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Sample records for high-purity ceramic powders

  1. Production of Ultrafine, High-purity Ceramic Powders Using the US Bureau of Mines Developed Turbomill

    NASA Technical Reports Server (NTRS)

    Hoyer, Jesse L.

    1993-01-01

    Turbomilling, an innovative grinding technology developed by the U.S. Bureau of Mines in the early 1960's for delaminating filler-grade kaolinitic clays, has been expanded into the areas of particle size reduction, material mixing, and process reaction kinetics. The turbomill, originally called an attrition grinder, has been used for particle size reduction of many minerals, including natural and synthetic mica, pyrophyllite, talc, and marble. In recent years, an all-polymer version of the turbomill has been used to produce ultrafine, high-purity, advanced ceramic powders such as SiC, Si3N4, TiB2, and ZrO2. In addition to particle size reduction, the turbomill has been used to produce intimate mixtures of high surface area powders and whiskers. Raw materials, TiN, AlN, and Al2O3, used to produce a titanium nitride/aluminum oxynitride (TiN/AlON) composite, were mixed in the turbomill, resulting in strength increases over samples prepared by dry ball milling. Using the turbomill as a leach vessel, it was found that 90.4 pct of the copper was extracted from the chalcopyrite during a 4-hour leach test in ferric sulfate versus conventional processing which involves either roasting of the ore for Cu recovery or leaching of the ore for several days.

  2. Electrolytic production of high purity aluminum using ceramic inert anodes

    DOEpatents

    Ray, Siba P.; Liu, Xinghua; Weirauch, Douglas A.; DiMilia, Robert A.; Dynys, Joseph M.; Phelps, Frankie E.; LaCamera, Alfred F.

    2002-01-01

    A method of producing commercial purity aluminum in an electrolytic reduction cell comprising ceramic inert anodes is disclosed. The method produces aluminum having acceptable levels of Fe, Cu and Ni impurities. The ceramic inert anodes used in the process may comprise oxides containing Fe and Ni, as well as other oxides, metals and/or dopants.

  3. Unusual ferromagnetism in high purity ZnO sintered ceramics

    SciTech Connect

    Das, J.; Pradhan, S.K.; Mishra, D.K.; Sahu, D.R.; Nayak, B.B.; Huang, Jow-Lay; Roul, B.K.

    2011-01-15

    We report our novel result regarding the observation of unusual but clean ferromagnetic (FM) signature at room temperature (RT) in high pure (99.999%) ZnO bulk ceramics processed by slow step sintering schedule (SSSS). All the sintered samples showed ferromagnetic signature at room temperature. However, sample sintered at 850 {sup o}C showed more prominent M-H loop and saturation magnetization with respect to samples sintered at 500 {sup o}C and 1300 {sup o}C. Observation of FM behavior in sintered ceramics may be attributed to the presence of defects like cation (Zn)/anion (O) vacancies and interstitials created during the processing of sample. It is anticipated that SSSS promotes enhanced physical bulk as well as surface densification and at the same time confined the outgassing of free oxygen and Zn from the bulk which are acting as suitable defect sites inside the sintered grains and grain boundary junctions. Our micro-Raman and X-ray photoelectron studies revealed the existence of these defects which are believed to be the origin of the unconventional ferromagnetism (FM) of ZnO bulk ceramic at room temperature.

  4. Ceramic Powders

    NASA Technical Reports Server (NTRS)

    1984-01-01

    In developing its product line of specialty ceramic powders and related products for government and industrial customers, including companies in the oil, automotive, electronics and nuclear industries, Advanced Refractory Technologies sought technical assistance from NERAC, Inc. in specific areas of ceramic materials and silicon technology, and for assistance in identifying possible applications of these materials in government programs and in the automotive and electronics industry. NERAC conducted a computerized search of several data bases and provided extensive information in the subject areas requested. NERAC's assistance resulted in transfer of technologies that helped ART staff develop a unique method for manufacture of ceramic materials to precise customer specifications.

  5. Synthesis of high purity nitride powders. (Latest citations from Engineered Materials abstracts). NewSearch

    SciTech Connect

    Not Available

    1994-10-01

    The bibliography contains citations concerning the synthesis and preparation of high purity nitride powders. Citations discuss the preparation of powders using chemical vapor deposition, carbothermic reactions, plasmochemical reactions, pyrolysis, sol gel processes, and self-propagating high-temperature synthesis. Citations concern boron nitrides, carbonitrides, aluminum nitrides, silicon nitrides, and titanium nitrides. (Contains a minimum of 246 citations and includes a subject term index and title list.)

  6. Synthesis of high purity nitride powders. (Latest citations from Engineered Materials abstracts). Published Search

    SciTech Connect

    1995-12-01

    The bibliography contains citations concerning the synthesis and preparation of high purity nitride powders. Citations discuss the preparation of powders using chemical vapor deposition, carbothermic reactions, plasmochemical reactions, pyrolysis, sol gel processes, and self-propagating high-temperature synthesis. Citations concern boron nitrides, carbonitrides, aluminum nitrides, silicon nitrides, and titanium nitrides.(Contains 50-250 citations and includes a subject term index and title list.) (Copyright NERAC, Inc. 1995)

  7. Synthesis of high purity carbide powders. (Latest citations from Engineered Materials abstracts). Published Search

    SciTech Connect

    Not Available

    1994-08-01

    The bibliography contains citations concerning the synthesis and preparation of high purity carbide powders. Articles discuss techniques of powder manufacture such as chemical vapor deposition, plasma arc reactions, sintering, hot pressing, combustion synthesis, precipitation, chemical reaction, self-propagating high temperature synthesis, shock or explosive compaction, and aerosol formation. Citations concern silicon carbides, titanium carbides, and other carbide materials and composites. (Contains 250 citations and includes a subject term index and title list.)

  8. Surface preparation for high purity alumina ceramics enabling direct brazing in hydrogen atmospheres

    DOEpatents

    Cadden, Charles H.; Yang, Nancy Yuan Chi; Hosking, Floyd M.

    2001-01-01

    The present invention relates to a method for preparing the surface of a high purity alumina ceramic or sapphire specimen that enables direct brazing in a hydrogen atmosphere using an active braze alloy. The present invention also relates to a method for directly brazing a high purity alumina ceramic or sapphire specimen to a ceramic or metal member using this method of surface preparation, and to articles produced by this brazing method. The presence of silicon, in the form of a SiO.sub.2 -containing surface layer, can more than double the tensile bond strength in alumina ceramic joints brazed in a hydrogen atmosphere using an active Au-16Ni-0.75 Mo-1.75V filler metal. A thin silicon coating applied by PVD processing can, after air firing, produce a semi-continuous coverage of the alumina surface with a SiO.sub.2 film. Room temperature tensile strength was found to be proportional to the fraction of air fired surface covered by silicon-containing films. Similarly, the ratio of substrate fracture versus interface separation was also related to the amount of surface silicon present prior to brazing. This process can replace the need to perform a "moly-manganese" metallization step.

  9. Plasma Sprayed Coatings of High-Purity Ceramics for Semiconductor and Flat-Panel-Display Production Equipment

    NASA Astrophysics Data System (ADS)

    Kitamura, Junya; Ibe, Hiroyuki; Yuasa, Fumi; Mizuno, Hiroaki

    2008-12-01

    High-purity oxide ceramic powders of alumina (Al2O3) and yttria (Y2O3) have been developed to apply to semiconductor and flat-panel-display (FPD) production equipment. The ceramic coatings on the inside chamber wall of the equipment are required to have high erosion resistance against CFx plasma in dry etching process for microfabrications of the devices. It is found that the yttria coating formed from agglomerated-and-sintered powder consisting of large primary particles has smoother eroded surface with high erosion resistance. Considering the particle deposition on the devices, this coating will be effective in decreasing generation of large-sized particles, which easily deposit on the devices. Electric insulating properties of the coatings are also investigated to apply to electrostatic chuck. Electric breakdown voltage of yttria coatings is comparable to that of alumina coatings. Smaller powder is effective for improving the electric properties, and the influence of coating purity is lower than that of the powder size.

  10. Ceramic powder compaction

    SciTech Connect

    Glass, S.J.; Ewsuk, K.G.; Mahoney, F.M.

    1995-12-31

    With the objective of developing a predictive model for ceramic powder compaction we have investigated methods for characterizing density gradients in ceramic powder compacts, reviewed and compared existing compaction models, conducted compaction experiments on a spray dried alumina powder, and conducted mechanical tests and compaction experiments on model granular materials. Die filling and particle packing, and the behavior of individual granules play an important role in determining compaction behavior and should be incorporated into realistic compaction models. These results support the use of discrete element modeling techniques and statistical mechanics principals to develop a comprehensive model for compaction, something that should be achievable with computers with parallel processing capabilities.

