MB) using H2O2 as a green oxidant under light irradiation (λ > 400 nm). The results demonstrated that the hollow CuFe2O4 spheres with graphite carbon coating exhibited superior catalytic activity. In the preparation process of catalyst, the addition of glucose was very important to its catalytic performance. Photoresponse analysis of the typical samples proved that CuFe2O4@graphite carbon core-shell hollow spheres possessed excellent photocurrent response and lower electrochemical impedance. In addition, a possible mechanism for photocatalytic degradation of MB had been presumed. Moreover, after five regeneration cycles, the graphite carbon coating hollow CuFe2O4 spheres still exhibited better properties.

  2. Collision-induced light scattering in a thin xenon layer between graphite slabs - MD study.

    PubMed

    Dawid, A; Górny, K; Wojcieszyk, D; Dendzik, Z; Gburski, Z

    2014-08-14

    The collision-induced light scattering many-body correlation functions and their spectra in thin xenon layer located between two parallel graphite slabs have been investigated by molecular dynamics computer simulations. The results have been obtained at three different distances (densities) between graphite slabs. Our simulations show the increased intensity of the interaction-induced light scattering spectra at low frequencies for xenon atoms in confined space, in comparison to the bulk xenon sample. Moreover, we show substantial dependence of the interaction-induced light scattering correlation functions of xenon on the distances between graphite slabs. The dynamics of xenon atoms in a confined space was also investigated by calculating the mean square displacement functions and related diffusion coefficients. The structural property of confined xenon layer was studied by calculating the density profile, perpendicular to the graphite slabs. Building of a fluid phase of xenon in the innermost part of the slot was observed. The nonlinear dependence of xenon diffusion coefficient on the separation distance between graphite slabs has been found. Copyright © 2014. Published by Elsevier B.V.

  3. Use of Guided Acoustic Waves to Assess the Effects of Thermal-Mechanical Cycling on Composite Stiffness

    NASA Technical Reports Server (NTRS)

    Seale, Michael D.; Madaras, Eric I.

    2000-01-01

    The introduction of new, advanced composite materials into aviation systems requires it thorough understanding of the long-term effects of combined thermal and mechanical loading. As part of a study to evaluate the effects of thermal-mechanical cycling, it guided acoustic (Lamb) wave measurement system was used to measure the bending and out-of-plane stiffness coefficients of composite laminates undergoing thermal-mechanical loading. The system uses a pulse/receive technique that excites an antisymmetric Lamb mode and measures the time-of-flight over a wide frequency range. Given the material density and plate thickness, the bending and out-of-plane shear stiffnesses are calculated from a reconstruction of the velocity dispersion curve. A series of 16 and 32-ply composite laminates were subjected to it thermal-mechanical loading profile in load frames equipped with special environmental chambers. The composite systems studied were it graphite fiber reinforced amorphous thermoplastic polyimide and it graphite fiber reinforced bismaleimide thermoset. The samples were exposed to both high and low temperature extremes its well as high and low strain profiles. The bending and out-of-plane stiffnesses for composite sample that have undergone over 6,000 cycles of thermal-mechanical loading are reported. The Lamb wave generated elastic stiffness results have shown decreases of up to 20% at 4,936 loading cycles for the graphite/thermoplastic samples and up to 64% at 4,706 loading cycles for the graphite/thermoset samples.

  4. Anisotropy in thermal conductivity of graphite flakes–SiC{sub p}/matrix composites: Implications in heat sinking design for thermal management applications

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

    Molina, J.M., E-mail: jmmj@ua.es; Departamento de Física Aplicada, Universidad de Alicante, Ap. 99, E-03080 Alicante; Departamento de Química Inorgánica, Universidad de Alicante, Ap. 99, | E-03080 Alicante

    2015-11-15

    Within the frame of heat dissipation for electronics, a very interesting family of anisotropic composite materials, fabricated by liquid infiltration of a matrix into preforms of oriented graphite flakes and SiC particles, has been recently proposed. Aiming to investigate the implications of the inherent anisotropy of these composites on their thermal conductivity, and hence on their potential applications, materials with matrices of Al–12 wt.% Si alloy and epoxy polymer have been fabricated. Samples have been cut at a variable angle with respect to the flakes plane and thermal conductivity has been measured by means of two standard techniques, namely, steadymore » state technique and laser flash method. Experimental results are presented and discussed in terms of current models, from which important technological implications for heat sinking design can be derived. - Highlights: • Anisotropy in thermal conductivity of graphite flakes-based composites is evaluated. • Samples are cut in a direction forming a variable angle with the oriented flakes. • For angles 0° and 90°, thermal conductivity does not depend on sample geometry. • For intermediate angles, thermal conductivity strongly depends on sample geometry. • “Thin” samples must be thicker than 600 μm, “thick” samples must be encapsulated.« less

  5. Microwave plasma chemical synthesis of nanocrystalline carbon film structures and study their properties

    NASA Astrophysics Data System (ADS)

    Bushuev, N.; Yafarov, R.; Timoshenkov, V.; Orlov, S.; Starykh, D.

    2015-08-01

    The self-organization effect of diamond nanocrystals in polymer-graphite and carbon films is detected. The carbon materials deposition was carried from ethanol vapors out at low pressure using a highly non-equilibrium microwave plasma. Deposition processes of carbon film structures (diamond, graphite, graphene) is defined. Deposition processes of nanocrystalline structures containing diamond and graphite phases in different volume ratios is identified. The solid film was obtained under different conditions of microwave plasma chemical synthesis. We investigated the electrical properties of the nanocrystalline carbon films and identified it's from various factors. Influence of diamond-graphite film deposition mode in non-equilibrium microwave plasma at low pressure on emission characteristics was established. This effect is justified using the cluster model of the structure of amorphous carbon. It was shown that the reduction of bound hydrogen in carbon structures leads to a decrease in the threshold electric field of emission from 20-30 V/m to 5 V/m. Reducing the operating voltage field emission can improve mechanical stability of the synthesized film diamond-graphite emitters. Current density emission at least 20 A/cm2 was obtained. Nanocrystalline carbon film materials can be used to create a variety of functional elements in micro- and nanoelectronics and photonics such as cold electron source for emission in vacuum devices, photonic devices, cathodoluminescent flat display, highly efficient white light sources. The obtained graphene carbon net structure (with a net size about 6 μm) may be used for the manufacture of large-area transparent electrode for solar cells and cathodoluminescent light sources

  6. Analytical Simulations of Energy-Absorbing Impact Spheres for a Mars Sample Return Earth Entry Vehicle

    NASA Technical Reports Server (NTRS)

    Billings, Marcus Dwight; Fasanella, Edwin L. (Technical Monitor)

    2002-01-01

    Nonlinear dynamic finite element simulations were performed to aid in the design of an energy-absorbing impact sphere for a passive Earth Entry Vehicle (EEV) that is a possible architecture for the Mars Sample Return (MSR) mission. The MSR EEV concept uses an entry capsule and energy-absorbing impact sphere designed to contain and limit the acceleration of collected samples during Earth impact without a parachute. The spherical shaped impact sphere is composed of solid hexagonal and pentagonal foam-filled cells with hybrid composite, graphite-epoxy/Kevlar cell walls. Collected Martian samples will fit inside a smaller spherical sample container at the center of the EEV's cellular structure. Comparisons were made of analytical results obtained using MSC.Dytran with test results obtained from impact tests performed at NASA Langley Research Center for impact velocities from 30 to 40 m/s. Acceleration, velocity, and deformation results compared well with the test results. The correlated finite element model was then used for simulations of various off-nominal impact scenarios. Off-nominal simulations at an impact velocity of 40 m/s included a rotated cellular structure impact onto a flat surface, a cellular structure impact onto an angled surface, and a cellular structure impact onto the corner of a step.

  7. Continuous Heterogeneous Photocatalysis in Serial Micro-Batch Reactors.

    PubMed

    Pieber, Bartholomäus; Shalom, Menny; Antonietti, Markus; Seeberger, Peter H; Gilmore, Kerry

    2018-01-29

    Solid reagents, leaching catalysts, and heterogeneous photocatalysts are commonly employed in batch processes but are ill-suited for continuous-flow chemistry. Heterogeneous catalysts for thermal reactions are typically used in packed-bed reactors, which cannot be penetrated by light and thus are not suitable for photocatalytic reactions involving solids. We demonstrate that serial micro-batch reactors (SMBRs) allow for the continuous utilization of solid materials together with liquids and gases in flow. This technology was utilized to develop selective and efficient fluorination reactions using a modified graphitic carbon nitride heterogeneous catalyst instead of costly homogeneous metal polypyridyl complexes. The merger of this inexpensive, recyclable catalyst and the SMBR approach enables sustainable and scalable photocatalysis. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. DC graphite arc furnace, a simple system to reduce mixed waste volume

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

    Wittle, J.K.; Hamilton, R.A.; Trescot, J.

    1995-12-31

    The volume of low-level radioactive waste can be reduced by the high temperature in a DC Graphite Arc Furnace. This volume reduction can take place with the additional benefit of having the solid residue being stabilized by the vitrified product produced in the process. A DC Graphite Arc Furnace is a simple system in which electricity is used to generate heat to vitrify the material and thermally decompose any organic matter in the waste stream. Examples of this type of waste are protective clothing, resins, and grit blast materials produced in the nuclear industry. The various Department of Energy (DOE)more » complexes produce similar low-level waste streams. Electro-Pyrolysis, Inc. and Svedala/Kennedy Van Saun are engineering and building small 50-kg batch and up to 3,000 kg/hr continuous feed DC furnaces for the remediation, pollution prevention, and decontamination and decommissioning segments of the treatment community. This process has been demonstrated under DOE sponsorship at several facilities and has been shown to produce stable waste forms from surrogate waste materials.« less

  9. Electrolysis of metal oxides in MgCl2 based molten salts with an inert graphite anode.

    PubMed

    Yuan, Yating; Li, Wei; Chen, Hualin; Wang, Zhiyong; Jin, Xianbo; Chen, George Z

    2016-08-15

    Electrolysis of solid metal oxides has been demonstrated in MgCl2-NaCl-KCl melt at 700 °C taking the electrolysis of Ta2O5 as an example. Both the cathodic and anodic processes have been investigated using cyclic voltammetry, and potentiostatic and constant voltage electrolysis, with the cathodic products analysed by XRD and SEM and the anodic products by GC. Fast electrolysis of Ta2O5 against a graphite anode has been realized at a cell voltage of 2 V, or a total overpotential of about 400 mV. The energy consumption was about 1 kW h kgTa(-1) with a nearly 100% Ta recovery. The cathodic product was nanometer Ta powder with sizes of about 50 nm. The main anodic product was Cl2 gas, together with about 1 mol% O2 gas and trace amounts of CO. The graphite anode was found to be an excellent inert anode. These results promise an environmentally-friendly and energy efficient method for metal extraction by electrolysis of metal oxides in MgCl2 based molten salts.

  10. Monolayer Adsorption of Ar and Kr on Graphite: Theoretical Isotherms and Spreading Pressures

    PubMed

    Mulero; Cuadros

    1997-02-01

    The validity of analytical equations for two-dimensional fluids in the prediction of monolayer adsorption isotherms and spreading pressures of rare gases on graphite is analyzed. The statistical mechanical theory of Steele is used to relate the properties of the adsorbed and two-dimensional fluids. In such theory the model of graphite is a perfectly flat surface, which means that only the first order contribution of the fluid-solid interactions are taken into account. Two analytical equations for two-dimensional Lennard-Jones fluids are used: one proposed by Reddy-O'Shea, based in the fit on pressure and potential energy computer simulated results, and other proposed by Cuadros-Mulero, based in the fit of the Helmholtz free energy calculated from computer simulated results of the radial distribution function. The theoretical results are compared with experimental results of Constabaris et al. (J. Chem. Phys. 37, 915 (1962)) for Ar and of Putnam and Fort (J. Phys. Chem. 79, 459 (1975)) for Kr. Good agreement is found using both equations in both cases.

  11. Multilayer graphane synthesized under high hydrogen pressure

    DOE PAGES

    Antonov, V. E.; Bashkin, I. O.; Bazhenov, A. V.; ...

    2015-12-19

    A new hydrocarbon – hydrographite – with the composition close to CH is shown to form from graphite and gaseous hydrogen at pressures above 2 GPa and temperatures from 450 to 700 °C. Hydrographite is a black solid thermally stable under ambient conditions. When heated in vacuum, it decomposes into graphite and molecular hydrogen at temperatures from 500 to 650 °C. Powder X-ray diffraction characterizes hydrographite as a multilayer “graphane II” phase predicted by ab initio calculations [Wen X-D et al. PNAS 2011; 108:6833] and consisting of graphane sheets in the chair conformation stacked along the hexagonal c axis inmore » the -ABAB- sequence. The crystal structure of the synthesized phase belongs to the P63mc space group. Moreover, the unit cell parameters are a = 2.53(1) Å and c = 9.54(1) Å and therefore exceed the corresponding parameters of graphite by 2.4(2)% and 42.0(3)%. Stretching vibrations of C–H groups on the surface of the hydrographite particles are examined by infrared spectroscopy.« less

  12. Interaction of the high energy deuterons with the graphite target in the plasma focus devices based on Lee model

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

    Akel, M., E-mail: pscientific2@aec.org.sy; Alsheikh Salo, S.; Ismael, Sh.

    2014-07-15

    Numerical experiments are systematically carried out using the Lee model code extended to compute the ion beams on various plasma focus devices operated with Deuterium gas. The deuteron beam properties of the plasma focus are studied for low and high energy plasma focus device. The energy spectral distribution for deuteron ions ejected from the pinch plasma is calculated and the ion numbers with energy around 1 MeV is then determined. The deuteron–graphite target interaction is studied for different conditions. The yield of the reaction {sup 12}C(d,n){sup 13}N and the induced radioactivity for one and multi shots plasma focus devices in themore » graphite solid target is investigated. Our results present the optimized high energy repetitive plasma focus devices as an alternative to accelerators for the production of {sup 13}N short lived radioisotopes. However, technical challenges await solutions on two fronts: (a) operation of plasma focus machines at high rep rates for a sufficient period of time (b) design of durable targets that can take the thermal load.« less

  13. Pechini process-derived tin oxide and tin oxide-graphite composites for lithium-ion batteries

    NASA Astrophysics Data System (ADS)

    Zhang, R.; Lee, Jim Y.; Liu, Z. L.

    The Pechini process [Ceram. Bull. 68 (1989) 1002] is used to obtain fine tin oxide powders that reduce the specific volume change in Li + insertion and extraction reactions. The suitability of these tin oxides as active materials for negative electrodes in lithium-ion batteries is investigated. From elemental analysis, it is found that the templating polymer network is almost completely obliterated after heating at 500 °C. The best tin oxide does not exhibit extensive crystallization of tin atoms even after 30 cycles of alloying and de-alloying reactions with Li. The structure and the specific capacity of the oxides are dependent on the heat treatment and remnants of the polymeric CH network can impose an unfavorable outcome. A capacity of 600 mAh g -1, which is unchanged for 30 cycles, can be obtained from tin oxide heat treated at 1000 °C. Composites of graphite and SnO 2 are also prepared and exhibit synergistic interactions between graphite and tin oxide which are similar to those reported previously [Electrochem. Solid State Lett. 3 (2000) 167].

  14. Drawing Sensors with Ball-Milled Blends of Metal-Organic Frameworks and Graphite

    PubMed Central

    Ko, Michael; Aykanat, Aylin; Smith, Merry K.