  11. Determination of trace elements in high purity alumina powder by helium enhanced direct current glow discharge mass spectrometry

    NASA Astrophysics Data System (ADS)

    Jung, Sehoon; Kim, Sunhye; Hinrichs, Joachim

    2016-08-01

    Trace impurities in high purity alumina powder were determined by fast flow direct current glow discharge mass spectrometry (GD-MS). The non-conductive samples were prepared with high purity graphite powder and used as a sample binder and as a secondary cathode. To improve the sensitivity of the GD-MS analysis, helium was introduced as an additional glow discharge gas to argon plasma. The quantification results of the GD-MS measurement were calculated by external calibration with matrix matched certified reference materials. The GD-MS results for the determination of Na, Mg, Si, Ca, Ti, V, Cr, Fe, Cu, Zn and Ga in the alumina samples agreed well with the certified values of a reference material and the results of chemical analysis using wet sample digestion with inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS). The GD-MS analysis is a rapid analysis technique to determine trace elements in non-conductive alumina to below mg·kg- 1 levels.

  12. High-purity, fine-particle boron nitride powder synthesis at -75 to 750C. Report of investigations/1986

    SciTech Connect

    Kalyoncu, R.S.

    1986-01-01

    Nonoxide ceramics with improved high-temperature properties could substitute for high-temperature alloys and reduce the Nation's dependence on imports of Cr, Co, Ni, and Mn. To meet the objective, the Bureau of Mines conducted research to synthesize ultrafine reactive boron nitride (BN) powders. BN powders were prepared at temperatures ranging from -75 degrees to 750 degrees C. Low-temperature reactions (-75 to 200/sup 0/C) between boron halides and N compounds led to formation of elemento-organic compounds that were thermally decomposed to ultrafine (approximately 100- to 150-A particle size) reactive BN powders. BN powders were also prepared through the reaction of a low-melting inorganic B compound (boric acid, borax) with an organic N compound (carbimide and thiocarbimide) in N/sub 2/ and/or ammonia (NH/sub 3/) atmospheres at temperatures between 500 and 750/sup 0/C. The report is based upon work done under an agreement between the University of Alabama and the Bureau of Mines.

  13. Ceramic oxide powders and the formation thereof

    DOEpatents

    Katz, J.L.; Chenghung Hung.

    1993-12-07

    Ceramic oxide powders and a method for their preparation. Ceramic oxide powders are obtained using a flame process whereby two or more precursors of ceramic oxides are introduced into a counterflow diffusion flame burner wherein said precursors are converted into ceramic oxide powders. The morphology, particle size, and crystalline form of the ceramic oxide powders are determined by process conditions. 14 figures.

  14. Ceramic oxide powders and the formation thereof

    DOEpatents

    Katz, Joseph L.; Hung, Cheng-Hung

    1993-01-01

    Ceramic oxide powders and a method for their preparation. Ceramic oxide powders are obtained using a flame process whereby two or more precursors of ceramic oxides are introduced into a counterflow diffusion flame burner wherein said precursors are converted into ceramic oxide powders. The morphology, particle size, and crystalline form of the ceramic oxide powders are determined by process conditions.

  15. Synthesis of high purity gallium nitride powders and growth and characterization of aluminum nitride and gallium nitride bulk single crystals

    NASA Astrophysics Data System (ADS)

    Balkas, Cengiz Mustafa

    Single crystalline platelets of aluminum nitride (AlN) ≤ 1 mm thick have been grown within the range 1950-2250sp°C on silicon carbide (SiC) substrates via sublimation-recondensation in a resistively heated graphite furnace. The source material was sintered AlN. A maximum growth rate of 500 mum/hr was achieved at 2150sp°C and a source-to-seed separation of 4 mm. Crystals grown at high temperatures ranged in color from blue to green due to the incorporation of Si and C from the SiC substrates; those grown at lower temperatures were colorless and transparent. Secondary-ion mass spectroscopy (SIMS) results showed approximately a two order of magnitude decrease in the concentrations of these two impurities in the transparent crystals. X-ray diffraction (XRD), transmission electron microscopy (TEM) and Raman spectroscopy studies revealed low densities of line and planar defects and a strain free material. The synthesis of high purity, single phase GaN powders was accomplished in a hot wall tube furnace via (1) the reaction of Ga(l) with ammonia (NHsb3) and (2) the conversion of Gasb2Osb3(s). Polyhedra of various shapes were obtained from both processes; some rod-shaped crystals were also observed in the material derived from Gasb2Osb3. The GaN powders produced via the first route were characterized via XRD technique. The diffraction data revealed the material to be single phase with a = 3.1891 A, c = 5.1855 A, in space group P6sb3mc, Z = 2 and Dsb{x} = 6.0886 gr/cmsp3. Scanning electron microscopy revealed a particle size distribution in the ground material between 1 and 5 mum with most of the particles being {≈}1{mu}m. The data obtained in this study was chosen to be the new standard for the powder diffraction pattern for this material by the International Center for Diffraction Data. Single crystals of GaN up to 3 mm in length were grown by sublimation of pellets of this material under an NHsb3 flow. Typical green densities were 50 to 60% of theoretical density

  16. Ceramic powder for sintering materials

    NASA Technical Reports Server (NTRS)

    Akiya, H.; Saito, A.

    1984-01-01

    Surface activity of ceramic powders such as MgO and Al2O3, for use in sintering with sp. emphasis on their particle size, shape, particle size distribution, packing, and coexisting additives and impurities are reviewed.

  17. The self-propagation high-temperature synthesis (SHS) of ultrafine high purity tungsten powder from scheelite

    SciTech Connect

    Jung, J.C.; Ko, S.G.; Won, C.W.; Cho, S.S.; Chun, B.S.

    1996-07-01

    High-purity tungsten was prepared by self-propagating high-temperature synthesis (SHS) process from a mixture of CaO{center_dot}WO{sub 3} and Mg. The complete reduction of CaO{center_dot}WO{sub 3} required a 33{percent} excess of magnesium over the stoichiometric molar ratio Mg/CaO{center_dot}WO{sub 3} of 3:1. The MgO and CaO in the product was leached with an HCl solution. The product tungsten had a purity of 99.980{percent} which was higher than that of the reactants. The high purity results because the non tungsten reactants and products are volatilized by the high temperatures generated during the rapid exothermic SHS reaction and are dissolved during HCl leaching of the product. {copyright} {ital 1996 Materials Research Society.}

  18. Method for molding ceramic powders

    DOEpatents

    Janney, M.A.

    1990-01-16

    A method for molding ceramic powders comprises forming a slurry mixture including ceramic powder, a dispersant for the metal-containing powder, and a monomer solution. The monomer solution includes at least one multifunctional monomer, a free-radical initiator, and an organic solvent. The slurry mixture is transferred to a mold, and the mold containing the slurry mixture is heated to polymerize and crosslink the monomer and form a firm polymer-solvent gel matrix. The solid product may be removed from the mold and heated to first remove the solvent and subsequently remove the polymer, where after the product may be sintered.

  19. Method for molding ceramic powders

    DOEpatents

    Janney, Mark A.

    1990-01-01

    A method for molding ceramic powders comprises forming a slurry mixture including ceramic powder, a dispersant for the metal-containing powder, and a monomer solution. The monomer solution includes at least one multifunctional monomer, a free-radical initiator, and an organic solvent. The slurry mixture is transferred to a mold, and the mold containing the slurry mixture is heated to polymerize and crosslink the monomer and form a firm polymer-solvent gel matrix. The solid product may be removed from the mold and heated to first remove the solvent and subsequently remove the polymer, whereafter the product may be sintered.

  20. Agglomeration of ceramic powders

    NASA Technical Reports Server (NTRS)

    Cawley, James D.; Larosa, Judith; Dirkse, Fredrick

    1989-01-01

    A research program directed at a critical comparison of numerical models for power agglomeration with experimental observations is currently underway. Central to this program is the quantitative characterization of the distribution of mass within an agglomerate as a function of time. Current experiments are designed to restrict agglomeration to a surface, which is oriented perpendicular to the force of gravity. These experiments are discussed with reference to: their significance to ceramic processing; artifacts which may be avoided in microgravity experiments; and the comparison of information available in real space (from optical microscopy) to that in reciprocal space (from light scattering). The principle machine requirement appears to be a need to obtain information at small scattering angles.

  1. High purity tungsten targets

    NASA Technical Reports Server (NTRS)

    1975-01-01

    High purity tungsten, which is used for targets in X-ray tubes was considered for space processing. The demand for X-ray tubes was calculated using the growth rates for dental and medical X-ray machines. It is concluded that the cost benefits are uncertain.

  2. Screening and classification of ceramic powders

    NASA Technical Reports Server (NTRS)

    Miwa, S.

    1983-01-01

    A summary is given of the classification technology of ceramic powders. Advantages and disadvantages of the wet and dry screening and classification methods are discussed. Improvements of wind force screening devices are described.

  3. Hydroxyapatite ceramics from hydrothermally prepared powders

    SciTech Connect

    Lin, C.H.; Huang, C.W.; Chang, S.C.

    1994-12-31

    Hydroxyapatite (Ca{sub 5}(PO{sub 4}){sub 3}(OH)) is an effective material for artificial human bone production. Hydroxyapatite powders were hydrothermally produced in this work by reacting Ca(OH){sub 2} with Na{sub 3}PO{sub 4}{center_dot}12H{sub 2}O in an autoclave at various temperature and for various times. The particle size of hydroxyapatite was observed to be very fine, uniform, around 50 nm, as well as independent of reaction time. The hydroxyapatite powders were compacted and sintered at various temperatures for 2 hrs. The density, grain size, and hardness of the hydroxyapatite ceramics were measured and compared with those of the hydroxyapatite ceramics produced by the powders from the commercial source. The hydroxyapatite ceramics from the hydrothermal powders were found to have a higher density, smaller grain size, and higher hardness. After the hydroxyapatite ceramics were dipped in a simulated biological body liquid for 10 days, the density and hardness of the hydroxyapatite ceramics from the hydrothermal powders were less deteriorated than those of the hydroxyapatite ceramics from the commercial powder.

  4. Method for classifying ceramic powder

    NASA Technical Reports Server (NTRS)

    Takabe, K.

    1983-01-01

    Under the invented method, powder A of particles of less than 10 microns, and carrier powder B, whose average particle diameter is more than five times that of powder A, are premixed so that the powder is less than 40 wt.% of the total mixture, before classifying.

  5. Ceramic powder synthesis in supercritical fluids

    SciTech Connect

    Adkins, C.L.J.; Russick, E.M.; Cesarano, J; Tadros, M.E.; Voigt, J.A.

    1996-04-01

    Gas-phase processing plays an important role in the commercial production of a number of ceramic powders. These include titanium dioxide, carbon black, zinc oxide, and silicon dioxide. The total annual output of these materials is on the order of 2 million tons. The physical processes involved in gas-phase synthesis are typical of those involved in solution -phase synthesis: chemical reaction kinetics, mass transfer, nucleation, coagulation, and condensation. This report focuses on the work done under a Laboratory-Directed Research and Development (LDRD) project that explored the use of various high pressure techniques for ceramic powder synthesis. Under this project, two approaches were taken. First, a continuous flow, high pressure water reactor was built and studied for powder synthesis. And second, a supercritical carbon dioxide static reactor, which was used in conjunction with surfactants, was built and used to generate oxide powders.

  6. Counterflow diffusion flame synthesis of ceramic oxide powders

    DOEpatents

    Katz, Joseph L.; Miquel, Philippe F.

    1997-01-01

    Ceramic oxide powders and methods for their preparation are revealed. Ceramic oxide powders are obtained using a flame process whereby one or more precursors of ceramic oxides are introduced into a counterflow diffusion flame burner wherein the precursors are converted into ceramic oxide powders. The nature of the ceramic oxide powder produced is determined by process conditions. The morphology, particle size, and crystalline form of the ceramic oxide powders may be varied by the temperature of the flame, the precursor concentration ratio, the gas stream and the gas velocity.

  7. Counterflow diffusion flame synthesis of ceramic oxide powders

    DOEpatents

    Katz, J.L.; Miquel, P.F.

    1997-07-22

    Ceramic oxide powders and methods for their preparation are revealed. Ceramic oxide powders are obtained using a flame process whereby one or more precursors of ceramic oxides are introduced into a counterflow diffusion flame burner wherein the precursors are converted into ceramic oxide powders. The nature of the ceramic oxide powder produced is determined by process conditions. The morphology, particle size, and crystalline form of the ceramic oxide powders may be varied by the temperature of the flame, the precursor concentration ratio, the gas stream and the gas velocity. 24 figs.

  8. Slip casting nano-particle powders for making transparent ceramics

    DOEpatents

    Kuntz, Joshua D.; Soules, Thomas F.; Landingham, Richard Lee; Hollingsworth, Joel P.

    2011-04-12

    A method of making a transparent ceramic including the steps of providing nano-ceramic powders in a processed or unprocessed form, mixing the powders with de-ionized water, the step of mixing the powders with de-ionized water producing a slurry, sonifing the slurry to completely wet the powder and suspend the powder in the de-ionized water, separating very fine particles from the slurry, molding the slurry, and curing the slurry to produce the transparent ceramic.

  9. Apparatus for producing nanoscale ceramic powders

    DOEpatents

    Helble, Joseph J.; Moniz, Gary A.; Morse, Theodore F.

    1995-09-05

    An apparatus provides high temperature and short residence time conditions for the production of nanoscale ceramic powders. The apparatus includes a confinement structure having a multiple inclined surfaces for confining flame located between the surfaces so as to define a flame zone. A burner system employs one or more burners to provide flame to the flame zone. Each burner is located in the flame zone in close proximity to at least one of the inclined surfaces. A delivery system disposed adjacent the flame zone delivers an aerosol, comprising an organic or carbonaceous carrier material and a ceramic precursor, to the flame zone to expose the aerosol to a temperature sufficient to induce combustion of the carrier material and vaporization and nucleation, or diffusion and oxidation, of the ceramic precursor to form pure, crystalline, narrow size distribution, nanophase ceramic particles.

  10. Apparatus for producing nanoscale ceramic powders

    DOEpatents

    Helble, Joseph J.; Moniz, Gary A.; Morse, Theodore F.

    1997-02-04

    An apparatus provides high temperature and short residence time conditions for the production of nanoscale ceramic powders. The apparatus includes a confinement structure having a multiple inclined surfaces for confining flame located between the surfaces so as to define a flame zone. A burner system employs one or more burners to provide flame to the flame zone. Each burner is located in the flame zone in close proximity to at least one of the inclined surfaces. A delivery system disposed adjacent the flame zone delivers an aerosol, comprising an organic or carbonaceous carrier material and a ceramic precursor, to the flame zone to expose the aerosol to a temperature sufficient to induce combustion of the carrier material and vaporization and nucleation, or diffusion and oxidation, of the ceramic precursor to form pure, crystalline, narrow size distribution, nanophase ceramic particles.

  11. On the Effect of Local Grain-Boundary Chemistry on the Macroscopic Mechanical Properties of a High Purity Y2O3-Al2O3-Containing Silicon Nitride Ceramic: Role of Oxygen

    SciTech Connect

    Ziegler, A; McNaney, J M; Hoffman, M J; Ritchie, R O

    2004-11-23

    The effects of grain-boundary chemistry on the mechanical properties were investigated on high-purity silicon nitride ceramics, specifically involving the role of oxygen. Varying the grain-boundary oxygen content, by control of oxidizing heat treatments and sintering additives, was found to result in a transition in fracture mechanism from transgranular to intergranular fracture, with an associated increase in fracture toughness. This phenomenon is correlated to an oxygen-induced change in grain-boundary chemistry that appears to affect fracture by ''weakening'' the interface, facilitating debonding and crack advance along the boundaries, and consequently toughening by grain bridging. It is concluded that if the oxygen content in the thin grain-boundary films exceeds a lower limit, which is {approx}0.87 equiv% oxygen content, then the interfacial structure and bonding characteristics favor intergranular debonding during crack propagation; otherwise, transgranular fracture ensues.

  12. Production of high purity radiothallium

    DOEpatents

    Lebowitz, Elliot; Greene, Margaret W.

    1976-11-23

    The method of producing high purity thallium-201 for use as a myocardial scanning agent comprising the steps of irradiating a thallium target with protons to give the reaction .sup.203 Tl(p,3n) .sup.201.sub.Pb, separating in ion exchange columns the lead from the thallium isotopes, permitting the lead to decay, and then purifying the thallium solution and converting the thallium present to thallous form in which it can be used.

  13. Preparation of high purity phosphorus

    DOEpatents

    Rupp, Arthur F.; Woo, David V.

    1981-01-01

    High purity phosphorus and phosphorus compounds are prepared by first reacting H.sub.3 PO.sub.4 with a lead compound such as PbO to form Pb.sub.3 (PO.sub.4).sub.2. The Pb.sub.3 (PO.sub.4).sub.2 is reduced with H.sub.2 at a temperature sufficient to form gaseous phosphorus which can be recovered as a high purity phosphorus product. Phosphorus compounds can be easily prepared by reacting the phosphorus product with gaseous reactants. For example, the phosphorus product is reacted with gaseous Cl.sub.2 to form PCl.sub.5. PCl.sub.5 is reduced to PCl.sub.3 by contacting it in the gaseous phase with solid elemental phosphorus. POCl.sub.3 can be prepared by contacting PCl.sub.5 in the gaseous phase with solid P.sub.2 O.sub.5. The general process is particularly suitable for the preparation of radiophosphorus compounds.

  14. Synthesis and properties of high-purity alumina

    SciTech Connect

    Martin, E.S.; Weaver, M.L. . Chemical Systems Div.)