    2017-01-01

    The synthetically tunable properties and intrinsic porosity of conductive metal-organic frameworks (MOFs) make them promising materials for transducing selective interactions with gaseous analytes in an electrically addressable platform. Consequently, conductive MOFs are valuable functional materials with high potential utility in chemical detection. The implementation of these materials, however, is limited by the available methods for device incorporation due to their poor solubility and moderate electrical conductivity. This manuscript describes a straightforward method for the integration of moderately conductive MOFs into chemiresistive sensors by mechanical abrasion. To improve electrical contacts, blends of MOFs with graphite were generated using a solvent-free ball-milling procedure. While most bulk powders of pure conductive MOFs were difficult to integrate into devices directly via mechanical abrasion, the compressed solid-state MOF/graphite blends were easily abraded onto the surface of paper substrates equipped with gold electrodes to generate functional sensors. This method was used to prepare an array of chemiresistors, from four conductive MOFs, capable of detecting and differentiating NH3, H2S and NO at parts-per-million concentrations. PMID:28946624

  15. A biosensor based on graphite epoxy composite electrode for aspartame and ethanol detection.

    PubMed

    Kirgöz, Ulkü Anik; Odaci, Dilek; Timur, Suna; Merkoçi, Arben; Alegret, Salvador; Beşün, Nurgün; Telefoncu, Azmi

    2006-06-16

    A gelatin membrane with carboxyl esterase and alcohol oxidase was subsequently integrated onto the surface of a graphite epoxy composite electrode (GECE). The developed biosensors showed linearity in the range of 2.5-400 microM for aspartame and 2.5-25 microM for ethanol with response times of 170 and 70s for each analyte, respectively. The resulting bienzyme biosensor was used for aspartame detection in diet coke samples and ethanol detection in beer and wine samples. From the obtained results, it can be concluded that the developed biosensor is a selective, practical and economic tool for aspartame and ethanol detection in real samples.

  16. Trace metal assay of U(3)O(8) powder by electrothermal AAS.

    PubMed

    Page, A G; Godbole, S V; Kulkarni, M J; Porwal, N K; Shelar, S S; Joshi, B D

    1983-10-01

    Methods have been developed for the direct determination of Ag, Ca, K., Li, Mg, Na, Pb, Sn and Zn in U(3)O(8) powder samples by electrothermal AAS. Nanogram and lower amounts of these elements have been determined with a relative standard deviation of 6-16% in mg amounts of sample (either alone or mixed with an equal weight of graphite). The results for NBL reference samples were in reasonable agreement with the certified values. X-Ray diffraction studies on the residues left from the graphite mixtures after the atomization cycle, confirmed the formation of uranium carbide (UC(2)).

  17. Analysis of Graphite-Reinforced Cementitious Composites

    NASA Technical Reports Server (NTRS)

    Vaughan, R. E.

    2002-01-01

    Strategically embedding graphite meshes in a compliant cementitious matrix produces a composite material with relatively high tension and compressive properties as compared to steel-reinforced structures fabricated from a standard concrete mix. Although these composite systems are somewhat similar, the methods used to analyze steel-reinforced composites often fail to characterize the behavior of their more advanced graphite-reinforced counterparts. This Technical Memorandum describes some of the analytical methods being developed to determine the deflections and stresses in graphite-reinforced cementitious composites. It is initially demonstrated that the standard transform section method fails to provide accurate results when the elastic moduli ratio exceeds 20. An alternate approach is formulated by using the rule of mixtures to determine a set of effective material properties for the composite. Tensile tests are conducted on composite samples to verify this approach. When the effective material properties are used to characterize the deflections of composite beams subjected to pure bending, an excellent agreement is obtained. Laminated composite plate theory is investigated as a means for analyzing even more complex composites, consisting of multiple graphite layers oriented in different directions. In this case, composite beams are analyzed using the laminated composite plate theory with material properties established from tensile tests. Then, finite element modeling is used to verify the results. Considering the complexity of the samples, a very good agreement is obtained.

  18. Electrical and galvanomagnetic properties of nanoporous carbon samples impregnated with bromine

    NASA Astrophysics Data System (ADS)

    Danishevskii, A. M.; Popov, V. V.; Kyutt, R. N.; Gordeev, S. K.

    2013-07-01

    Nanoporous carbon samples with a large specific surface area can be filled with heavier elements or their compounds, which makes it possible to investigate the interaction of their electronic subsystems with carbon. One of the elements convenient for filling pores of carbon materials is bromine. Impregnation of nanoporous carbon samples with bromine causes the occurrence of the processes of micropore filling, monolayer adsorption, and intercalation. It has been found that samples impregnated with bromine substantially change their electrical and galvanomagnetic properties, and these changes depend on the structure of the samples. It has been shown that, if in the skeleton of a porous carbon sample there is a fraction of graphite clusters, the impregnation of the sample with bromine increases the concentration of charged carriers (holes). But when the sample has a quasi-amorphous structure, the injection of bromine into the sample leads to the appearance of a certain concentration of electrons in addition to charged mobile holes of the initial sample; i.e., the electrical conductivity becomes bipolar. In the former case, bromine molecules intercalate graphite clusters and, since bromine is an acceptor during intercalation of graphite, the hole concentration in the carbon skeleton network increases. In the latter case, bromine molecules can only be adsorbed on pore walls. As a result, the adsorption interaction between the electron shells of bromine molecules and the carbon surface leads to the formation of a donor layer near the surface and to the generation of electrons in the carbon skeleton network.

  19. Carbon-14 bioassay for decommissioning of Hanford reactors.

    PubMed

    Carbaugh, Eugene H; Watson, David J

    2012-05-01

    The production reactors at the U.S. Department of Energy Hanford Site used large graphite piles as the moderator. As part of long-term decommissioning plans, the potential need for ¹⁴C radiobioassay of workers was identified. Technical issues associated with ¹⁴C bioassay and worker monitoring were investigated, including anticipated graphite characterization, potential intake scenarios, and the bioassay capabilities that may be required to support the decommissioning of the graphite piles. A combination of urine and feces sampling would likely be required for the absorption type S ¹⁴C anticipated to be encountered. However, the concentrations in the graphite piles appear to be sufficiently low that dosimetrically significant intakes of ¹⁴C are not credible, thus rendering moot the need for such bioassay.

  20. Carbon-14 Bioassay for Decommissioning of Hanford Reactors

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

    Carbaugh, Eugene H.; Watson, David J.

    2012-05-01

    The old production reactors at the US Department of Energy Hanford Site used large graphite piles as the moderator. As part of long-term decommissioning plans, the potential need for 14C radiobioassay of workers was identified. Technical issues associated with 14C bioassay and worker monitoring were investigated, including anticipated graphite characterization, potential intake scenarios, and the bioassay capabilities that may be required to support the decommissioning of the graphite piles. A combination of urine and feces sampling would likely be required for the absorption type S 14C anticipated to be encountered. However the concentrations in the graphite piles appear to bemore » sufficiently low that dosimetrically significant intakes of 14C are not credible, thus rendering moot the need for such bioassay.« less

  1. Effect of Graphitic Content on Carbon Supported Catalyst Performance

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

    Patel, Anant; Artyushkova, Kateryna; Atanassov, Plamen

    2011-07-01

    The effect of graphitic content on carbon supported platinum catalysts was investigated in order to investigate its influence on catalyst performance. Four catalysts of varying surface areas and graphitic content were analyzed using XPS, HREELS, and tested using RDE experiments. The catalysts were also heat treated at 150oC and 100%RH as means to uniformly age them. The heat treated samples were analyzed using the same methods to determine what changes had occurred due to this aging process. When compared to the BOL catalysts, heat treated catalysts displayed increased graphitic carbon and platinum metalic content, however they also showed depressed catalyticmore » activity. The primary cause is still under investigation, though it is believed to be related to loss of amorphous carbon content.« less

  2. Research on laser-removal of a deuterium deposit from a graphite sample

    NASA Astrophysics Data System (ADS)

    Kubkowska, M.; Skladnik-Sadowska, E.; Malinowski, K.; Sadowski, M. J.; Rosinski, M.; Gasior, P.

    2014-04-01

    The paper presents experimental results of investigation of a removal of deuterium deposits from a graphite target by means of pulsed laser beams. The sample was a part of the TEXTOR limiter with a deuterium-deposited layer. That target was located in the vacuum chamber, pumped out to 5×10-5 Torr, and it was irradiated with a Nd:YAG laser, which generated 3.5-ns pulses of energy of 0.5 J at λ1 = 1063 nm, or 0.1 J at λ3 = 355 nm.

  3. Graphite fluoride fibers and their applications in the space industry

    NASA Technical Reports Server (NTRS)

    Hung, Ching-Chen; Long, Martin; Dever, Therese

    1990-01-01

    Characterization and potential space applications of graphite fluoride fibers from commercially available graphitized carbon fibers are presented. Graphite fluoride fibers with fluorine to carbon ratios of 0.65 and 0.68 were found to have electrical resistivity values of 10(exp 4) and 10(exp 11) Ohms-cm, respectively, and thermal conductivity values of 24 and 5 W/m-K, respectively. At this fluorine content range, the fibers have tensile strength of 0.25 + or - 0.10 GPa (36 + or - 14 ksi), Young's modulus of 170 + or - 30 GPa (25 + or - 5 Msi). The coefficient of thermal expansion value of a sample with fluorine to carbon ratio of 0.61 was found to be 7 ppm/C. These properties change and approach the graphite value as the fluorine content approach 0. Electrically insulative graphite fluoride fiber is at least five times more thermally conductive than fiberglass. Therefore, it can be used as a heat sinking printed circuit board material for low temperature, long life power electronics in spacecraft. Also, partially fluorinated fiber with tailor-made physical properties to meet the requirements of certain engineering design can be produced. For example, a partially fluorinated fiber could have a predetermined CTE value in -1.5 to 7 ppm/C range and would be suitable for use in solar concentrators in solar dynamic power systems. It could also have a predetermined electrical resistivity value suitable for use as a low observable material. Experimental data indicate that slightly fluorinated graphite fibers are more durable in the atomic oxygen environment than pristine graphite. Therefore, fluorination of graphite used in the construction of spacecraft that would be exposed to the low Earth orbit atomic oxygen may protect defect sites in atomic oxygen protective coatings and therefore decrease the rate of degradation of graphite.

  4. Observation of an Ultrahard Phase of Graphite Quenched from High-pressure

    DTIC Science & Technology

    2011-02-01

    Polycrystalline NaCl at High Pressures and 300 °K. J. Geophys. Res. 1978, 83, 1257–1268. 23. Selvi , E.; Ma, Y.; Askoy, R.; Ertas, A.; White, A. High...Pressure X-ray Diffraction Study of Tungsten Disulfide. J. Phys. Chem. Solids 2006, 67, 2183–2186. 24. Askoy, R.; Ma, Y.; Selvi , E.; Chyu, M. C

  5. A novel metal-organic framework composite MIL-101(Cr)@GO as an efficient sorbent in dispersive micro-solid phase extraction coupling with UHPLC-MS/MS for the determination of sulfonamides in milk samples.

    PubMed

    Jia, Xiuna; Zhao, Pan; Ye, Xiu; Zhang, Lianjun; Wang, Ting; Chen, Qinyu; Hou, Xiaohong

    2017-07-01

    As a novel material, metal-organic framework/graphite oxide (MIL-101(Cr)@GO) has great potential for the pretreatment of trace analytes. In the present study, MIL-101(Cr)@GO was synthesized using a solvothermal synthesis method at the nanoscale and was applied as sorbent in the dispersive micro-solid phase extraction (DMSPE) for the enrichment of the trace sulfonamides (SAs) from milk samples for the first time. Several experimental parameters including kinds of sorbents, the effect of pH, the amount of MIL-101(Cr)@GO, ionic strength, adsorption time, desorption solvent and desorption time were investigated. Under the optimal conditions, the linear ranges were from 0.1 to 10μg/L, 0.2-20μg/L or 0.5-50μg/L for the analytes with regression coefficients (r) from 0.9942 to 0.9999. The limits of detection were between 0.012 and 0.145μg/L. The recoveries ranged from 79.83% to 103.8% with relative standard deviations (RSDs)<10% (n=3). MIL-101(Cr)@GO exhibited remarkable advantages compared to MIL-101(Cr), MIL-100(Fe), activated carbon and other sorbent materials used in pretreatment methods. A simple, rapid, sensitive, inexpensive and less solvent consuming method of DMSPE-ultra-high performance liquid chromatography-tandem mass spectrometry (DMSPE-UHPLC-MS/MS) was successfully applied to the pre-concentration and determination of twelve SAs in milk samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Hyperbranched polyglycerol/graphene oxide nanocomposite reinforced hollow fiber solid/liquid phase microextraction for measurement of ibuprofen and naproxen in hair and waste water samples.

    PubMed

    Rezaeifar, Zohreh; Es'haghi, Zarrin; Rounaghi, Gholam Hossein; Chamsaz, Mahmoud

    2016-09-01

    A new design of hyperbranched polyglycerol/graphene oxide nanocomposite reinforced hollow fiber solid/liquid phase microextraction (HBP/GO -HF-SLPME) coupled with high performance liquid chromatography used for extraction and determination of ibuprofen and naproxen in hair and waste water samples. The graphene oxide first synthesized from graphite powders by using modified Hummers approach. The surface of graphene oxide was modified using hyperbranched polyglycerol, through direct polycondensation with thionyl chloride. The ready nanocomposite later wetted by a few microliter of an organic solvent (1-octanol), and then applied to extract the target analytes in direct immersion sampling mode.After the extraction process, the analytes were desorbed with methanol, and then detected via high performance liquid chromatography (HPLC). The experimental setup is very simple and highly affordable. The main factors influencing extraction such as; feed pH, extraction time, aqueous feed volume, agitation speed, the amount of functionalized graphene oxide and the desorption conditions have been examined in detail. Under the optimized experimental conditions, linearity was observed in the range of 5-30,000ngmL(-1) for ibuprofen and 2-10,000ngmL(-1) for naproxen with correlation coefficients of 0.9968 and 0.9925, respectively. The limits of detection were 2.95ngmL(-1) for ibuprofen and 1.51ngmL(-1) for naproxen. The relative standard deviations (RSDs) were found to be less than 5% (n=5). Copyright © 2016 Elsevier B.V. All rights reserved.

  7. Chemical passivation as a method of improving the electrochemical corrosion resistance of Co-Cr-based dental alloy.

    PubMed

    Rylska, Dorota; Sokołowski, Grzegorz; Sokołowski, Jerzy; Łukomska-Szymańska, Monika

    2017-01-01

    The purpose of the study was to evaluate corrosion resistance of Wirobond C® alloy after chemical passivation treatment. The alloy surface undergone chemical passivation treatment in four different media. Corrosion studies were carried out by means of electrochemical methods in saline solution. Corrosion effects were determined using SEM. The greatest increase in the alloy polarization resistance was observed for passive layer produced in Na2SO4 solution with graphite. The same layer caused the highest increase in corrosion current. Generally speaking, the alloy passivation in Na2SO4 solution with graphite caused a substantial improvement of the corrosion resistance. The sample after passivation in Na2SO4 solution without graphite, contrary to others, lost its protective properties along with successive anodic polarization cycles. The alloy passivation in Na3PO4 solution with graphite was the only one that caused a decrease in the alloy corrosion properties. The SEM studies of all samples after chemical passivation revealed no pit corrosion - in contrast to the sample without any modification. Every successive polarization cycle in anodic direction of pure Wirobond C® alloy enhances corrosion resistance shifting corrosion potential in the positive direction and decreasing corrosion current value. The chemical passivation in solutions with low pH values decreases susceptibility to electrochemical corrosion of Co-Cr dental alloy. The best protection against corrosion was obtained after chemical passivation of Wirobond C® in Na2SO4 solution with graphite. Passivation with Na2SO4 in solution of high pH does not cause an increase in corrosion resistance of WIROBOND C. Passivation process increases alloy resistance to pit corrosion.