    1993-07-01

    High-purity alumina is intended primarily for the high-pressure sodium-vapor lamp envelope market and other specialty alumina applications such as abrasives, catalysts, and structural ceramics. High-purity alumina must calcine to Al[sub 2]O[sub 3] with minimal metal impurities ([>=]99.99% Al[sub 2]O[sub 3]). Sulfate and chloride impurities are also undesirable. High-purity alumina should have less than 20ppm alkali and alkaline-earth metals, and less than 10 ppm each in transition-metal impurities. A process for synthesizing alumina by converting pure aluminum metal to aluminum hydroxide and the resultant alumina properties are described.

  15. The modeling of the shock response of powdered ceramic materials

    NASA Astrophysics Data System (ADS)

    Rajendran, A. M.; Ashmawi, W. M.; Zikry, M. A.

    2006-06-01

    A two-cap constitutive model that incorporates inelastic yielding, frictional sliding, and densification was modified for shock-loading applications, and used to model shock-wave propagation of a powdered ceramic that is constrained by aluminum layers in a system, which is impacted by a flyer plate. The numerical results included analyses of the effects of shock stress amplitudes on densification, unloading behaviors, stress attenuation and dispersion, and stress and pressure distributions. An understanding of how interfacial impedances affect shock-front attenuation, dispersion, and propagation were obtained through modeling different shock-load conditions. The constitutive and computational models were validated with detailed simulations of shock-front experiments pertaining to powdered ceramics. It is shown how shock amplitude duration and rise time are related to stress evolution, and how physically limiting values result in inelastic damage. This analysis underscores how modeling with the appropriate constitutive description can provide insights on how powdered ceramics behave under impact-loading conditions.

  16. Laminated composite of magnetic alloy powder and ceramic powder and process for making same

    DOEpatents

    Moorhead, A.J.; Kim, H.

    1999-08-10

    A laminated composite structure of alternating metal powder layers, and layers formed of an inorganic bonding media powder, and a method for manufacturing same are disclosed. The method includes the steps of assembling in a cavity alternating layers of a metal powder and an inorganic bonding media of a ceramic, glass, and glass-ceramic. Heat, with or without pressure, is applied to the alternating layers until the particles of the metal powder are sintered together and bonded into the laminated composite structure by the layers of sintered inorganic bonding media to form a strong composite structure. The method finds particular application in the manufacture of high performance magnets wherein the metal powder is a magnetic alloy powder. 9 figs.

  17. Laminated composite of magnetic alloy powder and ceramic powder and process for making same

    DOEpatents

    Moorhead, Arthur J.; Kim, Hyoun-Ee

    1999-01-01

    A laminated composite structure of alternating metal powder layers, and layers formed of an inorganic bonding media powder, and a method for manufacturing same are discosed. The method includes the steps of assembling in a cavity alternating layers of a metal powder and an inorganic bonding media of a ceramic, glass, and glass-ceramic. Heat, with or without pressure, is applied to the alternating layers until the particles of the metal powder are sintered together and bonded into the laminated composite structure by the layers of sintered inorganic bonding media to form a strong composite structure. The method finds particular application in the manufacture of high performance magnets wherein the metal powder is a magnetic alloy powder.

  18. Ceramic fabrication process before firing-surface treatment of ceramic powder

    NASA Technical Reports Server (NTRS)

    Tsunoda, T.

    1984-01-01

    The surface treatment of powders is discussed. Stability of ceramic powders and surfaces and the improvement of moldability are addressed. Characteristics of surface treatment technology are given, including formation of inorganic surface-treated layers, liquid phase reactions, gas treatment, surface treatment by coupling agents, and the formation of results of surface treatment.

  19. Ceramic Inclusions In Powder Metallurgy Disk Alloys: Characterization and Modeling

    NASA Technical Reports Server (NTRS)

    Bonacuse, Pete; Kantzos, Pete; Telesman, Jack

    2002-01-01

    Powder metallurgy alloys are increasingly used in gas turbine engines, especially as the material chosen for turbine disks. Although powder metallurgy materials have many advantages over conventionally cast and wrought alloys (higher strength, higher temperature capability, etc.), they suffer from the rare occurrence of ceramic defects (inclusions) that arise from the powder atomization process. These inclusions can have potentially large detrimental effect on the durability of individual components. An inclusion in a high stress location can act as a site for premature crack initiation and thereby considerably reduce the fatigue life. Because these inclusions are exceedingly rare, they usually don't reveal themselves in the process of characterizing the material for a particular application (the cumulative volume of the test bars in a fatigue life characterization is typically on the order of a single actual component). Ceramic inclusions have, however, been found to be the root cause of a number of catastrophic engine failures. To investigate the effect of these inclusions in detail, we have undertaken a study where a known population of ceramic particles, whose composition and morphology are designed to mimic the 'natural' inclusions, are added to the precursor powder. Surface connected inclusions have been found to have a particularly large detrimental effect on fatigue life, therefore the volume of ceramic 'seeds' added is calculated to ensure that a minimum number will occur on the surface of the fatigue test bars. Because the ceramic inclusions are irregularly shaped and have a tendency to break up in the process of extrusion and forging, a method of calculating the probability of occurrence and expected intercepted surface and embedded cross-sectional areas were needed. We have developed a Monte Carlo simulation to determine the distributions of these parameters and have verified the simulated results with observations of ceramic inclusions found in macro

  20. APPARATUS FOR HIGH PURITY METAL RECOVERY

    DOEpatents

    Magel, T.T.

    1959-02-10

    An apparatus is described for preparing high purity metal such as uranium, plutonium and the like from an impure mass of the same metal. The apparatus is arranged so that the impure metal is heated and swept by a stream of hydrogen gas bearing a halogen such as iodine. The volatiie metal halide formed is carried on to a hot filament where the metal halide is decomposed and the molten high purity metal is collected in a rceeiver below

  1. Dimensional stability of high-purity Invar 36

    NASA Astrophysics Data System (ADS)

    Sokolowski, Witold M.; Jacobs, Stephen F.; Lane, Marc S.; O'Donnell, Timothy P.; Hsieh, Cheng

    1993-12-01

    High performance requirements for the Imaging Science Subsystem/Narrow Angle Camera (NAC) instrument on the NASA/Jet Propulsion Laboratory (JPL) Cassini spacecraft impose very stringent demands for dimensional stability of metering rods in the camera's athermalizing system. Invar 36 was chosen as a baseline material because it possibly could meet these requirements through high purity control and appropriate thermomechanical processes. A powder metallurgy process appears to be the manufacturing method to ensure high purity and cleanliness of this material. Therefore, a powder metallurgy manufacturer was contacted and high purity (HP) Invar 36 was produced per JPL engineering requirements. Several heat treatments were established and heat treated HP Invar 36 samples were evaluated. Coefficient of thermal expansion (CTE), thermal hysteresis and temporal stability test results are reported here. The test results indicate that JPL has succeeded in obtaining possibly the most dimensionally stable (lowest CTE plus lowest temporal change) Invar 36 material ever produced. CTE < 1 ppm/ degree(s)C are reported here along with temporal stability < 1 ppm/year. These dimensional stability properties will meet the requirements for metering rods on the NAC.

  2. Ceramic Inclusions in Powder Metallurgy Disk Alloys: Characterization and Modeling

    NASA Technical Reports Server (NTRS)

    Bonacuse, Peter J.

    2001-01-01

    Powder metallurgy alloys are increasingly used in gas turbine engines, especially in turbine disk applications. Although powder metallurgy materials have many advantages over conventionally cast and wrought alloys (higher strength, higher temperature capability, etc.), they suffer from the rare occurrence of ceramic defects (inclusions) that are inherent to the powder atomization process. These inclusions can have a potentially large detrimental effect on the durability of individual components. An inclusion in a high stress location can act as a site for premature crack initiation and thereby considerably reduce the fatigue life. Because these inclusions are exceedingly rare, they typically do not reveal themselves in the process of characterizing the material for a particular application (the cumulative volume of the test bars in a fatigue life characterization is typically on the order of a single actual component). Ceramic inclusions have, however, been found to be the root cause of a number of catastrophic engine failures. To investigate the effect of these inclusions in detail, we have undertaken a study where known populations of ceramic particles, whose composition and morphology are designed to mimic the "natural" inclusions, are added to the precursor powder. Surface-connected inclusions have been found to have a particularly large detrimental effect on fatigue life; therefore, the quantity of ceramic "seeds" added is calculated to ensure that a minimum number will intersect the surface of the fatigue test bars. Because the ceramic inclusions are irregularly shaped and have a tendency to break up in the process of extrusion and forging, a method of calculating the probability of occurrence and expected intercepted surface area was needed. We have developed a Monte Carlo simulation to determine the distributions of these parameters and have verified the simulated results with observations of ceramic inclusions found in macroscopic slices from extrusions

  3. Applied mechanics modeling of granulated ceramic powder compaction

    SciTech Connect

    Mahoney, F.M.; Readey, M.J.