  8. High-temperature Raman spectroscopy of solid oxide fuel cell materials and processes.

    PubMed

    Pomfret, Michael B; Owrutsky, Jeffrey C; Walker, Robert A

    2006-09-07

    Chemical and material processes occurring in high temperature environments are difficult to quantify due to a lack of experimental methods that can probe directly the species present. In this letter, Raman spectroscopy is shown to be capable of identifying in-situ and noninvasively changes in material properties as well as the formation and disappearance of molecular species on surfaces at temperatures of 715 degrees C. The material, yttria-stabilized zirconia or YSZ, and the molecular species, Ni/NiO and nanocrystalline graphite, factor prominently in the chemistry of solid oxide fuel cells (SOFCs). Experiments demonstrate the ability of Raman spectroscopy to follow reversible oxidation/reduction kinetics of Ni/NiO as well as the rate of carbon disappearance when graphite, formed in-situ, is exposed to a weakly oxidizing atmosphere. In addition, the Raman active phonon mode of YSZ shows a temperature dependent shift that correlates closely with the expansion of the lattice parameter, thus providing a convenient internal diagnostic for identifying thermal gradients in high temperature systems. These findings provide direct insight into processes likely to occur in operational SOFCs and motivate the use of in-situ Raman spectroscopy to follow chemical processes in these high-temperature, electrochemically active environments.

  9. Tailoring the physical properties of homopolymers and polymer nanocomposites via solid-state processing

    NASA Astrophysics Data System (ADS)

    Pierre, Cynthia

    Numerous approaches can be used to modify polymer properties. In this thesis, it is demonstrated that an innovative, continuous, industrially scalable process called solid-state shear pulverization (SSSP) can be used to enhance polymer properties with and without the addition of nanofillers. The SSSP process employs a modified twin-screw extruder in which the barrel is cooled rather than heated, resulting in the polymer being processed at a temperature below its glass transition temperature, if the polymer is amorphous, or its melt transition temperature, if the polymer is semi-crystalline. The material processed via SSSP experiences high levels of shear and compressive stresses, resulting in many repeated fragmentation and fusion steps during pulverization, which can lead to mechanochemistry. This research provides the first in-depth study on the effect of SSSP processing on the molecular structure as well as physical properties of homopolymers. Rheological characterization has demonstrated an increase in the melt viscosity of pulverized poly(ethylene terephthalate) (PET), which can be ascribed to the in situ formation of lightly branched PET. Further evidence of branched PET is provided via a dramatic increase in the rate of crystallization of the pulverized samples. These results suggest that SSSP processing can enhance the reuse and recyclability of PET. While SSSP processing has dramatic effects on the structure of polyesters and consequently their properties, a mild effect is observed for polyolefins. This thesis also demonstrates via a combination of methods that the well-exfoliated state can be achieved via SSSP processing of various polymer nanocomposites, using as-received, unmodified fillers. For example, extensive comparisons are made concerning the thermal stability in air or nitrogen atmosphere of polypropylene (PP)/clay, PP/graphite, and PP/carbon nanotube (CNT) nanocomposites made by SSSP. These comparisons suggest that the mechanism by which CNTs enhance the thermal stability of PP differs from the mechanism associated with clay and graphite.

  10. Enhancing the oxidation resistance of graphite by applying an SiC coat with crack healing at an elevated temperature

    NASA Astrophysics Data System (ADS)

    Park, Jae-Won; Kim, Eung-Seon; Kim, Jae-Un; Kim, Yootaek; Windes, William E.

    2016-08-01

    The potential of reducing the oxidation of the supporting graphite components during normal and/or accident conditions in the Very High Temperature Reactor (VHTR) design has been studied. In this work efforts have been made to slow the oxidation process of the graphite with a thin SiC coating (∼ 10 μm). Upon heating at ≥ 1173 K in air, the spallations and cracks were formed in the dense columnar structured SiC coating layer grown on the graphite with a functionally gradient electron beam physical vapor deposition (EB-PVD. In accordance with the formations of these defects, the sample was vigorously oxidized, leaving only the SiC coating layer. Then, efforts were made to heal the surface defects using additional EB-PVD with ion beam bombardment and chemical vapor deposition (CVD). The EB-PVD did not effectively heal the cracks. But, the CVD was more appropriate for crack healing, likely due to its excellent crack line filling capability with a high density and high aspect ratio. It took ∼ 34 min for the 20% weight loss of the CVD crack healed sample in the oxidation test with annealing at 1173 K, while it took ∼ 8 min for the EB-PVD coated sample, which means it took ∼4 times longer at 1173 K for the same weight reduction in this experimental set-up.

  11. Reversible temperature regulation of electrical and thermal conductivity using liquid–solid phase transitions

    PubMed Central

    Zheng, Ruiting; Gao, Jinwei; Wang, Jianjian; Chen, Gang

    2011-01-01

    Reversible temperature tuning of electrical and thermal conductivities of materials is of interest for many applications, including seasonal regulation of building temperature, thermal storage and sensors. Here we introduce a general strategy to achieve large contrasts in electrical and thermal conductivities using first-order phase transitions in percolated composite materials. Internal stress generated during a phase transition modulates the electrical and thermal contact resistances, leading to large contrasts in the electrical and thermal conductivities at the phase transition temperature. With graphite/hexadecane suspensions, the electrical conductivity changes 2 orders of magnitude and the thermal conductivity varies up to 3.2 times near 18 °C. The generality of the approach is also demonstrated in other materials such as graphite/water and carbon nanotube/hexadecane suspensions. PMID:21505445

  12. Reversible temperature regulation of electrical and thermal conductivity using liquid-solid phase transitions.

    PubMed

    Zheng, Ruiting; Gao, Jinwei; Wang, Jianjian; Chen, Gang

    2011-01-01

    Reversible temperature tuning of electrical and thermal conductivities of materials is of interest for many applications, including seasonal regulation of building temperature, thermal storage and sensors. Here we introduce a general strategy to achieve large contrasts in electrical and thermal conductivities using first-order phase transitions in percolated composite materials. Internal stress generated during a phase transition modulates the electrical and thermal contact resistances, leading to large contrasts in the electrical and thermal conductivities at the phase transition temperature. With graphite/hexadecane suspensions, the electrical conductivity changes 2 orders of magnitude and the thermal conductivity varies up to 3.2 times near 18 °C. The generality of the approach is also demonstrated in other materials such as graphite/water and carbon nanotube/hexadecane suspensions.

  13. Enhanced low-temperature lithium storage performance of multilayer graphene made through an improved ionic liquid-assisted synthesis

    NASA Astrophysics Data System (ADS)

    Raccichini, Rinaldo; Varzi, Alberto; Chakravadhanula, Venkata Sai Kiran; Kübel, Christian; Balducci, Andrea; Passerini, Stefano

    2015-05-01

    The electrochemical properties of graphene are strongly depending on its synthesis. Between the different methods proposed so far, liquid phase exfoliation turns out to be a promising method for the production of graphene. Unfortunately, the low yield of this technique, in term of solid material obtained, still limit its use to small scale applications. In this article we propose a low cost and environmentally friendly method for producing multilayer crystalline graphene with high yield. Such innovative approach, involving an improved ionic liquid assisted, microwave exfoliation of expanded graphite, allows the production of graphene with advanced lithium ion storage performance, for the first time, at low temperatures (<0 °C), as low as -30 °C, with respect to commercially available graphite.

  14. Indirect measurement of N-14 quadrupolar coupling for NH3 intercalated in potassium graphite

    NASA Technical Reports Server (NTRS)

    Tsang, T.; Fronko, R. M.; Resing, H. A.

    1987-01-01

    A method for indirect measurement of the nuclear quadrupolar coupling was developed and applied to NH3 molecules in the graphite intercalation compound K(NH3)4.3C24, which has a layered structure with alternating carbon and intercalant layers. Three triplets were observed in the H-1 NMR spectra of the compound. The value of the N-14 quadrupolar coupling constant of NH3 (3.7 MHz), determined indirectly from the H-1 NMR spectra, was intermediate between the gas value of 4.1 MHz and the solid-state value of 3.2 MHz. The method was also used to deduce the (H-1)-(H-1) and (N-14)-(H-1) dipolar interactions, the H-1 chemical shifts, and the molecular orientations and motions of NH3.

  15. Exfoliation of graphite into graphene in polar solvents mediated by amphiphilic hexa-peri-hexabenzocoronene.

    PubMed

    Kabe, Ryota; Feng, Xinliang; Adachi, Chihaya; Müllen, Klaus

    2014-11-01

    A water-soluble surfactant consisting of hexa-peri-hexabenzocoronene (HBC) as hydrophobic aromatic core and hydrophilic carboxy substituents was synthesized. It exhibited a self-assembled nanofiber structure in the solid state. Profiting from the π interactions between the large aromatic core of HBC and graphene, the surfactant mediated the exfoliation of graphite into graphene in polar solvents, which was further stabilized by the bulky hydrophilic carboxylic groups. A graphene dispersion with a concentration as high as 1.1 mg L(-1) containing 2-6 multilayer nanosheets was obtained. The lateral size of the graphene sheets was in the range of 100-500 nm based on atomic force microscope (AFM) and transmission electron microscope (TEM) measurements. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Transitions between type A flake, type D flake, and coral graphite eutectic structures in cast irons

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

    Park, J.S.; Verhoeven, J.D.

    1996-09-01

    Directional solidification experiments were used to measure the transition velocities between the type A and coral eutectic structures in high-purity cast irons and between the type A and type D eutectic structures in S and Te doped cast irons. Introduction of O into the gas atmosphere was found to have little effect on the A {R_arrow} D transition velocities in S doped alloys, but it produced a strong reduction in the A {R_arrow} coral transition velocities in high-purity irons. Transmission electron microscopy revealed interesting variations in the defect structures of the graphite in the flake irons vs the type ofmore » flake (A or D) and the type of doping element. Scanning Auger microscopy demonstrated that both S and Te segregate to the iron/graphite interface. In the S doped alloys, type A flakes are generally covered with a monolayer of S with patches of O in the form of iron oxide having a thickness on the order of 2 nm. A series of experiments, including examination of fracture surfaces at the quenched solid/liquid growth front, have shown that S segregates to the iron/graphite interfaces from the liquid at the growth front, but O forms at these interfaces during the cooldown. These results are discussed in relation to current models of eutectic growth in cast irons.« less

  17. Magnetic porous Fe3O4/carbon octahedra derived from iron-based metal-organic framework as heterogeneous Fenton-like catalyst

    NASA Astrophysics Data System (ADS)

    Li, Wenhui; Wu, Xiaofeng; Li, Shuangde; Tang, Wenxiang; Chen, Yunfa

    2018-04-01

    The synthesis of effective and recyclable Fenton-like catalyst is still a key factor for advanced oxidation processes. Herein, magnetic porous Fe3O4/carbon octahedra were constructed by a two-step controlled calcination of iron-based metal organic framework. The porous octahedra were assembled by interpenetrated Fe3O4 nanoparticles coated with graphitic carbon layer, offering abundant mesoporous channels for the solid-liquid contact. Moreover, the oxygen-containing functional groups on the surface of graphitic carbon endow the catalysts with hydrophilic nature and well-dispersion into water. The porous Fe3O4/carbon octahedra show efficiently heterogeneous Fenton-like reactions for decomposing the organic dye methylene blue (MB) with the help of H2O2, and nearly 100% removal efficiency within 60 min. Furthermore, the magnetic catalyst retains the activity after ten cycles and can be easily separated by external magnetic field, indicating the long-term catalytic durability and recyclability. The good Fenton-like catalytic performance of the as-synthesized Fe3O4/carbon octahedra is ascribed to the unique mesoporous structure derived from MOF-framework, as well as the sacrificial role and stabilizing effect of graphitic carbon layer. This work provides a facile strategy for the controllable synthesis of integrated porous octahedral structure with graphitic carbon layer, and thereby the catalyst holds significant potential for wastewater treatment.

  18. Ag induced electromagnetic interference shielding of Ag-graphite/PVDF flexible nanocomposites thinfilms

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

    Kumaran, R.; Alagar, M.; Dinesh Kumar, S.

    We report Ag nanoparticle induced Electromagnetic Interference (EMI) shielding in a flexible composite films of Ag nanoparticles incorporated graphite/poly-vinylidene difluoride (PVDF). PVDF nanocomposite thin-films were synthesized by intercalating Ag in Graphite (GIC) followed by dispersing GIC in PVDF. The X-ray diffraction analysis and the high-resolution transmission electron microscope clearly dictate the microstructure of silver nanoparticles in graphite intercalated composite of PVDF matrix. The conductivity values of nanocomposites are increased upto 2.5 times when compared to neat PVDF having a value of 2.70 S/cm at 1 MHz. The presence of Ag broadly enhanced the dielectric constant and lowers the dielectric loss of PVDFmore » matrix proportional to Ag content. The EMI shielding effectiveness of the composites is 29.1 dB at 12.4 GHz for the sample having 5 wt. % Ag and 10 wt. % graphite in PVDF.« less

  19. Observation of Persistent Currents in Finely Dispersed Pyrolytic Graphite

    NASA Astrophysics Data System (ADS)

    Saad, M.; Gilmutdinov, I. F.; Kiiamov, A. G.; Tayurskii, D. A.; Nikitin, S. I.; Yusupov, R. V.

    2018-01-01

    The trapped magnetic flux in the finely ground pyrolytic graphite sample annealed at 670 K in air has been observed. Flux trapping occurs on cooling of the sample from room temperature to 10 K in a magnetic field of 1 T. The magnitude and sign of the induced trapped moment remain unchanged when the applied magnetic field is varied within ±1 T at T K. The trapped magnetic flux is manifested in the displacement of the magnetization curve relative to that of the sample cooled in zero field. Displacement magnitude gradually decreases with the temperature increase up to 350 K, not reaching zero. The set of experimental observations probably reflects the presence in the sample of a granular high-temperature superconducting phase.

  20. Percolation transition in carbon composite on the basis of fullerenes and exfoliated graphite

    NASA Astrophysics Data System (ADS)

    Berezkin, V. I.; Popov, V. V.

    2018-01-01

    The electrical conductivity of a carbon composite on the basis of C60 fullerenes and exfoliated graphite is investigated in the range of relative contents of components from 0 to 100%. The samples are obtained by the thermal treatment of the initial dispersed mixtures in vacuum in the diffusion-adsorption process and their further cold pressing. The resistivity of the samples gradually increases with an increase in the fraction of fullerenes, and a sharp transition from the conductive state to the dielectric one is observed after achieving certain concentrations of C60. The interpretation of the results within the percolation theory makes it possible to evaluate the percolation threshold (expressed as a relative content of graphite) as equal to 4.45 wt % and the critical conductivity index as equal to 1.85 (which is typical for three-dimensional twocomponent disordered media including those having pores).