    1995-08-01

    In ceramic manufacturing processes such as dry-pressing, correlations between applied compacting pressure and resultant powder compact density are essential for defining reliable process conditions for ceramic components. Pressure-density diagrams have been developed as a tool for both process control and for understanding the compaction behavior of different powders. These types of diagrams, however, pertain only to the averag@ properties of a powder compact and do not address a significant issue in powder compaction processes: the formation of density gradients within the compact. Continuum-based mechanics models of varying complexity have addressed the influence of frictional forces acting at the powder-die wall interface which dissipate the applied pressure throughout the compact. Resulting pressure distribution models are then typically coupled with empirical functions relating pressure and density to obtain a green density distribution in the compact. All of these models predict similar trends; however, none predict the distribution with sufficient accuracy to be considered as a design tool for industrial applications.

  4. Ceramics in gas turbine: Powder and process characterization

    NASA Technical Reports Server (NTRS)

    Dutta, S.

    1977-01-01

    Some of the intrinsic properties of various forms of Si3N4 and SiC are listed and limitations of such materials' availability are pointed out. The essential features/parameters to characterize a batch of powder are discussed including the standard techniques for such characterization. In process characterization, parameters in sintering, reaction sintering, and hot pressing processes are discussed including the factors responsible for strength limitations in ceramic bodies. Significant improvements in material properties can be achieved by reducing or eliminating the strength limiting factors with consistent powder and process characterization along with process control.

  5. Preparation of TEM samples for hard ceramic powders.

    PubMed

    Xu, Qiang; Kumar, Vikas; de Kruijff, Tom; Jansen, Jacob; Zandbergen, Henny W

    2008-12-01

    It is challenging to prepare a good sample for high-resolution electron microscopy of polycrystalline ceramic powders containing hard particles or particles with a strong preferential cleavage. Here we demonstrate that embedding the particles in a Cu matrix in a pressed pellet allows for straightforward conventional ion milling. The method is applied to powders of Mg10Ir19B16 and Na0.5CoO2 to show its feasibility, whereby transmission electron microscopy (TEM) samples with crystalline areas thinner than 10 nm can be obtained easily. PMID:18722061

  6. Ceramic Tool For Preconsolidation Of Powder-Coated Towpreg

    NASA Technical Reports Server (NTRS)

    Baucom, Robert M.; Sandusky, Donald A.; Marchello, Joseph M.

    1994-01-01

    Tool converts partly formed towpreg into preconsolidated towpreg ribbon. In technique, towpreg coated with thermoplastic powder converted into preconsolidated ribbon without use of plasticizers or solvents. Relying on melt flow and proper application of tension, friction, and cooling, technique ensures both consistent distribution of polymer within, and consistent cross section of ribbon. Ceramic preconsolidation tool includes heated and cooled halves thermally insulated from each other.

  7. Low temperature fabrication from nano-size ceramic powders

    SciTech Connect

    Gonzalez, E.J.; Piermarini, G.J.; Hockey, B.

    1995-06-01

    The objective of the compaction process is to produce a dense green-state compact from a nanosize powder that subsequently can be sintered at high temperatures to form a dense ceramic piece. High density in the green-state after pressing is of primary importance for achieving high densities after sintering. Investigation of the compaction behavior of ceramic powders, therefore, is an important part of characterization of raw ceramic powders and evaluation of their compaction behavior, analysis of interaction between particles, and the study of microstructure of green body (unsintered) during pressure-forming processes. The compaction of nanosize ceramic particles into high density green bodies is very difficult. For the nanosize materials used in this study (amorphous Si{sub 3}N{sub 4} and {gamma} Al{sub 2}O{sub 3}), there is no evidence by TEM of partial sintering after synthesis. Nevertheless, strong aggregation forces, such as the van der Waals surface forces of attraction, exist and result in moderate precursor particle agglomeration. More importantly, these attractive surface forces, which increase in magnitude with decreasing particle size, inhibit interparticle sliding necessary for particle rearrangement to denser bodies during subsequent compaction. Attempts to produce high density green body compacts of nanosize particles, therefore, generally have been focused on overcoming these surface forces of attraction by using either dispersive fluids or high pressures with or without lubricating liquids. In the present work, the use of high pressure has been employed as a means of compacting nanosize powders to relatively high green densities.

  8. High purity silane and silicon production

    NASA Technical Reports Server (NTRS)

    Breneman, William C. (Inventor)

    1987-01-01

    Silicon tetrachloride, hydrogen and metallurgical silicon are reacted at about 400.degree.-600.degree. C. and at pressures in excess of 100 psi, and specifically from about 300 up to about 600 psi to form di- and trichlorosilane that is subjected to disproportionation in the presence of an anion exchange resin to form high purity silane. By-product and unreacted materials are recycled, with metallurgical silicon and hydrogen being essentially the only consumed feed materials. The silane product may be further purified, as by means of activated carbon or cryogenic distillation, and decomposed in a fluid bed or free space reactor to form high purity polycrystalline silicon and by-product hydrogen which can be recycled for further use. The process results in simplified waste disposal operations and enhances the overall conversion of metallurgical grade silicon to silane and high purity silicon for solar cell and semiconductor silicon applications.

  9. Ceramics in gas turbines - Powder and process characterization

    NASA Technical Reports Server (NTRS)

    Dutta, S.

    1977-01-01

    The role of powder and process characterization in producing high quality silicon nitride and silicon carbide components, for gas turbine applications, is described. Some of the intrinsic properties of various forms of Si3N4 and SiC are listed and limitations of such materials' availability have been pointed out. The essential features/parameters to characterize a batch of powder have been discussed including the standard techniques for such characterization. In process characterization, parameters in sintering, reaction sintering, and hot pressing processes are discussed including the factors responsible for strength limitations in ceramic bodies. It is inevitable that significant improvements in material properties can be achieved by reducing or eliminating the strength limiting factors with consistent powder and process characterization along with process control.

  10. Manufacturing of transparent ZnS ceramics by powders sintering

    NASA Astrophysics Data System (ADS)

    Merdrignac-Conanec, O.; Hakmeh, N.; Durand, G.; Zhang, X.-H.

    2016-05-01

    We report the use of the low cost hot-pressing technique to produce ZnS for multispectral operation, from visible up to 12 μm. Considerable progress has been obtained by developing efficient precipitation and combustion powders synthesis procedures. The main emphasis has been on the elaboration of ZnS precursor powders with controlled morphology/chemical composition to reduce extrinsic scattering and impurities. We were able to produce ZnS parts with visible transparency and transmission in the 8-12 μm range that is comparable to that of CVD ZnS. The correlation of processing variables with powders sinterability and optical transmission of the HPed ceramics is discussed.

  11. A versatile powder production and collection system for rapidly solidified metal and ceramic powders

    NASA Astrophysics Data System (ADS)

    Khor, K. A.

    1992-08-01

    A versatile system is described which is capable of producing fine metal and ceramic powders using three different modes of a plasma solidification process: microatomization-plasma rapid solidification using air or inert gas as the quenching medium and plasma rapid solidification using water as the quenching medium. The testing and evaluation of the system is carried out using stainless steel 316 and yttria stabilized zirconia for microatomization experiments and alumina for other plasma solidification experiments. The microatomized powders are spherical with particle sizes ranging from 0.5 to 50 microns. The productivity of the pilot-scale system is 4 kg/hr.

  12. Preparation of γ-AlON transparent ceramics by one-step method with high-activity Al2O3 powders

    NASA Astrophysics Data System (ADS)

    Sun, Wenzhou; Chen, Yuhong; Wu, Laner; Jiang, Yong

    2013-06-01

    In this paper, γ-AlON transparent ceramics are fabricated by one-step method—reactived hot-pressuring sintering technology by using as-prepared γ-Al2O3 powder as raw material. And the sintering process is also improved from two aspects: adjusting sintered technique parameters and improving the sintering agents. XRD, SEM, ICP-AES analysis results show that as-prepared γ-Al2O3 powders have advantages of super-fine, high-purity and high-activity so that can meet the requirements of starting material. By adding 1wt% Y2O3 as sintering agent, single-phase γ-AlON transparent ceramic can be fabricated under the optimum technological condition: hot-pressure sintering at 1950°C for 6h, under nitrogen atmosphere. The results from XRD and SEM indicate that the γ-AlON ceramic has high density and fine microstructures with relative density of 99.22%. The test result of IR spectrum show that the ceramic yield the best transmittance of 18.42% at 2.5μm and its transmitting wavelength range extend from 1.5 to 4.5μm.

  13. High purity silica reflecting heat shield development

    NASA Technical Reports Server (NTRS)

    Congdon, W.

    1974-01-01

    A reflecting heat shield composed of fused silica in which the scattering results from the refractive index mismatch between silica particles and the voids introduced during the fabrication process is developed. Major considerations and conclusions of the development are: the best material to use is Type A, which is capable of ultra-high-purity and which does not show the 0.243 micrometer absorption band; the reflection efficiency of fused silica is decreased at higher temperatures due to the bathochromic shift of the ultraviolet cut-off; for a given silica material, over the wavelength region and particle sizes tested, the monodisperse particle size configurations produce higher reflectances than continuous particle size configurations; and the smaller monodisperse particle size configurations give higher reflectance than the larger ones. A reflecting silica configuration that is an efficient reflector of shock layer radiation at high ablation temperatures is achieved by tailoring the matrix for optimum scattering and using an ultra-high-purity material.

  14. Derivation of high-purity oligodendroglial progenitors.

    PubMed

    Hatch, Maya N; Nistor, Gabriel; Keirstead, Hans S

    2009-01-01

    Oligodendrocytes are a type of glial cells that play a critical role in supporting the central nervous system (CNS), in particular insulating axons within the CNS by wrapping them with a myelin sheath, thereby enabling saltatory conduction. They are lost, and myelin damaged - demyelination - in a wide variety of neurological disorders. Replacing depleted cell types within demyelinated areas, however, has been shown experimentally to achieve remyelination and so help restore function. One method to produce oligodendrocytes for cellular replacement therapies is through the use of progenitor or stem cells. The ability to differentiate progenitor or stem cells into high-purity fates not only permits the generation of specific cells for transplantation therapies, but also provides powerful tools for studying cellular mechanisms of development. This chapter outlines methods of generating high-purity OPCs from multipotent neonatal progenitor or human embryonic stem cells. PMID:19378196

  15. Method of high purity silane preparation

    DOEpatents

    Tsuo, Y. Simon; Belov, Eugene P.; Gerlivanov, Vadim G.; Zadde, Vitali V.; Kleschevnikova, Solomonida I.; Korneev, Nikolai N.; Lebedev, Eugene N.; Pinov, Akhsarbek B.; Ryabenko, Eugene A.; Strebkov, Dmitry S.; Chernyshev, Eugene A.

    2000-01-01

    A process for the preparation of high purity silane, suitable for forming thin layer silicon structures in various semiconductor devices and high purity poly- and single crystal silicon for a variety of applications, is provided. Synthesis of high-purity silane starts with a temperature assisted reaction of metallurgical silicon with alcohol in the presence of a catalyst. Alcoxysilanes formed in the silicon-alcohol reaction are separated from other products and purified. Simultaneous reduction and oxidation of alcoxysilanes produces gaseous silane and liquid secondary products, including, active part of a catalyst, tetra-alcoxysilanes, and impurity compounds having silicon-hydrogen bonds. Silane is purified by an impurity adsorption technique. Unreacted alcohol is extracted and returned to the reaction with silicon. Concentrated mixture of alcoxysilanes undergoes simultaneous oxidation and reduction in the presence of a catalyst at the temperature -20.degree. C. to +40.degree. C. during 1 to 50 hours. Tetra-alcoxysilane extracted from liquid products of simultaneous oxidation and reduction reaction is directed to a complete hydrolysis. Complete hydrolysis of tetra-alcoxysilane results in formation of industrial silica sol and alcohol. Alcohol is dehydrated by tetra-alcoxysilane and returned to the reaction with silicon.

  16. Physico-chemistry and cytotoxicity of ceramics: part I: characterization of ceramic powders.

    PubMed

    Dion, I; Rouais, F; Baquey, C; Lahaye, M; Salmon, R; Trut, L; Cazorla, J P; Huong, P V; Monties, J R; Havlik, P

    1997-05-01

    The morphology of Al2O3, ZrO2/Y2O3, AIN, B4C, BN, SiC, Si3N4, TiB2, TiC, TiN ceramic, graphite and diamond powders has been studied by scanning electron microscopy (SEM) and the specific area of each powder was determined with the BET method. X-ray diffraction (XRD) investigations have been carried out in order to evaluate the crystallinity and determine the constitutive phases. The chemical composition was assessed by classical chemical analyses and by X-ray microprobe; some powders were studied by the laser micro-Raman technique. Correlations have been established between all these results. PMID:15348756

  17. Hot Superplastic Powder Forging for Transparent nanocrystalline Ceramics

    SciTech Connect

    Cannon, W. Roger

    2006-05-22

    The program explored a completely new, economical method of manufacturing nanocrystalline ceramics, Hot Superplastic Powder Forging (HSPF). The goal of the work was the development of nanocrystalline/low porosity optically transparent zirconia/alumina. The high optical transparency should result from lack of grain boundary scattering since grains will be smaller than one tenth the wavelength of light and from elimination of porosity. An important technological potential for this process is manufacturing of envelopes for high-pressure sodium vapor lamps. The technique for fabricating monolithic nanocrystalline material does not begin with powder whose particle diameter is <100 nm as is commonly done. Instead it begins with powder whose particle diameter is on the order of 10-100 microns but contains nanocrystalline crystallites <<100 nm. Spherical particles are quenched from a melt and heat treated to achieve the desired microstructure. Under a moderate pressure within a die or a mold at temperatures of 1100C to 1300C densification is by plastic flow of superplastic particles. A nanocrystalline microstructure results, though some features are greater than 100nm. It was found, for instance, that in the fully dense Al2O3-ZrO2 eutectic specimens that a bicontinuous microstructure exists containing <100 nm ZrO2 particles in a matrix of Al2O3 grains extending over 1-2 microns. Crystallization, growth, phase development and creep during hot pressing and forging were studied for several compositions and so provided some details on development of polycrystalline microstructure from heating quenched ceramics.

  18. High-purity thermoacoustic isotope enrichment.

    PubMed

    Swift, G W; Geller, D A; Backhaus, S N

    2014-08-01

    In a tube many wavelengths long, thermoacoustic separation of a gas mixture can produce very high purities. A flexible wall allows a spatially continuous supply of acoustic power into such a long tube. Coiling the tube and immersing it in a fluid lets a single-wavelength, circulating, traveling pressure wave in the fluid drive all the wavelengths in the tube wall and gas. Preliminary measurements confirm many aspects of the concept with neon ((20)Ne and (22)Ne) and highlight some challenges of practical implementation. PMID:25096099

  19. Method for preparing high purity vanadium

    DOEpatents

    Schmidt, Frederick; Carlson, O. Norman

    1986-09-09

    A method for preparing high purity vanadium having a low silicon content has been developed. Vanadium pentoxide is reduced with a stoichiometric, or slightly deficient amount of aluminum to produce a vanadium-aluminum alloy containing an excess of oxygen. Silicon is removed by electron-beam melting the alloy under oxidizing conditions to promote the formation of SiO which is volatile at elevated temperatures. Excess oxygen is removed by heating the alloy in the presence of calcium metal to form calcium oxide.

  20. Method for preparing high purity vanadium

    DOEpatents

    Schmidt, F.; Carlson, O.N.

    1984-05-16

    A method for preparing high purity vanadium having a low silicon content has been developed. Vanadium pentoxide is reduced with a stoichiometric, or slightly deficient amount of aluminum to produce a vanadium-aluminum alloy containing an excess of oxygen. Silicon is removed by electron-beam melting the alloy under oxidizing conditions to promote the formation of SiO which is volatile at elevated temperatures. Excess oxygen is removed by heating the alloy in the presence of calcium metal to form calcium oxide.

  1. Zirconia-based powders and properties of sintered ceramics for biomedical applications

    NASA Astrophysics Data System (ADS)

    Kulkov, S.; Buyakova, S.

    2015-11-01

    Porous ceramics obtained from ultra-fine powders have been studied. The porosity of ceramic samples was from 15 to 80 %. The structure of the ceramic materials was a cellular structure. A distinctive feature of all the deformation diagram obtained in the experiment was their nonlinearity at low deformations which was described by the parabolic law. It was shown that the observed nonlinear elasticity for low deformations on deformation diagrams is due to mechanical instability of the cellular elements in the ceramic carcass.

  2. High purity silica reflective heat shield development

    NASA Technical Reports Server (NTRS)

    Nachtscheim, P. R.; Blome, J. C.

    1976-01-01

    A hyperpure vitreous silica material is being developed for use as a reflective and ablative heat shield for planetary entry. Various purity grades and forms of raw materials were evaluated along with various processing methods. Slip casting of high purity grain was selected as the best processing method, resulting in a highly reflective material in the wavelength bands of interest (the visible and ultraviolet regions). The selected material was characterized with respect to optical, mechanical and physical properties using a limited number of specimens. The process has been scaled up to produce a one-half scale heat shield (18 in. dia.) (45.72 cm) for a Jupiter entry vehicle. This work is now being extended to improve the structural safety factor of the heat shield by making hyperpure silica material tougher through the addition of silica fibers.