  1. Synthesis and characterization of MOF-aminated graphite oxide composites for CO2 capture

    NASA Astrophysics Data System (ADS)

    Zhao, Yunxia; Ding, Huiling; Zhong, Qin

    2013-11-01

    A kind of metal-organic frameworks (MOF-5) and aminated graphite oxide (AGO) composites were prepared for CO2 capture to mitigate global warming. MOF-5, MOF-5/GO (composite of MOF-5 and graphite oxide) and MOF-5/AGO samples were characterized by X-ray powder diffraction (XRD), infrared spectroscopy (IR), scanning electron microscope (SEM), nitrogen adsorption as well as thermogravimetric analysis to figure out their chemistry and structure information. Three types of samples with suitable specific surface area and pore diameter were chosen to test CO2 adsorption performance and stability under humidity conditions. The results indicate that high surface area and pore volume, pore similar in size to the size of gas adsorbate, and extra reactive sites modified in the composites contributes to the high CO2 capacity. Besides, the composites involved by GO or AGO show better anti-moisture performance than the parent MOF.

  2. Ultra high vacuum adhesion testing of NERVA engine materials

    NASA Technical Reports Server (NTRS)

    1970-01-01

    The primary objective of this research program was to determine the effects of surface cleaning and deliberate gaseous contamination on the adhesion behavior of selected candidate materials for use in the NERVA nuclear rocket engine program. Using a torsion balance technique, the relationship between the normal compressive load applied to crossed rod samples and the resultant contact resistance was used to ascertain the extent of adhesion under each set of experimental conditions. In addition to an evaluation of the static adhesion behavior of selected materials combinations, the experimental apparatus was modified to permit a similar investigation relating to the effects of specific tangential displacements of the sample wires, i.e., their sliding friction behavior. During the course of this subcontract, the materials combinations 440 C vs. 440 C. pyrographite vs ZTA graphite, Nbc (graphite) vs. Nbc (graphite), and Electrolize Inconel 718 vs. Au electroplated 302 S/S were evaluated.

  3. Ion irradiation to simulate neutron irradiation in model graphites: Consequences for nuclear graphite

    NASA Astrophysics Data System (ADS)

    Galy, N.; Toulhoat, N.; Moncoffre, N.; Pipon, Y.; Bérerd, N.; Ammar, M. R.; Simon, P.; Deldicque, D.; Sainsot, P.

    2017-10-01

    Due to its excellent moderator and reflector qualities, graphite was used in CO2-cooled nuclear reactors such as UNGG (Uranium Naturel-Graphite-Gaz). Neutron irradiation of graphite resulted in the production of 14C which is a key issue radionuclide for the management of the irradiated graphite waste. In order to elucidate the impact of neutron irradiation on 14C behavior, we carried out a systematic investigation of irradiation and its synergistic effects with temperature in Highly Oriented Pyrolitic Graphite (HOPG) model graphite used to simulate the coke grains of nuclear graphite. We used 13C implantation in order to simulate 14C displaced from its original structural site through recoil. The collision of the impinging neutrons with the graphite matrix carbon atoms induces mainly ballistic damage. However, a part of the recoil carbon atom energy is also transferred to the graphite lattice through electronic excitation. The effects of the different irradiation regimes in synergy with temperature were simulated using ion irradiation by varying Sn(nuclear)/Se(electronic) stopping power. Thus, the samples were irradiated with different ions of different energies. The structure modifications were followed by High Resolution Transmission Electron Microscopy (HRTEM) and Raman microspectrometry. The results show that temperature generally counteracts the disordering effects of irradiation but the achieved reordering level strongly depends on the initial structural state of the graphite matrix. Thus, extrapolating to reactor conditions, for an initially highly disordered structure, irradiation at reactor temperatures (200 - 500 °C) should induce almost no change of the initial structure. On the contrary, when the structure is initially less disordered, there should be a "zoning" of the reordering: In "cold" high flux irradiated zones where the ballistic damage is important, the structure should be poorly reordered; In "hot" low flux irradiated zones where the ballistic impact is lower and can therefore be counteracted by temperature, a better reordering of the structure should be achieved. Concerning 14C, except when located close to open pores where it can be removed through radiolytic corrosion, it tends to stabilize in the graphite matrix into sp2 or sp3 structures with variable proportions depending on the irradiation conditions.

  4. Simultaneous determination of atropine and scopolamine in buckwheat and related products using modified QuEChERS and liquid chromatography tandem mass spectrometry.

    PubMed

    Chen, Hongping; Marín-Sáez, Jesús; Romero-González, Roberto; Garrido Frenich, Antonia

    2017-03-01

    A method was developed for the determination of atropine and scopolamine in buckwheat and related products. A modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) extraction procedure was evaluated. Dispersive solid phase extraction (d-SPE) was studied as clean-up step, using graphitized black carbon (GBC) and primary secondary amine (PSA). The extract was diluted with water (50:50, v/v) prior to chromatographic analysis. The method was validated and recoveries (except chia samples spiked at 10μg/kg) ranged from 75% to 92%. Intra and inter-day precision was lower than or equal to 17%. The limit of quantification of atropine and scopolamine was 0.4 and 2μg/kg, respectively. Eight types of samples (buckwheat, wheat, soy, buckwheat flour, buckwheat noodle, amaranth grain, chia seeds and peeled millet) were analyzed. Target compounds were not found above the detection limits of the method, but three transformation products of scopolamine (norscopine, hydroscopolamine and dihydroxyscopolamine) were putative identified in the tested samples using high resolution mass spectrometry (Exactive-Orbitrap). Copyright © 2016 Elsevier Ltd. All rights reserved.

  5. Resistivity of Carbon-Carbon Composites Halved

    NASA Technical Reports Server (NTRS)

    Gaier, James R.

    2004-01-01

    Carbon-carbon composites have become the material of choice for applications requiring strength and stiffness at very high temperatures (above 2000 C). These composites comprise carbon or graphite fibers embedded in a carbonized or graphitized matrix. In some applications, such as shielding sensitive electronics in very high temperature environments, the performance of these materials would be improved by lowering their electrical resistivity. One method to lower the resistivity of the composites is to lower the resistivity of the graphite fibers, and a proven method to accomplish that is intercalation. Intercalation is the insertion of guest atoms or molecules into a host lattice. In this study the host fibers were highly graphitic pitch-based graphite fibers, or vapor-grown carbon fibers (VGCF), and the intercalate was bromine. Intercalation compounds of graphite are generally thought of as being only metastable, but it has been shown that the residual bromine graphite fiber intercalation compound is remarkably stable, resisting decomposition even at temperatures at least as high as 1000 C. The focus of this work was to fabricate composite preforms, determine whether the fibers they were made from were still intercalated with bromine after processing, and determine the effect on composite resistivity. It was not expected that the resistivity would be lowered as dramatically as with graphite polymer composites because the matrix itself would be much more conductive, but it was hoped that the gains would be substantial enough to warrant its use in high-performance applications. In a collaborative effort supporting a Space Act Agreement between the NASA Glenn Research Center and Applied Sciences, Inc. (Cedarville, OH), laminar preforms were fabricated with pristine and bromine-intercalated pitch-based fibers (P100 and P100-Br) and VGCF (Pyro I and Pyro I-Br). The green preforms were carbonized at 1000 C and then heat treated to 3000 C. To determine whether the fibers in the samples were still intercalated after composite fabrication, they were subjected to X-ray diffraction. The composites containing intercalated graphite fibers showed much higher background scatter than that of pristine fibers, indicating the presence of bromine in the samples. More importantly, faint features indicative of intercalation were visible in the diffraction pattern, showing that the fibers were still intercalated.

  6. Lunar sample analysis

    NASA Technical Reports Server (NTRS)

    Housley, R. M.

    1983-01-01

    The evolution of the lunar regolith under solar wind and micrometeorite bombardment is discussed as well as the size distribution of ultrafine iron in lunar soil. The most important characteristics of complex graphite, sulfide, arsenide, palladium, and platinum mineralization in a pegmatoid pyroxenite of the Stillwater Complex in Montana are examined. Oblique reflected light micrographs and backscattered electron SEM images of the graphite associations are included.

  7. Graphite/isobutylene-isoprene rubber highly porous cryogels as new sorbents for oil spills and organic liquids.

    PubMed

    Hu, Yan; Liu, Xiaoyan; Zou, Junchen; Gu, Ting; Chai, Wenbo; Li, Hongbing

    2013-08-28

    The preparation, by a freeze-thaw method, of new graphite/isobutylene-isoprene rubber (IIR) sorbents for oil and organic liquid is described. Graphite was expected to improve the adsorption properties. The cryogels were prepared by solution crosslinking IIR rubber in the presence of graphite in benzene at various temperatures, using sulfur monochloride as the crosslinker, and characterized by SEM and contact angle measurements. The dried cryogels, with interconnected macropores were sponge-like soft materials, with excellent buoyancy and hydrophobicity. They also showed excellent sorption characteristics, with the best sample exhibiting maximum sorption capacities of 17.8 g g(-1) for crude oil, 21.6 g g(-1) for diesel oil, and 23.4 g g(-1) for lubricating oil, respectively. The samples also showed excellent sorption capability for organic liquids, absorbing up to around twenty times their own mass. After rapid and effective desorption, taking just 3-5 h, the cryogels were recovered. They could also be reused more than 30 times by simply centrifuging to remove the sorbed liquid. These characteristics mean that the cryogels prepared in this study are promising materials for removal of large-scale oil or toxic organic spills.

  8. Contribution a l'etude et au developpement de nouvelles poudres de fonte

    NASA Astrophysics Data System (ADS)

    Boisvert, Mathieu

    L'obtention de graphite libre dans des pieces fabriquees par metallurgie des poudres (M/P) est un defi auquel plusieurs chercheurs se sont attardes. En effet, la presence de graphite apres frittage ameliore l'usinabilite des pieces, permettant donc de reduire les couts de production, et peut aussi engendrer une amelioration des proprietes tribologiques. L'approche utilisee dans cette these pour tenter d'obtenir du graphite libre apres frittage est par l'utilisation de nouvelles poudres de fontes atomisees a l'eau. L'atomisation a l'eau etant un procede de production de poudres relativement peu couteux qui permet de grandes capacites de production, le transfert des decouvertes de ce doctorat vers des applications industrielles sera donc economiquement plus favorable. En plus de l'objectif d'obtenir du graphite libre apres frittage, un autre aspect important des travaux est le controle de la morphologie du graphite libre apres frittage. En effet, il est connu dans la litterature des fontes coulees/moulees que la morphologie du graphite influencera les proprietes des fontes, ce qui est aussi vrai pour les pieces de M/P. Les fontes ductiles, pour lesquelles le graphite est sous forme de nodules spheroidaux isoles les uns des autres, possedent des proprietes mecaniques superieures aux fontes grises pour lesquelles le graphite est sous forme lamellaire et continu dans la matrice. Les resultats presentes dans cette these montrent qu'il est possible, dans des melanges contenant des poudres de fontes, d'avoir un controle sur la morphologie du graphite et donc sur les proprietes des pieces. Le controle de la morphologie du graphite a principalement ete realise par le type de frittage et le phenomene de diffusion " uphill " du carbone cause par des gradients en silicium. En effet, pour les frittages en phase solide, tous les nodules de graphite sont presents a l'interieur des grains de poudre apres frittage. Pour les frittages en phase liquide, l'intensite de la diffusion " uphill " permet de conserver plus ou moins de graphite nodulaire a l'interieur des regions riches en silicium, alors que le reste du graphite precipite sous forme lamellaire/vermiculaire dans les regions interparticulaires. L'etude des poudres de fontes et la recherche des mecanismes regissant la morphologie du graphite dans les fontes coulees/moulees nous ont amenes a produire des poudres de fontes traitees au magnesium avant l'atomisation. Plusieurs resultats fondamentaux ont ete obtenus de la caracterisation des poudres traitees au magnesium et de leur comparaison avec des poudres de chimies similaires non traitees au magnesium. D'abord, il a ete possible d'observer des bifilms d'oxyde de silicium dans la structure du graphite primaire d'une poudre de fonte grise hypereutectique. Il s'agit des premieres images montrant la structure double de ces defauts, venant ainsi appuyer la theorie elaboree par le professeur John Campbell. Ensuite, il a ete montre que le traitement au magnesium forme une atmosphere protectrice gazeuse autogeneree qui empeche l'oxydation de la surface du bain liquide et donc, la formation et l'entrainement des bifilms. Le role du magnesium sur la morphologie du graphite est de diminuer le soufre en solution en formant des precipites de sulfure de magnesium et ainsi d'augmenter l'energie d'interface graphite-liquide. En reponse a cette grande energie d'interface graphite-liquide, le graphite cherche a minimiser son ratio surface/volume, ce qui favorise la formation de graphite spheroidal. De plus, deux types de germination ont ete observes dans la poudre de fonte hypereutectique traitee au magnesium. Le premier type est une germination heterogene sur un nombre limite de particules faites de magnesium, d'aluminium, de silicium et d'oxygene. Le deuxieme type est une germination homogene des nodules dans certaines regions du liquide plus riches en silicium. L'observation du centre reel tridimensionnel, en microscopie electronique en transmission en haute resolution, d'un des nodules ayant subi une germination homogene a permis de confirmer que le mode de croissance du graphite spheroidal se produit selon le modele de la croissance en feuille de chou. (Abstract shortened by ProQuest.).

  9. Characterization of nuclear graphite elastic properties using laser ultrasonic methods

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

    Zeng, Fan W; Han, Karen; Olasov, Lauren R

    2015-01-01

    Laser ultrasonic methods have been used to characterize the elastic behaviors of commercially-available and legacy nuclear graphites. Since ultrasonic techniques are sensitive to various aspects of graphite microstructure including preferred grain orientation, microcrack orientation and porosity, laser ultrasonics is a candidate technique for monitoring graphite degradation and structural integrity in environments expected in high-temperature, gas-cooled nuclear reactors. Aspects of materials texture can be assessed by studying ultrasonic wavespeeds as a function of propagation direction and polarization. Shear wave birefringence measurements, in particular, can be used to evaluate elastic anisotropy. In this work, laser ultrasonic measurements of graphite moduli have beenmore » made to provide insight into the relationship between the microstructures and the macroscopic stiffnesses of these materials. In particular, laser ultrasonic measurements have been made using laser line sources to produce shear waves with specific polarizations. By varying the line orientation relative to the sample, shear wave birefringence measurements have been recorded. Results from shear wave birefringence measurements show that an isostatically molded graphite, such as PCIB, behaves isotropically, while an extruded graphite, such as H-451, displays significant ultrasonic texture. Graphites have complicated microstructures that depend on the manufacturing processes used, and ultrasonic texture in these materials could originate from grain orientation and preferred microcrack alignment. Effects on material isotropy due to service related microstructural changes are possible and the ultimate aim of this work is to determine the degree to which these changes can be assessed nondestructively using laser ultrasonics measurements« less

  10. Processing of ultra-high molecular weight polyethylene/graphite composites by ultrasonic injection moulding: Taguchi optimization.

    PubMed

    Sánchez-Sánchez, Xavier; Elias-Zuñiga, Alex; Hernández-Avila, Marcelo

    2018-06-01

    Ultrasonic injection moulding was confirmed as an efficient processing technique for manufacturing ultra-high molecular weight polyethylene (UHMWPE)/graphite composites. Graphite contents of 1 wt%, 5 wt%, and 7 wt% were mechanically pre-mixed with UHMWPE powder, and each mixture was pressed at 135 °C. A precise quantity of the pre-composites mixtures cut into irregularly shaped small pieces were subjected to ultrasonic injection moulding to fabricate small tensile specimens. The Taguchi method was applied to achieve the optimal level of ultrasonic moulding parameters and to maximize the tensile strength of the composites; the results showed that mould temperature was the most significant parameter, followed by the graphite content and the plunger profile. The observed improvement in tensile strength in the specimen with 1 wt% graphite was of 8.8% and all composites showed an increase in the tensile modulus. Even though the presence of graphite produced a decrease in the crystallinity of all the samples, their thermal stability was considerably higher than that of pure UHMWPE. X-ray diffraction and scanning electron microscopy confirmed the exfoliation and dispersion of the graphite as a function of the ultrasonic processing. Fourier transform infrared spectra showed that the addition of graphite did not influence the molecular structure of the polymer matrix. Further, the ultrasonic energy led oxidative degradation and chain scission in the polymer. Copyright © 2018 Elsevier B.V. All rights reserved.