  3. Workshop on Preserving High Purity Uranium-233

    SciTech Connect

    Krichinsky, Alan M; Giaquinto, Joseph; Canaan, R Douglas {Doug}

    2016-01-01

    A workshop was held on at the MARC X conference to provide a forum for the scientific community to communicate needs for high-purity 233U and its by-products in order to preserve critical items otherwise slated for downblending and disposal. Currently, only a small portion of the U.S. holdings of separated 233U is being preserved. However, many additional kilograms of 233U (>97% pure) still are destined to be downblended which will permanently destroy their potential value for many other applications. It is not likely that this material will ever be replaced due to a lack of operating production capability. Summaries of information conveyed at the workshop and feedback obtained from the scientific community are presented herein.

  4. Processing to obtain high-purity gallium

    NASA Astrophysics Data System (ADS)

    Bautista, Renato G.

    2003-03-01

    Gallium has become increasingly popular as a substrate material for electronic devices. Aside from ore, gallium can be obtained from such industrial sources as the Bayer process caustic liquor that is a byproduct of bauxite processing, flue dust removed from the fume-collection system in plants that produce aluminum by the electrolytic process, zinc refinery residues, gallium scrap materials, and coal fly ash. The purification process for gallium can start with solvent-extraction processes where the concentrations of impurities, especially metals, are reduced to the ppm range. This article describes how ultra-purification techniques can be employed to reduce the undesirable impurities to the low ppb range. The various procedures described give an idea as to the extent of work needed to obtain and prepare high-purity gallium for electronic application.

  5. Dynamic shear deformation in high purity Fe

    SciTech Connect

    Cerreta, Ellen K; Bingert, John F; Trujillo, Carl P; Lopez, Mike F; Gray, George T

    2009-01-01

    The forced shear test specimen, first developed by Meyer et al. [Meyer L. et al., Critical Adiabatic Shear Strength of Low Alloyed Steel Under Compressive Loading, Metallurgical Applications of Shock Wave and High Strain Rate Phenomena (Marcel Decker, 1986), 657; Hartmann K. et al., Metallurgical Effects on Impact Loaded Materials, Shock Waves and High Strain rate Phenomena in Metals (Plenum, 1981), 325-337.], has been utilized in a number of studies. While the geometry of this specimen does not allow for the microstructure to exactly define the location of shear band formation and the overall mechanical response of a specimen is highly sensitive to the geometry utilized, the forced shear specimen is useful for characterizing the influence of parameters such as strain rate, temperature, strain, and load on the microstructural evolution within a shear band. Additionally, many studies have utilized this geometry to advance the understanding of shear band development. In this study, by varying the geometry, specifically the ratio of the inner hole to the outer hat diameter, the dynamic shear localization response of high purity Fe was examined. Post mortem characterization was performed to quantify the width of the localizations and examine the microstructural and textural evolution of shear deformation in a bcc metal. Increased instability in mechanical response is strongly linked with development of enhanced intergranular misorientations, high angle boundaries, and classical shear textures characterized through orientation distribution functions.

  6. High-purity silicon crystal growth investigations

    NASA Technical Reports Server (NTRS)

    Ciszek, T. F.; Schuyler, T.; Hurd, J. L.; Fearheiley, M.; Evans, C.; Elder, R.

    1986-01-01

    Information is given on evaporation and segregation contributions to impurity profiles of floating zone crystals (FZ); high-purity silicon float zoning (FZ); minority-carrier lifetime measurement of heavily doped silicon crystals; the effect of some crystal growth parameters on minority-carrier lifetime; and defect investigations by X-ray topography in graphical and tabular form. It was concluded that evaporation contributes substantially to impurity reduction when FZ or cold-crucible growth is conducted in a vacuum; boron and gallium may be more favorable dopants than indium or aluminum for obtaining high minority-carrier lifetimes; minority-carrier lifetimes greater than 100 microseconds are feasible at a 2 times 10 to the 17th power cm-3 doping level; minority-carrier lifetime decreases with increasing crystal cooling rate and also with the presence of dislocations; the method used to clean silicon feed rods affects lifetime; and microdefect densities in dislocation-free FZ crystals appear to be lower with Ga doping than with B doping.

  7. Biaxial deformation in high purity aluminum

    DOE PAGESBeta

    Livescu, V.; Bingert, J. F.; Liu, C.; Lovato, M. L.; Patterson, B. M.

    2015-09-25

    The convergence of multiple characterization tools has been applied to investigate the relationship of microstructure on damage evolution in high purity aluminum. The extremely coarse grain size of the disc-shaped sample provided a quasi-two dimensional structure from which the location of surface-measured features could be inferred. In particular, the role of pre-existing defects on damage growth was accessible due to the presence of casting porosity in the aluminum. Micro tomography, electron backscatter diffraction, and digital image correlation were applied to interrogate the sample in three dimensions. Recently micro-bulge testing apparatus was used to deform the pre-characterized disc of aluminum inmore » biaxial tension, and related analysis techniques were applied to map local strain fields. Subsequent post-mortem characterization of the failed sample was performed to correlate structure to damaged regions. We determined that strain localization and associated damage was most strongly correlated with grain boundary intersections and plastic anisotropy gradients between grains. Pre-existing voids played less of an apparent role than was perhaps initially expected. Finally, these combined techniques provide insight to the mechanism of damage initiation, propagation, and failure, along with a test bed for predictive damage models incorporating anisotropic microstructural effects.« less

  8. Biaxial deformation in high purity aluminum

    SciTech Connect

    Livescu, V.; Bingert, J. F.; Liu, C.; Lovato, M. L.; Patterson, B. M.

    2015-09-25

    The convergence of multiple characterization tools has been applied to investigate the relationship of microstructure on damage evolution in high purity aluminum. The extremely coarse grain size of the disc-shaped sample provided a quasi-two dimensional structure from which the location of surface-measured features could be inferred. In particular, the role of pre-existing defects on damage growth was accessible due to the presence of casting porosity in the aluminum. Micro tomography, electron backscatter diffraction, and digital image correlation were applied to interrogate the sample in three dimensions. Recently micro-bulge testing apparatus was used to deform the pre-characterized disc of aluminum in biaxial tension, and related analysis techniques were applied to map local strain fields. Subsequent post-mortem characterization of the failed sample was performed to correlate structure to damaged regions. We determined that strain localization and associated damage was most strongly correlated with grain boundary intersections and plastic anisotropy gradients between grains. Pre-existing voids played less of an apparent role than was perhaps initially expected. Finally, these combined techniques provide insight to the mechanism of damage initiation, propagation, and failure, along with a test bed for predictive damage models incorporating anisotropic microstructural effects.

  9. High-purity germanium crystal growing

    SciTech Connect

    Hansen, W.L.; Haller, E.E.

    1982-10-01

    The germanium crystals used for the fabrication of nuclear radiation detectors are required to have a purity and crystalline perfection which is unsurpassed by any other solid material. These crystals should not have a net electrically active impurity concentration greater than 10/sup 10/cm/sup -3/ and be essentially free of charge trapping defects. Such perfect crystals of germanium can be grown only because of the highly favorable chemical and physical properties of this element. However, ten years of laboratory scale and commercial experience has still not made the production of such crystals routine. The origin and control of many impurities and electrically active defect complexes is now fairly well understood but regular production is often interrupted for long periods due to the difficulty of achieving the required high purity or to charge trapping in detectors made from crystals seemingly grown under the required conditions. The compromises involved in the selection of zone refining and crystal grower parts and ambients is discussed and the difficulty in controlling the purity of key elements in the process is emphasized. The consequences of growing in a hydrogen ambient are discussed in detail and it is shown how complexes of neutral defects produce electrically active centers.

  10. Ultrastructure processing of advanced ceramics

    SciTech Connect

    Mackenzie, J.D.; Ulrich, D.R.

    1988-01-01

    Experimental investigations and applications of advanced ceramics are discussed in reviews and reports presented at the Third International Conference on Ultrastructure Processing of Ceramics, Glasses, and Composites held in San Diego in February 1987. Sections are devoted to precursors and chemistry for ultrastructure processing; sol-gel science and technology; powders and colloids; advanced ceramics; and composites, new materials, and techniques. Particular attention is given to silicon oxynitride and sialon ceramics from organosilicon powders, fluoropolymer-modified silicate glasses, Raman and FTIR spectroscopy of rapid sol-gel processes, a low-temperature route to high-purity Ti/Zr/Hf diboride powders and films, and sol-gel methods for SiO2 optical-fiber coatings. Diagrams, drawings, graphs, micrographs, and tables of numerical data are included.