  11. Mesoproterozoic graphite deposits, New Jersey Highlands: Geologic and stable isotopic evidence for possible algal origins

    USGS Publications Warehouse

    Volkert, R.A.

    2000-01-01

    Graphite deposits of Mesoproterozoic age are locally abundant in the eastern New Jersey Highlands, where they are hosted by sulphidic biotite-quartz-feldspar gneiss, metaquartzite, and anatectic pegmatite. Gneiss and metaquartzite represent a shallow marine shelf sequence of locally organic-rich sand and mud. Graphite from massive deposits within metaquartzite yielded ??13C values of -26 ?? 2??? (1??), and graphite from massive deposits within biotite-quartz-feldspar gneiss yielded ??13C values of -23 ??4???. Disseminated graphite from biotite-quartz-feldspar gneiss country rock was -22 ??3???, indistinguishable from the massive deposits hosted by the same lithology. Anatectic pegmatite is graphitic only where generated from graphite-bearing host rocks; one sample gave a ??13C value of -15???. The ??34S values of trace pyrrhotite are uniform within individual deposits, but vary from 0 to 9??? from one deposit to another. Apart from pegmatitic occurrences, evidence is lacking for long-range mobilization of carbon during Grenvillian orogenesis or post-Grenvillian tectonism. The field, petrographic, and isotope data suggest that massive graphite was formed by granulite-facies metamorphism of Proterozoic accumulations of sedimentary organic matter, possibly algal mats. Preservation of these accumulations in the sedimentary environment requires anoxic basin waters or rapid burial. Anoxia would also favour the accumulation of dissolved ferrous iron in basin waters, which may explain some of the metasediment-hosted massive magnetite deposits in the New Jersey Highlands. ?? 2000 NRC.

  12. Origin of melting point depression for rare gas solids confined in carbon pores

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

    Morishige, Kunimitsu, E-mail: morishi@chem.ous.ac.jp; Kataoka, Takaaki

    To obtain insights into the mechanism of the melting-point depression of rare gas solids confined in crystalline carbon pores, we examined the freezing and melting behavior of Xe and Ar confined to the crystalline pores of ordered mesoporous carbons as well as compressed exfoliated graphite compared to the amorphous pores of ordered mesoporous silicas, by means of X-ray diffraction. For the Xe and Ar confined to the crystalline carbon pores, there was no appreciable thermal hysteresis between freezing and melting. Furthermore, the position of the main diffraction peak did not change appreciably on freezing and melting. This strongly suggests thatmore » the liquids confined in the carbon pores form a multilayered structure parallel to the smooth walls. For the Xe and Ar confined to the amorphous silica pores, on the other hand, the position of the main diffraction peak shifted into higher scattering angle on freezing suggested that the density of the confined solid is distinctly larger than for the confined liquid. Using compressed exfoliated graphite with carbon walls of higher crystallinity, we observed that three-dimensional (3D) microcrystals of Xe confined in the slit-shaped pores melted to leave the unmelted bilayers on the pore walls below the bulk triple point. The lattice spacing of the 3D microcrystals confined is larger by ∼0.7% than that of the bilayer next to the pore walls in the vicinity of the melting point.« less

  13. Corrosion of 316 stainless steel in high temperature molten Li2BeF4 (FLiBe) salt

    NASA Astrophysics Data System (ADS)

    Zheng, Guiqiu; Kelleher, Brian; Cao, Guoping; Anderson, Mark; Allen, Todd; Sridharan, Kumar

    2015-06-01

    In support of structural material development for the fluoride-salt-cooled high-temperature reactor (FHR), corrosion tests of 316 stainless steel were performed in the potential primary coolant, molten Li2BeF4 (FLiBe) at 700 °C for an exposure duration up to 3000 h. Tests were performed in both 316 stainless steel and graphite capsules. Corrosion in both capsule materials occurred by the dissolution of chromium from the stainless steel into the salt which led to the depletion of chromium predominantly along the grain boundaries of the test samples. The samples tested in graphite capsules showed a factor of two greater depth of corrosion attack as measured in terms of chromium depletion, compared to those tested in 316 stainless steel capsules. The samples tested in graphite capsules showed the formation of Cr7C3 particulate phases throughout the depth of the corrosion layer. Samples tested in both types of capsule materials showed the formation of MoSi2 phase due to increased activity of Mo and Si as a result of Cr depletion, and furthermore corrosion promoted the formation of a α-ferrite phase in the near-surface regions of the 316 stainless steel. Based on the corrosion tests, the corrosion attack depth in FLiBe salt was predicted as 17.1 μm/year and 31.2 μm/year for 316 stainless steel tested in 316 stainless steel and in graphite capsules respectively. It is in an acceptable range compared to the Hastelloy-N corrosion in the Molten Salt Reactor Experiment (MSRE) fuel salt.

  14. Graphene nanocomposites for electrochemical cell electrodes

    DOEpatents

    Zhamu, Aruna; Jang, Bor Z.; Shi, Jinjun

    2015-11-19

    A composite composition for electrochemical cell electrode applications, the composition comprising multiple solid particles, wherein (a) a solid particle is composed of graphene platelets dispersed in or bonded by a first matrix or binder material, wherein the graphene platelets are not obtained from graphitization of the first binder or matrix material; (b) the graphene platelets have a length or width in the range of 10 nm to 10 .mu.m; (c) the multiple solid particles are bonded by a second binder material; and (d) the first or second binder material is selected from a polymer, polymeric carbon, amorphous carbon, metal, glass, ceramic, oxide, organic material, or a combination thereof. For a lithium ion battery anode application, the first binder or matrix material is preferably amorphous carbon or polymeric carbon. Such a composite composition provides a high anode capacity and good cycling response. For a supercapacitor electrode application, the solid particles preferably have meso-scale pores therein to accommodate electrolyte.

  15. Nonprevalence of biochemical fossils in kerogen from pre-Phanerozoic sediments

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

    Leventhal, J.; Suess, S. E.; Cloud, P.

    Evidence of biochemical and geochemical evolution was sought in insoluble carbonaceous matter from 30 selected pre-Phanerozoic sediments ranging in age from about 3.8 to about 0.7 x 10 9 years. The carbon isotope ratios observed were in the range of -20 to -32 per mil with reference to the Peedee belemnite standard, similar to those previously reported. No systematic trends are obvious to us. Stepwise pyrolysis-gas-chromatography showed only molecules with fewer than 8 carbon atoms at the level of sensitivity of 10 -9 g of organics in a 10 mg rock sample. Carbon, hydrogen, and nitrogen analyses showed noncarbonate carbonmore » from less than 0.1 percent to more than 3 percent, with very small amounts of N. The H/C (atomic) ratios on HCl-leached and HF-treated samples were generally less than 0.3. Evidence of low pyrolysis yields (micro-analysis) and low H/C atomic ratios (macro-analysis) implies that the carbonaceous solids in even the least metamorphosed of these ancient sediments have evolved far toward amorphous carbon or graphite and do not yield useful ''biochemical fossils.''« less

  16. Solid-Lubricant, Polymer - Polymeric and Functionalized Fiber- and Powder Reinforced Composites of Ultra-High Molecular Weight Polyethylene

    NASA Astrophysics Data System (ADS)

    Panin, S. V.; Alexenko, V. O.; Buslovich, D. G.; Anh, Nguyen Duc; Qitao, Huang

    2018-01-01

    Mechanical and tribotechnical characteristics of solid-lubricant and polymer-polymeric composites of UHMWPE were studied for the sake of design extrudable, wear-resistant, self-lubricant polymer mixtures for Additive Manufacturing (AM). Tribotechnical properties of UHMWPE blends with the optimized content of solid lubricant fillers (polytetrafluoroethylene, calcium stearate, molybdenum disulphide, colloidal graphite, boron nitride) were studied under dry sliding friction at different velocities (V = 0.3 and 0.5 m/s) and loads (P = 60 and 140 N). Also, in order to increase strength and wear-resistance of UHMWPE composites they were reinforced with wollastonite microfibers and aluminum metahydroxide AlO (OH) microparticles preliminary treated (functionalized) in polyorganosiloxane. The comparison on measured mechanical and tribotechnical properties are given with interpretation of the mechanisms of observed phenomenon.

  17. Self-Organizing Batteries

    DTIC Science & Technology

    2005-12-16

    of these principles to a lithium ion battery , resulting in the demonstration of the first self-organized rechargeable battery. These accomplishments...spherical graphite widely used as a lithium ion battery anode, was used as the high-index endmember and was attached to an AFM cantilever. Its...resulting junctions could be stable under electrochemical conditions typical of lithium ion battery systems. We used PEG + LiClO 4 as our model solid

  18. Low-Energy, Hydrogen-Free Method of Diamond Synthesis

    NASA Technical Reports Server (NTRS)

    Varshney, Deepak (Inventor); Morell, Gerardo (Inventor); Weiner, Brad R. (Inventor); Makarov, Vladimir (Inventor)

    2013-01-01

    Diamond thin films were deposited on copper substrate by the Vapor Solid (VS) deposition method using a mixture of fullerene C(sub 60) and graphite as the source material. The deposition took place only when the substrate was kept in a narrow temperature range of approximately 550-650 C. Temperatures below and above this range results in the deposition of fullerenes and other carbon compounds, respectively.

  19. Solid Lubricants for Space Structures

    DTIC Science & Technology

    1993-04-17

    will utilize mechanically interlocked hardware (caged bearings or bearings for ultra precision gimbals pointing mechanisms) controlled through precision...structure unless the lubricant were of low vapor pressure and/or suitably sealed to I prevent molecular effusion . While temperatures within spacecraft or...incorporation in the continuous cast system. The die made of graphite, consists of a plurality of openings or holes located in the die and positioned (unlined

  20. Nanostructured composite material graphite/TiO2 and its antibacterial activity under visible light irradiation.

    PubMed

    Dědková, Kateřina; Lang, Jaroslav; Matějová, Kateřina; Peikertová, Pavlína; Holešinský, Jan; Vodárek, Vlastimil; Kukutschová, Jana

    2015-08-01

    The paper addresses laboratory preparation, characterization and in vitro evaluation of antibacterial activity of graphite/TiO2 nanocomposites. Composites graphite/TiO2 with various ratio of TiO2 nanoparticles (30wt.%, and 50wt.%) to graphite were prepared using a thermal hydrolysis of titanylsulfate in the presence of graphite particles, and subsequently dried at 80°C. X-ray powder diffraction, transmission electron microscopy and Raman microspectroscopy served as phase-analytical methods distinguishing anatase and rutile phases in the prepared composites. Scanning and transmission electron microscopy techniques were used for characterization of morphology of the prepared samples. A developed modification of the standard microdilution test was used for in vitro evaluation of daylight induced antibacterial activity, using four common human pathogenic bacterial strains (Staphylococcus aureus, Escherichia coli, Enterococcus faecalis and Pseudomonas aeruginosa). Antibacterial activity of the graphite/TiO2 nanocomposites could be based mainly on photocatalytic reaction with subsequent potential interaction of reactive oxygen species with bacterial cells. During the antibacterial activity experiments, the graphite/TiO2 nanocomposites exhibited antibacterial activity, where differences in the onset of activity and activity against bacterial strains were observed. The highest antibacterial activity evaluated as minimum inhibitory concentration was observed against P. aeruginosa after 180min of irradiation. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Comparison on graphite, graphene oxide and reduced graphene oxide: Synthesis and characterization

    NASA Astrophysics Data System (ADS)

    Hidayah, N. M. S.; Liu, Wei-Wen; Lai, Chin-Wei; Noriman, N. Z.; Khe, Cheng-Seong; Hashim, U.; Lee, H. Cheun

    2017-10-01

    Graphene oxide (GO) and reduced graphene oxide (RGO) are known to have superior properties for various applications. This work compares the properties of GO and RGO with graphite. GO was prepared by using Improved Hummer's method whereas the produced GO was subjected to chemical reduction with the use of hydrazine hydrate. Graphite, GO and RGO had different morphologies, quality, functionalized groups, UV-Vis absorption peaks and crystallinity. With the removal of oxygen-containing functional group during reduction for RGO, the quality of samples was decreased due to higher intensity of D band than G band was seen in Raman results. In addition, platelet-like surface can be observed on the surface of graphite as compared to GO and RGO where wrinkled and layered flakes, and crumpled thin sheets were observed on GO and RGO surface respectively. Fourier Transform Infra-Red (FTIR) analysis showed the presence of abundant oxygen-containing functional groups in GO as compared to RGO and graphite. The characteristic peaks at 26.62°, 9.03° and 24.10° for graphite, GO and RGO, respectively, can be detected from X-Ray diffraction (XRD). Furthermore, the reduction also caused red shift at 279nm from 238nm, as obtained from ultraviolet visible (UV-Vis) analysis. The results proved that GO was successfully oxidized from graphite whereas RGO was effectively reduced from GO.

  2. Sputtering graphite coating to improve the elevated-temperature cycling ability of the LiMn2O4 electrode.

    PubMed

    Wang, Jiexi; Zhang, Qiaobao; Li, Xinhai; Wang, Zhixing; Guo, Huajun; Xu, Daguo; Zhang, Kaili

    2014-08-14

    To improve the cycle performance of LiMn2O4 at elevated temperature, a graphite layer is introduced to directly cover the surface of a commercial LiMn2O4-based electrode via room-temperature DC magnetron sputtering. The as-modified cathodes display improved capacity retention as compared to the bare LiMn2O4 cathode (BLMO) at 55 °C. When sputtering graphite for 30 min, the sample shows the best cycling performance at 55 °C, maintaining 96.2% capacity retention after 200 cycles. Reasons with respect to the graphite layer for improving the elevated-temperature performance of LiMn2O4 are systematically investigated via the methods of cyclic voltammetry, electrochemical impedance spectroscopy, X-ray photoelectron spectrometry, scanning and transmission electron microscopy, X-ray diffraction and inductively coupled plasma-atomic emission spectrometry. The results demonstrate that the graphite coated LiMn2O4 cathode has much less increased electrode polarization and electrochemical impedance than BLMO during the elevated-temperature cycling process. Furthermore, the graphite layer is able to alleviate the severe dissolution of manganese ions into the electrolyte and mitigate the morphological and structural degradation of LiMn2O4 during cycling. A model for the electrochemical kinetics process is also suggested for explaining the roles of the graphite layer in suppressing the Mn dissolution.

  3. Preparation of graphene by electrical explosion of graphite sticks.

    PubMed

    Gao, Xin; Xu, Chunxiao; Yin, Hao; Wang, Xiaoguang; Song, Qiuzhi; Chen, Pengwan

    2017-08-03

    Graphene nanosheets were produced by electrical explosion of high-purity graphite sticks in distilled water at room temperature. The as-prepared samples were characterized by various techniques to find different forms of carbon phases, including graphite nanosheets, few-layer graphene, and especially, mono-layer graphene with good crystallinity. Delicate control of energy injection is critical for graphene nanosheet formation, whereas mono-layer graphene was produced under the charging voltage of 22.5-23.5 kV. On the basis of electrical wire explosion and our experimental results, the underlying mechanism that governs the graphene generation was carefully illustrated. This work provides a simple but innovative route for producing graphene nanosheets.

  4. Eddy current inspection of graphite fiber components

    NASA Technical Reports Server (NTRS)

    Workman, G. L.; Bryson, C. C.

    1990-01-01

    The recognition of defects in materials properties still presents a number of problems for nondestructive testing in aerospace systems. This project attempts to utilize current capabilities in eddy current instrumentation, artificial intelligence, and robotics in order to provide insight into defining geometrical aspects of flaws in composite materials which are capable of being evaluated using eddy current inspection techniques. The unique capabilities of E-probes and horseshoe probes for inspecting probes for inspecting graphite fiber materials were evaluated and appear to hold great promise once the technology development matures. The initial results are described of modeling eddy current interactions with certain flaws in graphite fiber samples.

  5. Imaging graphite in air by scanning tunneling microscopy - Role of the tip

    NASA Technical Reports Server (NTRS)

    Colton, R. J.; Baker, S. M.; Driscoll, R. J.; Youngquist, M. G.; Baldeschwieler, J. D.; Kaiser, W. J.

    1988-01-01

    Atomically resolved images of highly oriented pyrolytic graphite (HOPG) in air at point contact have been obtained. Direct contact between tip and sample or contact through a contamination layer provides a conduction mechanism in addition to the exponential tunneling mechanism responsible for scanning tunneling microscopy (STM) imaging. Current-voltage (I-V) spectra were obtained while scanning in the current imaging mode with the feedback circuit interrupted in order to study the graphite imaging mechanism. Multiple tunneling tips are probably responsible for images without the expected hexagonal or trigonal symmetry. The observations indicate that the use of HOPG for testing and calibration of STM instrumentation may be misleading.

  6. GRAFEC: A New Spanish Program to Investigate Waste Management Options for Radioactive Graphite - 12399

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

    Marquez, Eva; Pina, Gabriel; Rodriguez, Marina

    Spain has to manage about 3700 tons of irradiated graphite from the reactor Vandellos I as radioactive waste. 2700 tons are the stack of the reactor and are still in the reactor core waiting for retrieval. The rest of the quantities, 1000 tons, are the graphite sleeves which have been already retrieved from the reactor. During operation the graphite sleeves were stored in a silo and during the dismantling stage a retrieval process was carried out separating the wires from the graphite, which were crushed and introduced into 220 cubic containers of 6 m{sup 3} each and placed in interimmore » storage. The graphite is an intermediate level radioactive waste but it contains long lived radionuclides like {sup 14}C which disqualifies disposal at the low level waste repository of El Cabril. Therefore, a new project has been started in order to investigate two new options for the management of this waste type. The first one is based on a selective decontamination of {sup 14}C by thermal methods. This method is based on results obtained at the Research Centre Juelich (FZJ) in the Frame of the EC programs 'Raphael' and 'Carbowaste'. The process developed at FZJ is based on a preferential oxidation of {sup 14}C in comparison to the bulk {sup 12}C. Explanations for this effect are the inhomogeneous distribution and a weaker bounding of {sup 14}C which is not incorporated in the graphite lattice. However these investigations have only been performed with graphite from the high temperature reactor Arbeitsgemeinschaft Versuchsreaktor Juelich AVR which has been operated in a non-oxidising condition or research reactor graphite operated at room temperature. The reactor Vandellos I has been operated with CO{sub 2} as coolant and significant amounts of graphite have been already oxidised. The aim of the project is to validate whether a {sup 14}C decontamination can also been achieved with graphite from Vandellos I. A second possibility under investigation is the encapsulation of the graphite in a long term stable glass matrix. The principal applicability has been already proved by FNAG. Crushed graphite mixed with a suitable glass powder has been pressed at elevated temperature under vacuum. The vacuum is required to avoid gas enclosures in the obtained product. The obtained products, named IGM for 'Impermeable Graphite Matrix', have densities above 99% of theoretical density. The amount of glass has been chosen with respect to the pore volume of the former graphite parts. The method allows the production of encapsulated graphite without increasing the disposal volume. This paper will give a short overview of characterisation results of different irradiated graphite materials obtained at CIEMAT and in the Carbowaste project as well as the proposed methods and the actual status of the program including first results about leaching of non-radioactive IGM samples and hopefully first tendencies concerning the C-14 separation from graphite of Vandellos I by thermal treatment. Both processes, the thermal treatment as well as the IGM, have the potential to solve problems related to the management of irradiated graphite in Spain. However the methods have only been tested with different types of i-graphite and virgin graphite, respectively. Only investigations with real i-graphite from Spain will reveal whether the described methods are applicable to graphite from Vandellos I. However all partners are convinced that one of these new methods or a combination of them will lead to a feasible option to manage i-graphite in Spain on an industrial scale. (authors)« less

  7. Heat Treatment Used to Strengthen Enabling Coating Technology for Oil-Free Turbomachinery

    NASA Technical Reports Server (NTRS)

    Edmonds, Brian J.; DellaCorte, Christopher

    2002-01-01

    The PS304 high-temperature solid lubricant coating is a key enabling technology for Oil- Free turbomachinery propulsion and power systems. Breakthroughs in the performance of advanced foil air bearings and improvements in computer-based finite element modeling techniques are the key technologies enabling the development of Oil-Free aircraft engines being pursued by the Oil-Free Turbomachinery team at the NASA Glenn Research Center. PS304 is a plasma spray coating applied to the surface of shafts operating against foil air bearings or in any other component requiring solid lubrication at high temperatures, where conventional materials such as graphite cannot function.

  8. Method of preparing graphene-sulfur nanocomposites for rechargeable lithium-sulfur battery electrodes

    DOEpatents

    Liu, Jun; Lemmon, John P; Yang, Zhenguo; Cao, Yuliang; Li, Xiaolin

    2015-04-07

    A method of preparing a graphene-sulfur nanocomposite for a cathode in a rechargeable lithium-sulfur battery comprising thermally expanding graphite oxide to yield graphene layers, mixing the graphene layers with a first solution comprising sulfur and carbon disulfide, evaporating the carbon disulfide to yield a solid nanocomposite, and grinding the solid nanocomposite to yield the graphene-sulfur nanocomposite. Rechargeable-lithium-sulfur batteries having a cathode that includes a graphene-sulfur nanocomposite can exhibit improved characteristics. The graphene-sulfur nanocomposite can be characterized by graphene sheets with particles of sulfur adsorbed to the graphene sheets. The sulfur particles have an average diameter of less than 50 nm.

  9. WKB calculation of multiple spin exchange in monolayer solid 3He

    NASA Astrophysics Data System (ADS)

    Ashizawa, Hisayuki; Hirashima, D. S.

    2000-10-01

    An insight is given into the multiple spin exchange in the registered 3×3 phase of solid 3He adsorbed on graphite with a WKB calculation taking account of the corrugation of the substrate potential. The corrugation is essential for this phase to be realized, and is found to suppress the exchange processes of many (>=4) particles to make only the two- and the three-spin exchanges relevant. When the magnitude of the corrugation is modest, the exchange can be ferromagnetic, in agreement with the experiment by Ikegami et al. [Phys. Rev. Lett. 81, 2478 (1998)]. Validity and limitation of the WKB approximation are also discussed.

  10. Determination of indium in geological materials by electrothermal-atomization atomic absorption spectrometry with a tungsten-impregnated graphite furance

    USGS Publications Warehouse

    Zhou, L.; Chao, T.T.; Meier, A.L.

    1984-01-01

    The sample is fused with lithium metaborate and the melt is dissolved in 15% (v/v) hydrobromic acid. Iron(III) is reduced with ascorbic acid to avoid its coextraction with indium as the bromide into methyl isobutyl ketone. Impregnation of the graphite furnace with sodium tungstate, and the presence of lithium metaborate and ascorbic acid in the reaction medium improve the sensitivity and precision. The limits of determination are 0.025-16 mg kg-1 indium in the sample. For 22 geological reference samples containing more than 0.1 mg kg-1 indium, relative standard deviations ranged from 3.0 to 8.5% (average 5.7%). Recoveries of indium added to various samples ranged from 96.7 to 105.6% (average 100.2%). ?? 1984.

  11. Advanced Materials and Fabrication Techniques for the Orion Attitude Control Motor

    NASA Technical Reports Server (NTRS)

    Gorti, Sridhar; Holmes, Richard; O'Dell, John; McKechnie, Timothy; Shchetkovskiy, Anatoliy

    2013-01-01

    Rhenium, with its high melting temperature, excellent elevated temperature properties, and lack of a ductile-to-brittle transition temperature (DBTT), is ideally suited for the hot gas components of the ACM (Attitude Control Motor), and other high-temperature applications. However, the high cost of rhenium makes fabricating these components using conventional fabrication techniques prohibitive. Therefore, near-net-shape forming techniques were investigated for producing cost-effective rhenium and rhenium alloy components for the ACM and other propulsion applications. During this investigation, electrochemical forming (EL-Form ) techniques were evaluated for producing the hot gas components. The investigation focused on demonstrating that EL-Form processing techniques could be used to produce the ACM flow distributor. Once the EL-Form processing techniques were established, a representative rhenium flow distributor was fabricated, and samples were harvested for material properties testing at both room and elevated temperatures. As a lower cost and lighter weight alternative to an all-rhenium component, rhenium- coated graphite and carbon-carbon were also evaluated. The rhenium-coated components were thermal-cycle tested to verify that they could withstand the expected thermal loads during service. High-temperature electroforming is based on electrochemical deposition of compact layers of metals onto a mandrel of the desired shape. Mandrels used for electro-deposition of near-net shaped parts are generally fabricated from high-density graphite. The graphite mandrel is easily machined and does not react with the molten electrolyte. For near-net shape components, the inner surface of the electroformed part replicates the polished graphite mandrel. During processing, the mandrel itself becomes the cathode, and scrap or refined refractory metal is the anode. Refractory metal atoms from the anode material are ionized in the molten electrolytic solution, and are deposited onto the cathodic mandrel by electrochemical reduction. Rotation of the mandrel ensures uniform distribution of refractory material. The EL-Form process allows for manufacturing in an inert atmosphere with deposition rates from 0.0004 to 0.002 in./h (10.2 to 50.8 m/h). Thicknesses typically range from microns to greater than 0.5 in. (13 mm). The refractory component produced is fabricated, dependably, to within one micron of the desired tolerances with no shrinkage or distortion as in other refractory metal manufacture techniques. The electroforming process has been used to produce solid, nonporous deposits of rhenium, iridium, niobium, tungsten, and their alloys.

  12. Isotopic measurements (C,N,O) of detonation soot produced from labeled and unlabeled Composition B-3 indicate source of solid carbon residues

    NASA Astrophysics Data System (ADS)

    Podlesak, David; Manner, Virginia; Amato, Ronald; Dattelbaum, Dana; Gusavsen, Richard; Huber, Rachel

    2017-06-01

    Detonation of HE is an exothermic process whereby metastable complex molecules are converted to simple stable molecules such as H2 O, N2, CO, CO2, and solid carbon. The solid carbon contains various allotropes such as detonation nanodiamonds, graphite, and amorphous carbon. It is well known that certain HE formulations such as Composition B (60% RDX, 40% TNT) produce greater amounts of solid carbon than other more oxygen-balanced formulations. To develop a greater understanding of how formulation and environment influence solid carbon formation, we synthesized TNT and RDX with 13 C and 15 N at levels slightly above natural abundance levels. Synthesized RDX and TNT were mixed at a ratio of 60:40 to form Composition B and solid carbon residues were collected from detonations of isotopically-labeled as well as un-labelled Composition B. The raw HE and detonation residues were analyzed isotopically for C, N, O isotopic compositions. We will discuss differences between treatments groups as a function of formulation and environment. LA-UR - 17-21266.

  13. Encapsulation of LiFePO4 by in-situ graphitized carbon cage towards enhanced low temperature performance as cathode materials for lithium ion batteries

    NASA Astrophysics Data System (ADS)

    Yao, Bin; Ding, Zhaojun; Zhang, Jianxin; Feng, Xiaoyu; Yin, Longwei

    2014-08-01

    The severe capacity decay of LiFePO4 at low temperatures (≤0 °C) limits its wide applications as cathode materials for energy storage batteries. Creating comprehensive carbon network between particles with improved electronic conductivity is a well known solution to this problem. Here, a novel structured LiFePO4/C composite was prepared by a facile solid state route, in which nanosized LiFePO4 spheres were encapsulated by in-situ graphitized carbon cages. With the enhancement in electronic conductivity (2.15e-1 S cm-1), the composite presented excellent rate performance at room temperature and remarkable capacity retention at -40 °C, with charge transfer resistance much lower than commercial LiFePO4.

  14. FOD impact testing of composite fan blades

    NASA Technical Reports Server (NTRS)

    Johns, R. H.

    1974-01-01

    The results of impact tests on large, fiber composite fan blades for aircraft turbofan engine applications are discussed. Solid composite blades of two different sizes and designs were tested. Both graphite/epoxy and boron/epoxy were evaluated. In addition, a spar-shell blade design was tested that had a boron/epoxy shell bonded to a titanium spar. All blades were tested one at a time in a rotating arm rig to simulate engine operating conditions. Impacting media included small gravel, two inch diameter ice balls, gelatin and RTV foam-simulated birds, as well as starlings and pigeons. The results showed little difference in performance between the graphite and boron/epoxy blades. The results also indicate that composite blades may be able to tolerate ice ball and small bird impacts but need improvement to tolerate birds in the small duck and larger category.

  15. FOD impact testing of composite fan blades

    NASA Technical Reports Server (NTRS)

    Johns, R. H.

    1974-01-01

    The results of impact tests on large, fiber composite fan blades for aircraft turbofan engine applications are discussed. Solid composite blades of two different sizes and designs were tested. Both graphite/epoxy and boron/epoxy were evaluated. In addition, a spar-shell blade design was tested that had a boron/epoxy shell bonded to a titanium spar. All blades were tested one at a time in a rotating arm rig to simulate engine operating conditions. Impacting media included small gravel, two inch diameter ice balls, gelatin, and RTV foam-simulated birds, as well as starlings and pigeons. The results showed little difference in performance between the graphite and boron/epoxy blades. The results also indicate that composite blades may be able to tolerate ice ball and small bird impacts but need improvement to tolerate birds in the small duck and larger category.

  16. Impact testing on composite fan blades

    NASA Technical Reports Server (NTRS)

    Johns, R. H.

    1974-01-01

    The results of impact tests on large, fiber composite fan blades for aircraft turbofan engine applications are discussed. Solid composite blades of two different sizes and designs were tested. Both graphite/epoxy and boron/epoxy were evaluated. In addition, a spar-shell blade design was tested that had a boron/epoxy shell bonded to a titanium spar. All blades were tested one at a time in a rotating arm rig to simulate engine operating conditions. Impacting media included small gravel, two inch diameter ice balls, gelatin and RTV foam-simulated birds, as well as starlings and pigeons. The results showed little difference in performance between the graphite and boron/epoxy blades. The results also indicate that composite blades may be able to tolerate ice ball and small bird impacts but need improvement to tolerate birds in the small duck and larger category.

  17. Particle production of a graphite target system for the intensity frontier

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

    Ding, X.; Kirk, H.; McDonald, K. T.

    2015-05-03

    A solid graphite target system is considered for an intense muon and/or neutrino source in support of physics at the intensity frontier. We previously optimized the geometric parameters of the beam and target to maximize particle production at low energies by incoming protons with kinetic energy of 6.75 GeV and an rms geometric emittance of 5 mm-mrad using the MARS15(2014) code. In this study, we ran MARS15 with ROOT-based geometry and also considered a mercury-jet target as an upgrade option. The optimization was extended to focused proton beams with transverse emittances from 5 to 50 mm-mrad, showing that the particlemore » production decreases slowly with increasing emittance. We also studied beam-dump configurations to suppress the rate of undesirable high-energy secondary particles in the beam.« less

  18. Thickness-dependent phase transition in graphite under high magnetic field

    NASA Astrophysics Data System (ADS)

    Taen, Toshihiro; Uchida, Kazuhito; Osada, Toshihito

    2018-03-01

    Various electronic phases emerge when applying high magnetic fields in graphite. However, the origin of a semimetal-insulator transition at B ≃30 T is still not clear, while an exotic density-wave state is theoretically proposed. In order to identify the electronic state of the insulator phase, we investigate the phase transition in thin-film graphite samples that were fabricated on silicon substrate by a mechanical exfoliation method. The critical magnetic fields of the semimetal-insulator transition in thin-film graphite shift to higher magnetic fields, accompanied by a reduction in temperature dependence. These results can be qualitatively reproduced by a density-wave model by introducing a quantum size effect. Our findings establish the electronic state of the insulator phase as a density-wave state standing along the out-of-plane direction, and help determine the electronic states in other high-magnetic-field phases.

  19. Silicone modified resins for graphite fiber laminates

    NASA Technical Reports Server (NTRS)

    Frost, L. W.; Bower, G. M.

    1979-01-01

    The development of silicon modified resins for graphite fiber laminates which will prevent the dispersal of graphite fibers when the composites are burned is discussed. Eighty-five silicone modified resins were synthesized and evaluated including unsaturated polyesters, thermosetting methacrylates, epoxies, polyimides, and phenolics. Neat resins were judged in terms of Si content, homogeneity, hardness, Char formation, and thermal stability. Char formation was estimated by thermogravimetry to 1,000 C in air and in N2. Thermal stability was evaluated by isothermal weight loss measurements for 200 hrs in air at three temperatures. Four silicone modified epoxies were selected for evaluation in unidirectional filament wound graphite laminates. Neat samples of these resins had 1,000 C char residues of 25 to 50%. The highest flexural values measured for the laminates were a strength of 140 kpsi and a modulus of 10 Mpsi. The highest interlaminar shear strength was 5.3 kpsi.

  20. Synthesis and characterization of LiFePO4/C cathode materials by sol-gel method.

    PubMed

    Liu, Shuxin; Yin, Hengbo; Wang, Haibin; Wang, Hong

    2014-09-01

    The carbon coated LiFePO4 cathode materials (LiFePO4/C) were successfully synthesized by sol-gel method with glucose, citric acid and PEG-4000 as dispersant and carbon source, respectively. The microstructure and grain size of LiFePO4/C composite were characterized by X-ray diffraction, Raman spectroscopy, transmission electron microscopy. The results showed that the carbon source and calcination temperature had important effect on the graphitization degree of carbon; the carbon decomposed by citric acid had higher graphitization degree; with calcination temperature rising, the graphitization degree of carbon increased and the particles size increased. The graphitization degree and grain size were very important for improving the electrochemical performance of LiFePO4 cathode materials, according to the experimental results, the sample LFP-700 (LFP-C) which was synthesized with citric acid as dispersant at 700 degree C had lower polarization and larger discharge capacity.

  1. Direct fabrication of 3D graphene on nanoporous anodic alumina by plasma-enhanced chemical vapor deposition

    PubMed Central

    Zhan, Hualin; Garrett, David J.; Apollo, Nicholas V.; Ganesan, Kumaravelu; Lau, Desmond; Prawer, Steven; Cervenka, Jiri

    2016-01-01

    High surface area electrode materials are of interest for a wide range of potential applications such as super-capacitors and electrochemical cells. This paper describes a fabrication method of three-dimensional (3D) graphene conformally coated on nanoporous insulating substrate with uniform nanopore size. 3D graphene films were formed by controlled graphitization of diamond-like amorphous carbon precursor films, deposited by plasma-enhanced chemical vapour deposition (PECVD). Plasma-assisted graphitization was found to produce better quality graphene than a simple thermal graphitization process. The resulting 3D graphene/amorphous carbon/alumina structure has a very high surface area, good electrical conductivity and exhibits excellent chemically stability, providing a good material platform for electrochemical applications. Consequently very large electrochemical capacitance values, as high as 2.1 mF for a sample of 10 mm3, were achieved. The electrochemical capacitance of the material exhibits a dependence on bias voltage, a phenomenon observed by other groups when studying graphene quantum capacitance. The plasma-assisted graphitization, which dominates the graphitization process, is analyzed and discussed in detail. PMID:26805546

  2. Direct fabrication of 3D graphene on nanoporous anodic alumina by plasma-enhanced chemical vapor deposition.

    PubMed

    Zhan, Hualin; Garrett, David J; Apollo, Nicholas V; Ganesan, Kumaravelu; Lau, Desmond; Prawer, Steven; Cervenka, Jiri

    2016-01-25

    High surface area electrode materials are of interest for a wide range of potential applications such as super-capacitors and electrochemical cells. This paper describes a fabrication method of three-dimensional (3D) graphene conformally coated on nanoporous insulating substrate with uniform nanopore size. 3D graphene films were formed by controlled graphitization of diamond-like amorphous carbon precursor films, deposited by plasma-enhanced chemical vapour deposition (PECVD). Plasma-assisted graphitization was found to produce better quality graphene than a simple thermal graphitization process. The resulting 3D graphene/amorphous carbon/alumina structure has a very high surface area, good electrical conductivity and exhibits excellent chemically stability, providing a good material platform for electrochemical applications. Consequently very large electrochemical capacitance values, as high as 2.1 mF for a sample of 10 mm(3), were achieved. The electrochemical capacitance of the material exhibits a dependence on bias voltage, a phenomenon observed by other groups when studying graphene quantum capacitance. The plasma-assisted graphitization, which dominates the graphitization process, is analyzed and discussed in detail.

  3. Tension strength of a thick graphite/epoxy laminate after impact by a 1/2-in. radius impactor

    NASA Technical Reports Server (NTRS)

    Poe, C. C., Jr.; Illg, W.; Garber, D. P.

    1986-01-01

    NASA is developing graphite/epoxy filament-wound cases for solid rocket motors of the space shuttle. They are wet-wound with AS4W graphite fiber and HBRF-55A epoxy. The membrane region is about 1.4 inches thick. Two 30-inch-diameter by 12-inch-long cylinders were impacted every two inches of circumference with 1/2-inch radius impactors that were dropped from various heights. One cylinder was empty and the other was filled with inert propellant. Two-inch-wide test specimens were cut from the cylinders. Each was centered on an impact site. The specimens were x-rayed and loaded to failure in uniaxial tension. Rigid body mechanics and the Hertz law were used to predict impact force, local deformations, contact diameters, and contact pressures. The depth of impact damage was predicted using Love's solution for pressure applied on part of the boundary of a semi-infinite body. The predictions were reasonably good. The strengths of the impacted specimens were reduced by as much as 37 percent without visible surface damage. Even the radiographs did not reveal the nonvisible damage.

  4. Immobilization of paracetamol and benzocaine pro-drug derivatives as long-range self-organized monolayers on graphite.

    PubMed

    Popoff, Alexandre; Fichou, Denis

    2008-05-01

    We show here by means of scanning tunneling microscopy (STM) at the liquid/solid interface that paracetamol and benzocaine molecules bearing a long aliphatic chain can be immobilized on highly oriented pyrolitic graphite (HOPG) as perfectly ordered two-dimensional domains extending over several hundreds of nanometers. In both cases, high-resolution STM images reveal that compounds 1 and 2 self-assemble into parallel lamellae having a head-to-head arrangement. The paracetamol heads of 1 are in a zigzag position with entangled n-dodecyloxy side chains while benzocaine heads of compound 2 are perfectly aligned as a double row and have their palmitic side chains on either sides of the head alignment. We attribute the very long-range ordering of these two pro-drug derivatives on HOPG to the combined effects of intermolecular H-bonding on one side and Van der Waals interactions between aliphatic side chains and graphite on the other side. The 2D immobilization of pro-drug derivatives via a non-destructive physisorption mechanism could prove to be useful for applications such as drug delivery if it can be realized on a biocompatible substrate.

  5. High performance sulfur graphite full cell for next generation sulfur Li-ion battery

    NASA Astrophysics Data System (ADS)

    Wu, Yunwen; Momma, Toshiyuki; Yokoshima, Tokihiko; Nara, Hiroki; Osaka, Tetsuya

    2018-06-01

    Sulfur (S) Li-ion battery which use the metallic Li free anode is deemed as a promising solution to conquer the hazards originating from Li metal. However, stable cycling performance and low production price of the S Li-ion battery still remain challenging. Here, we propose a S-LixC full cell system by paring a S cathode and a pre-lithiated graphite anode which is cheap and commercially available. It shows stable cycling performance with a capacity around 1300 mAh (g-S)-1 at 0.2 C-rate and 1000 mAh (g-S)-1 at 0.5 C-rate. In addition, 0.1% per cycle capacity fading rate with a capacity retention of 880 mAh (g-S)-1 after 400 cycles at 0.2 C-rate has been achieved. The pre-formed solid electrolyte interphase (SEI) layer on the pre-lithaited graphite anode largely contributes to the high capacity performance. Notably, a 10-times-enlarged scale of S-LixC laminate type full cell has been assembled with high capacity performance (around 1000 mAh (g-S)-1) even after high rate cycling.

  6. Nucleation of ripplocations through atomistic modeling of surface nanoindentation in graphite

    NASA Astrophysics Data System (ADS)

    Freiberg, D.; Barsoum, M. W.; Tucker, G. J.

    2018-05-01

    In this work, we study the nucleation and subsequent evolution behavior of ripplocations - a newly proposed strain accommodating defect in layered materials where one, or more, layers buckle orthogonally to the layers - using atomistic modeling of graphite. To that effect, we model the response to cylindrical indenters with radii R of 50, 100, and 250 nm, loaded edge-on into graphite layers and the strain gradient effects beneath the indenter are quantified. We show that the response is initially elastic followed by ripplocation nucleation, and growth of multiple fully reversible ripplocation boundaries below the indenter. In the elastic region, the stress is found to be a function of indentation volume; beyond the elastic regime, the interlayer strain gradient emerges as paramount in the onset of ripplocation nucleation and subsequent in-plane stress relaxation. Furthermore, ripplocation boundaries that nucleate from the alignment of ripplocations on adjacent layers are exceedingly nonlocal and propagate, wavelike, away from the indented surface. This work not only provides a critical understanding of the mechanistic underpinnings of the deformation of layered solids and formation of kink boundaries, but also provides a more complete description of the nucleation mechanics of ripplocations and their strain field dependence.

  7. A new strategy for the modification of a carbon paste electrode with carrageenan hydrogel for a sensitive and selective determination of arsenic in natural waters.

    PubMed

    Núñez, Claudia; Arancibia, Verónica; Triviño, Juan José

    2018-09-01

    An adsorptive stripping voltammetric method for the determination of As(III) and As total in water samples using a carrageenan modified carbon paste electrode is presented for the first time (CAR-CPE). The modified electrode was prepared in different ways: by adding CAR in solid form or as a hydrogel together with graphite and paraffin, as well as adsorbing CAR by applying a potential on an unmodified carbon paste electrode. The best results were obtained when CAR was incorporated as hydrogel (HCAR-CPE). The selection of the ratio amounts for electrode preparation was carried out applying a multivariate experimental design. Variables like amount of graphite (U 1 ), HCAR (U 2 ) and paraffin (U 3 ) were optimized using a (2 K +2K+C) model. The results showed that the amount of HCAR was the most significant factor, and the adequate U 1 :U 2 :U 3 ratio to prepare the electrode was: 493 mg of graphite, 214 μL of paraffin and 134 μL of carrageenan as gel. The optimum parameters for the determination of As(III) were pH = 3.25 (0.01 mol L -1 H 3 PO 4 /H 2 PO 4 - solution); E acc = -0.50 V and t acc = 30 s. The electrode presents good linear behavior concentration range from 0.50 to 6.70 μg L -1 , with a limit of detection of 0.22 μg L -1 . The relative standard deviation was 5.0% at the 1.5 μg L -1 As(III) level (n = 16). The method was validated by quantifying As(III) in spiked tap water from laboratory (RE: 3.0%), and it was applied for the determination of As total in water samples from the Loa River (North of Chile) prior reduction of As(V) with Na 2 S 2 O 3 solution, obtaining 814.00 ± 0.03 μg L -1 . The results of the proposed method were compared with those obtained by adsorptive stripping voltammetry with HMDE and by Inductively Coupled Plasma Mass Spectrometry (ICP-MS) techniques. Copyright © 2018 Elsevier B.V. All rights reserved.

  8. Formation and Inhibition of Metallic Lithium Microstructures in Lithium Batteries Driven by Chemical Crossover

    DOE PAGES

    Li, Wangda; Kim, Un-Hyuck; Dolocan, Andrei; ...

    2017-05-14

    The formation of metallic lithium microstructures in the form of dendrites or mosses at the surface of anode electrodes (e.g., lithium metal, graphite, and silicon) leads to rapid capacity fade and poses grave safety risks in rechargeable lithium batteries. In this work, we present here a direct, relative quantitative analysis of lithium deposition on graphite anodes in pouch cells under normal operating conditions, paired with a model cathode material, the layered nickel-rich oxide LiNi 0.61Co 0.12Mn 0.27O 2, over the course of 3000 charge-discharge cycles. Secondary-ion mass spectrometry chemically dissects the solid-electrolyte interphase (SEI) on extensively cycled graphite with virtuallymore » atomic depth resolution and reveals substantial growth of Li-metal deposits. With the absence of apparent kinetic (e.g., fast charging) or stoichiometric restraints (e.g., overcharge) during cycling, we show lithium deposition on graphite is triggered by certain transition-metal ions (manganese in particular) dissolved from the cathode in a disrupted SEI. This insidious effect is found to initiate at a very early stage of cell operation (<200 cycles) and can be effectively inhibited by substituting a small amount of aluminum (~1 mol %) in the cathode, resulting in much reduced transition-metal dissolution and drastically improved cyclability. In conclusion, our results may also be applicable to studying the unstable electrodeposition of lithium on other substrates, including Li metal.« less

  9. Formation and Inhibition of Metallic Lithium Microstructures in Lithium Batteries Driven by Chemical Crossover

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

    Li, Wangda; Kim, Un-Hyuck; Dolocan, Andrei

    The formation of metallic lithium microstructures in the form of dendrites or mosses at the surface of anode electrodes (e.g., lithium metal, graphite, and silicon) leads to rapid capacity fade and poses grave safety risks in rechargeable lithium batteries. In this work, we present here a direct, relative quantitative analysis of lithium deposition on graphite anodes in pouch cells under normal operating conditions, paired with a model cathode material, the layered nickel-rich oxide LiNi 0.61Co 0.12Mn 0.27O 2, over the course of 3000 charge-discharge cycles. Secondary-ion mass spectrometry chemically dissects the solid-electrolyte interphase (SEI) on extensively cycled graphite with virtuallymore » atomic depth resolution and reveals substantial growth of Li-metal deposits. With the absence of apparent kinetic (e.g., fast charging) or stoichiometric restraints (e.g., overcharge) during cycling, we show lithium deposition on graphite is triggered by certain transition-metal ions (manganese in particular) dissolved from the cathode in a disrupted SEI. This insidious effect is found to initiate at a very early stage of cell operation (<200 cycles) and can be effectively inhibited by substituting a small amount of aluminum (~1 mol %) in the cathode, resulting in much reduced transition-metal dissolution and drastically improved cyclability. In conclusion, our results may also be applicable to studying the unstable electrodeposition of lithium on other substrates, including Li metal.« less

  10. Perfluoroalkyl-substituted ethylene carbonates: Novel electrolyte additives for high-voltage lithium-ion batteries

    NASA Astrophysics Data System (ADS)

    Zhu, Ye; Casselman, Matthew D.; Li, Yan; Wei, Alexander; Abraham, Daniel P.

    2014-01-01

    A new family of polyfluoroalkyl-substituted ethylene carbonates is synthesized and tested as additives in lithium-ion cells containing EC:EMC + LiPF6-based electrolyte. The influence of these compounds is investigated in Li1.2Ni0.15Mn0.55Co0.1O2//graphite cells via a combination of galvanostatic cycling and electrochemical impedance spectroscopy (EIS) tests. Among the four additives studied in this work (4-(trifluoromethyl)-1,3-dioxolan-2-one (TFM-EC), 4-(perfluorobutyl)-1,3-dioxolan-2-one (PFB-EC), 4-(perfluorohexyl)-1,3-dioxolan-2-one (PFH-EC), and 4-(perfluorooctyl)-1,3-dioxolan-2-one (PFO-EC)), small amounts (0.5 wt%) of PFO-EC is found to be most effective in lessening cell performance degradation during extended cycling. Linear sweep voltammetry (LSV), X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy are used to further characterize the effects of PFO-EC on the positive and negative electrodes. LSV data from the electrolyte, and XPS analyses of electrodes harvested after cycling, suggest that PFO-EC is oxidized on the cathode forming surface films that slow electrode/cell impedance rise. Differential capacity (dQ/dV) plots from graphite//Li cells suggest that PFO-EC is involved in solid electrolyte interphase (SEI) formation. Raman data from anodes after cycling suggest that structural disordering of graphite is reduced by the addition of PFO-EC, which may explain the improved cell capacity retention.

  11. Exfoliated graphite with graphene flakes as potential candidates for TL dosimeters at high gamma doses.

    PubMed

    Ortiz-Morales, A; López-González, E; Rueda-Morales, G; Ortega-Cervantez, G; Ortiz-Lopez, J

    2018-06-06

    Graphite powder (GP) subjected to microwave radiation (MWG) results in exfoliation of graphite particles into few-layered graphene flakes (GF) intermixed with partially exfoliated graphite particles (PEG). Characterization of MWG by Scanning Electron Microscopy (SEM), Atomic Force Microscopy (AFM) and Raman spectroscopy reveal few-layer GF with sizes ranging from 0.2 to 5 µm. Raman D, G, and 2D (G') bands characteristic of graphitic structures include evidence of the presence of bilayered graphene. The thermoluminescent (TL) dosimetric properties of MWG are evaluated and can be characterized as a gamma-ray sensitive and dose-resistant material with kinetic parameters (activation energy for the main peak located at 400 and 408 K is 0.69 and 0.72 eV) and threshold dose (~1 kGy and 5 kGy respectively). MWG is a low-Z material (Z eff = 6) with a wide linear range of TL dose-response (0.170-2.5 kGy) tested at doses in the 1-20 kGy range with promising results for applications in gamma-ray dosimetry. Results obtained in gamma irradiated MWG are compared with those obtained in graphite powder samples (GP) without microwave treatment. Copyright © 2018 Elsevier Ltd. All rights reserved.

  12. Pencil graphite leads as simple amperometric sensors for microchip electrophoresis.

    PubMed

    Natiele Tiago da Silva, Eiva; Marques Petroni, Jacqueline; Gabriel Lucca, Bruno; Souza Ferreira, Valdir

    2017-11-01

    In this work we demonstrate, for the first time, the use of inexpensive commercial pencil graphite leads as simple amperometric sensors for microchip electrophoresis. A PDMS support containing one channel was fabricated through soft lithography and sanded pencil graphite leads were inserted into this channel to be used as working electrodes. The electrochemical and morphological characterization of the sensor was carried out. The graphite electrode was coupled to PDMS microchips in end-channel configuration and electrophoretic experiments were performed using nitrite and ascorbate as probe analytes. The analytes were successfully separated and detected in well-defined peaks with satisfactory resolution using the microfluidic platform proposed. The repeatability of the pencil graphite electrode was satisfactory (RSD values of 1.6% for nitrite and 12.3% for ascorbate, regarding the peak currents) and its lifetime was estimated to be ca. 700 electrophoretic runs over a cost of ca. $ 0.05 per electrode. The limits of detection achieved with this system were 2.8 μM for nitrite and 5.7 μM for ascorbate. For proof of principle, the pencil graphite electrode was employed for the real analysis of well water samples and nitrite was successfully quantified at levels below its maximum contaminant level established in Brazil and US. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Evaluation of ammonia as diluent for serum sample preparation and determination of selenium by graphite furnace atomic absorption spectrometry*1

    NASA Astrophysics Data System (ADS)

    Hernández-Caraballo, Edwin A.; Burguera, Marcela; Burguera, José L.

    2002-12-01

    A method for the determination of total selenium in serum samples by graphite furnace atomic absorption spectrometry was evaluated. The method involved direct introduction of 1:5 diluted serum samples (1% v/v NH 4OH+0.05% w/v Triton X-100 ®) into transversely heated graphite tubes, and the use of 10 μg Pd+3 μg Mg(NO 3) 2 as chemical modifier. Optimization of the modifier mass and the atomization temperature was conducted by simultaneously varying such parameters and evaluating both the integrated absorbance and the peak height/peak area ratio. The latter allowed the selection of compromise conditions rendering good sensitivity and adequate analyte peak profiles. A characteristic mass of 49 pg and a detection limit (3s) of 6 μg 1 -1 Se, corresponding to 30 μg l -1 Se in the serum sample, were obtained. The analyte addition technique was used for calibration. The accuracy was assessed by the determination of total selenium in Seronorm™ Trace Elements Serum Batch 116 (Nycomed Pharma AS). The method was applied for the determination of total selenium in ten serum samples taken from individuals with no known physical affection. The selenium concentration ranged between 79 and 147 μg l -1, with a mean value of 114±22 μg l -1.

  14. SEA LION--A TIME-DEPENDENT APPROXIMATE AERO-THERMODYNAMIC CODE TO CALCULATE AXIAL TEMPERATURE DISTRIBUTIONS OF MULTIPLE CONDUITS

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

    Var, R.E.; Uthe, P.M. Jr.

    1961-06-01

    No abstract.<>15:021066No abstract.<>15:021067The behavior of refractory materials in high temperature environments is being investigated in order to establish good working data and general principles. The areas of interest include thermal and mechanical properties, and mechanisms of loss of material at the surface by evaporative processes or by reaction with free- radial species. Studies of the nature of species arising directly from a solid surface by evaporation are being pursued utilizing three independent . techniques. Applicability of the matrix-isolation technique was demonstrated, and in the cases of boric oxide and carbon evidence was obtained for the presence of B/sub 2/O/sub 3/more » and C/sub 3/ in the respective vapors. A newly built wide- range mass spectrometer of high resolving power was brought into service. Incidental to this, measurements of the heat of vaporization of palladium were made giving an approximate value of 93 kcal per mole. The third approach for determining vapor species is by emission spectroscopy for which a furnace capable of operation at 3000 deg C is practically complete. Work was done on reactions of nitrogen and hydrogen atoms with solid surfaces. It was found that with nitrogen atoms and carbon an appreciable reaction occurs when carbon is heated up to the vicinity of 1350 deg C. With hydrogen atoms and carbon on the other hand, reaction takes place at about room temperature. Techniques are being improved in order to obtain quantitative data leading to an understanding of the kinetics and mechanisms involved. Investigations of the thermal properties of solids at high temperatures gave substantial results. Thermal conductivity data were obtained using an improved version of the Longmire technique for carbon, graphite, and several refractory metals including titanium snd zircorium. An extension of this method using transient heating to measure the specific heats of solids was also developed, and work with graphite established the validity of the technique. A new technique of determining conductivity using periodic heating of a wire sample was devised. The equipment for applying it, particularly to single-crystal samples, is nearly completed. A theoretical study has revealed a method capable in principle of simultaneously determining the thermal conductivity and specific heat of a sample at high temperatures. Data on the spectral emissivities of certain single crystals were obtained at 725 to 2125 deg C. Values for the two extremes of temperature respectively are: titanium carbide --0.40 and 0.32, titanium diboride--0.26 and 0.24, riobium carbide --0.28 snd 0.22. Work toward the measurement of other physical properties at very high temperatures was largely on the design and construction of equipment and the preparation of materials for specimens. A furnace and testing fixtures were constructed for bending single crystals at elevated temperatures, and work is proceeding on the production of highpurity MgO crystals, for which the highest grade carbon electrodes were found necessary. Another furnace is being constructed for conducting tensile snd creep tests on refractory compounds at temperatures up to 2700 deg C, and a pulse-echo technique is being developed for measuring elastic properties at high temperatures. An additional special furnace was designed and is being built to permit x ray measurements on specimens at high temperatures, and some x ray studies were also undertaken at room temperature to help characterize refractory compounds which . were produced as specimen materials. (auth)« less

  15. Effects of high energy radiation on the mechanical properties of epoxy graphite fiber reinforced composites

    NASA Technical Reports Server (NTRS)

    Gilbert, R. D.; Fornes, R. E.; Memory, J. D.

    1983-01-01

    The effects of high energy radiation on mechanical properties and on the molecular and structural properties of graphite fiber reinforced composites are assessed so that durability in space applications can be predicted. A listing of composite systems irradiated along with the maximum radiation dose applied and type of mechanical tests performed is shown. These samples were exposed to 1/2 MeV electrons.

  16. Cooling Curve Analysis of Micro- and Nanographite Particle-Embedded Salt-PCMs for Thermal Energy Storage Applications

    NASA Astrophysics Data System (ADS)

    Sudheer, R.; Prabhu, K. N.

    2017-08-01

    In recent years, the focus of phase change materials (PCM) research was on the development of salt mixtures with particle additives to improve their thermal energy storage (TES) functionalities. The effect of addition of microsized (50 μm) and nanosized (400 nm) graphite particles on TES parameters of potassium nitrate was analyzed in this work. A novel technique of computer-aided cooling curve analysis was employed here to study the suitability of large inhomogeneous PCM samples. The addition of graphite micro- and nanoparticles reduced the solidification time of the PCM significantly enhancing the heat removal rates, in the first thermal cycle. The benefits of dispersing nanoparticles diminished in successive 10 thermal cycles, and its performance was comparable to the microparticle-embedded PCM thereafter. The decay of TES functionalities on thermal cycling is attributed to the agglomeration of nanoparticles which was observed in SEM images. The thermal diffusivity property of the PCM decreased with addition of graphite particles. With no considerable change in the cooling rates and a simultaneous decrease in thermal diffusivity, it is concluded that the addition of graphite particles increased the specific heat capacity of the PCM. It is also suggested that the additive concentration should not be greater than 0.1% by weight of the PCM sample.

  17. Reinforcement of cement-based matrices with graphite nanomaterials

    NASA Astrophysics Data System (ADS)

    Sadiq, Muhammad Maqbool

    Cement-based materials offer a desirable balance of compressive strength, moisture resistance, durability, economy and energy-efficiency; their tensile strength, fracture energy and durability in aggressive environments, however, could benefit from further improvements. An option for realizing some of these improvements involves introduction of discrete fibers into concrete. When compared with today's micro-scale (steel, polypropylene, glass, etc.) fibers, graphite nanomaterials (carbon nanotube, nanofiber and graphite nanoplatelet) offer superior geometric, mechanical and physical characteristics. Graphite nanomaterials would realize their reinforcement potential as far as they are thoroughly dispersed within cement-based matrices, and effectively bond to cement hydrates. The research reported herein developed non-covalent and covalent surface modification techniques to improve the dispersion and interfacial interactions of graphite nanomaterials in cement-based matrices with a dense and well graded micro-structure. The most successful approach involved polymer wrapping of nanomaterials for increasing the density of hydrophilic groups on the nanomaterial surface without causing any damage to the their structure. The nanomaterials were characterized using various spectrometry techniques, and SEM (Scanning Electron Microscopy). The graphite nanomaterials were dispersed via selected sonication procedures in the mixing water of the cement-based matrix; conventional mixing and sample preparation techniques were then employed to prepare the cement-based nanocomposite samples, which were subjected to steam curing. Comprehensive engineering and durability characteristics of cement-based nanocomposites were determined and their chemical composition, microstructure and failure mechanisms were also assessed through various spectrometry, thermogravimetry, electron microscopy and elemental analyses. Both functionalized and non-functionalized nanomaterials as well as different micro-scale fibers were used for comparison purposes at different volume fractions. Replicated mixes and tests were considered to provide the basis for statistically reliable inferences. Theoretical studies were conducted in order to develop insight into the reinforcement mechanisms of properly functionalized graphite nanomaterials. The results suggested that modified graphite nanomaterials improve the mechanical performance of cement-based matrices primarily through control of microcrack size and propagation, relying on their close spacing within matrix and dissipation of substantial energy by debonding and frictional pullout over their enormous surface areas. The gains in barrier qualities of cement-based materials with introduction of modified graphite nanomaterials could be attributed to the increased tortuosity of diffusion paths in the presence of closely spaced nanomaterials. Experimental investigations were designed and implemented towards identification of the optimum (nano- and micro-scale) reinforcement systems for high-performance concrete through RSA (Response Surface Analysis). A comprehensive experimental data base was developed on the mechanical, physical and durability characteristics as well as the structure and composition of high-performance cementitious nanocomposites reinforced with modified graphite nanomaterials and/ or different micro-fibers.

  18. Dry Lubrication of High Temperature Silicon Nitride Rolling Contacts.

    DTIC Science & Technology

    1980-11-01

    comparable to M50 bearing steel [2]. Quality control measures were implemented in the areas of raw material inspection as well as non-destructive evaluation...to oil lubricated bearing steels . Due to the apparent success of graphite at high tem- perature, three vendors were selected that manufacture graph...hybrid bearings ( steel rings and silicon nitride balls) to establish solid lubricant/cage design practices. High temperature bearing tests with silicon

  19. Inexpensive Chemiresistor Sensors for Real Time Ground Water Contamination Measurement

    DTIC Science & Technology

    2002-04-01

    for Liquid Phase PEVA -40-C Chemiresistor Under Vapor Phase Exposure...29 6 -40-C (’ DIP • LDRD LOD MTBE ppb ppm PCP PDPP PECH PEVA PIB RH SAW SEED SERDP SLM trans-DCE TCE VERI voc L1R!Ro...Nomenclature Suffix for polymer inks, indicating percentage of total solids weight made up of graphitized carbon particles (e.g., PEVA -40-C) dual inline

  20. Solid Lubricated Rolling Element Bearings

    DTIC Science & Technology

    1979-02-15

    lubricant into uneven patches of varnish . This varnish , along with the file-like action of the exposed ball carbides on the relatively softer races, can...its structure. Fluorine , one of the most reactive elements, reacts with graphite without combustion from about 790’F to 1022°F, forming a grey-colored...to allow for molding and machining after molding. 0 Method 2 (Hughes) Impregnating these dense weaves with a Thermid 600 polyimide varnish

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