  11. Characterization of composite materials based on cement-ceramic powder blended binder

    NASA Astrophysics Data System (ADS)

    Kulovaná, Tereza; Pavlík, Zbyšek

    2016-06-01

    Characterization of newly developed composite mortars with incorporated ceramic powder coming from precise brick cutting as partial Portland cement replacement up to 40 mass% is presented in the paper. Fine ceramic powder belongs to the pozzolanic materials. Utilization of pozzolanic materials is accompanied by lower request on energy needed for Portland clinker production which generally results in lower production costs of blended binder and lower CO2 emission. In this paper, the ceramic powder is used in cement based mortar composition in amount of 8, 16, 24, 32, and 40 mass% of cement. Chemical composition of ceramic powder is analyzed by X-Ray Fluorescence and X-Ray Diffraction. The particle size distribution of ceramics is accessed on laser diffraction principle. For 28 days cured mortar samples, basic physical and mechanical properties are experimentally determined. The obtained results demonstrate that ceramic powder has potential to replace a part of Portland cement in composition of cement based composites and to reduce negative environmental impact of their production.

  12. Fabrication of Fine-Grained Positive Temperature Coefficient Ceramics from Chemically Prepared Powder

    NASA Astrophysics Data System (ADS)

    Deguchi, Takeshi; Sumiyama, Tomoko; Yamaguchi, Iwao; Kinugasa, Masanori; Igarashi, Hideji

    1991-09-01

    Fine barium titanate powders were prepared by chemical synthesis to fabricate positive temperature coefficient ceramics. The calcining condition adapted for the chemical powder was experimentally determined to be a lower temperature than that for conventional powders. Microstructure and temperature dependence of resistivity of the fired samples were examined as a function of firing temperature. Niobium ions doped at a synthesizing stage of barium titanate were homogeneously diffused into a titanium lattice at a low temperature of 1150°C, and fine-grained PTC ceramics with grain sizes of 2˜3 μm were fabricated at that temperature.

  13. Characterization of ceramic powders by an X-ray measuring method

    NASA Technical Reports Server (NTRS)

    Ziegler, B.

    1983-01-01

    X-ray line broadening analysis gives quantitative data on structural changes of ceramic powders after different processing steps. Various Al2O3 powders were investigated and the following points are discussed on the basis of these results: X-ray line broadening analysis, structural changes during grinding, structural changes during annealing, influence of structural properties on sintering behavior and application of line broadening analysis to quality control of powders.

  14. The influence of granulated powder temporary organics composition on ceramic structure and properties

    NASA Astrophysics Data System (ADS)

    Veselov, S.; Belousova, N.; Zamyatina, A.; Sokolov, I.; Felofyanova, A.

    2016-04-01

    The influence of granulated powder binder/plasticizer ratio on epy microstructure and properties of sintered ceramic specimens is shown using submicron alumina. The fracture mode, microstructure and properties analyses of a green part and sintered samples obtained with different organic ratio contained in granulated powder are presented. It was stated that the usage of PVA (grade 16/1) and PEG 400 at an equal ratio results in a uniform distribution of granulated powder in a die and high green density. It is also shown that an addition of 2 wt. % of PVA and 2 wt. % of PEG400 into granules of ceramic press powder allows obtaining A1203 ceramic with apparent density of about 3,91 g/cm3 and bending strength of up to 410 MPa.

  15. High-purity silicon for solar cell applications

    NASA Technical Reports Server (NTRS)

    Dosaj, V. D.; Hunt, L. P.; Schei, A.

    1978-01-01

    The article discusses the production of solar cells from high-purity silicon. The process consists of reducing the level of impurities in the raw materials, preventing material contamination before and after entering the furnace, and performing orders-of-magnitude reduction of metal impurity concentrations. The high-purity raw materials are considered with reference to carbon reductants, silica, and graphite electrodes. Attention is also given to smelting experiments used to demonstrate, in an experimental-scale furnace, the production of high-purity SoG-Si. It is found that high-purity silicon may be produced from high-purity quartz and chemically purified charcoal in a 50-kVA arc furnace. The major contamination source is shown to be impurities from the carbon reducing materials.

  16. Targets for producing high purity I-123

    NASA Technical Reports Server (NTRS)

    Blue, J. W. (Inventor)

    1978-01-01

    Tellurium powder in improved targets is bombarded with a cyclotron beam to produce Xe-123. Flowing gas streams carry the Xe-123 through one cold trap which removes Xe-123 that subsequently decays to I-123. During this bombardment energy is deposited in the target material causing its temperature to rise. Some of the tellurium vaporizes and subsequently condenses on surfaces that are cooler than the vaporization temperature. Provision is made for the repeated bombardment of this condensed tellurium.

  17. Compaction of Ceramic Microspheres, Spherical Molybdenum Powder and Other Materials to 3 GPa

    SciTech Connect

    Carlson, S R; Bonner, B P; Ryerson, F J; Hart, M M

    2006-01-27

    Pressure-volume relationships were measured at room temperature for eight granular materials and one specimen of epoxy foam. The granular materials included hollow ceramic microspheres, spherical molybdenum powder, Ottawa sand, aluminum, copper, titanium and silicon carbide powders and glassy carbon spheres. Measurements were made to 0.9 GPa in a liquid medium press for all of the granular materials and to 3 GPa in a solid medium press for the ceramic microspheres and molybdenum powder. A single specimen of epoxy foam was compressed to 30 MPa in the liquid medium press. Bulk moduli were calculated as a function of pressure for the ceramic microspheres, the molybdenum powder and three other granular materials. The energy expended in compacting the granular materials was determined by numerically integrating pressure-volume curves. More energy was expended per unit volume in compacting the molybdenum powder to 1 GPa than for the other materials, but compaction of the ceramic microspheres required more energy per gram due to their very low initial density. The merge pressure, the pressure at which all porosity is removed, was estimated for each material by plotting porosity against pressure on a semi-log plot. The pressure-volume curves were then extrapolated to the predicted merge pressures and numerically integrated to estimate the energy required to reach full density for each material. The results suggest that the glassy carbon spheres and the ceramic microspheres would require more energy than the other materials to attain full density.

  18. Ultra high purity, dimensionally stable INVAR 36

    NASA Technical Reports Server (NTRS)

    Sokolowski, Witold M. (Inventor); Lane, Marc S. (Inventor); Hsieh, Cheng H. (Inventor); Odonnell, Timothy P. (Inventor)

    1995-01-01

    An INVAR 36 material having long-term dimensional stability is produced by sintering a blend of powders of nickel and iron under pressure in an inert atmosphere to form an alloy containing less than 0.01 parts of carbon and less than 0.1 part aggregate and preferably 0.01 part individually of Mn, Si, P, S and Al impurities. The sintered alloy is heat treated and slowly and uniformly cooled to form a material having a coefficient of thermal expansion of less than 1 ppm/C and a temporal stability of less than 1 ppm/year.

  19. Ultra high purity, dimensionally stable INVAR 36

    NASA Technical Reports Server (NTRS)

    Sokolowski, Witold M. (Inventor); Lane, Marc S. (Inventor); Odonnell, Timothy P. (Inventor); Hsieh, Cheng H. (Inventor)

    1994-01-01

    An INVAR 36 material having long-term dimensional stability is produced by sintering a blend of powders of nickel and iron under pressure in an inert atmosphere to form an alloy containing less than 0.01 parts of carbon and less than 0.1 part aggregate and preferably 0.01 part individually of Mn, Si, P, S and Al impurities. The sintered alloy is heat treated and slowly and uniformly cooled to form a material having a coefficient of thermal expansion of less than 1 ppm/C and a temporal stability of less than 1 ppm/year.

  20. Process for producing high purity silicon nitride by the direct reaction between elemental silicon and nitrogen-hydrogen liquid reactants

    DOEpatents

    Pugar, E.A.; Morgan, P.E.D.

    1987-09-15

    A process is disclosed for producing, at a low temperature, a high purity reaction product consisting essentially of silicon, nitrogen, and hydrogen which can then be heated to produce a high purity alpha silicon nitride. The process comprises: reacting together a particulate elemental high purity silicon with a high purity nitrogen-hydrogen reactant in its liquid state (such as ammonia or hydrazine) having the formula: N/sub n/H/sub (n+m)/ wherein: n = 1--4 and m = 2 when the nitrogen-hydrogen reactant is straight chain, and 0 when the nitrogen-hydrogen reactant is cyclic. High purity silicon nitride can be formed from this intermediate product by heating the intermediate product at a temperature of from about 1200--1700/degree/C for a period from about 15 minutes up to about 2 hours to form a high purity alpha silicon nitride product. The discovery of the existence of a soluble Si/endash/N/endash/H intermediate enables chemical pathways to be explored previously unavailable in conventional solid-state approaches to silicon-nitrogen ceramics

  1. Process for producing high purity silicon nitride by the direct reaction between elemental silicon and nitrogen-hydrogen liquid reactants

    DOEpatents

    Pugar, Eloise A.; Morgan, Peter E. D.

    1990-01-01

    A process is disclosed for producing, at a low temperature, a high purity reaction product consisting essentially of silicon, nitrogen, and hydrogen which can then be heated to produce a high purity alpha silicon nitride. The process comprises: reacting together a particulate elemental high purity silicon with a high purity nitrogen-hydrogen reactant in its liquid state (such as ammonia or hydrazine) having the formula: N.sub.n H.sub.(n+m) wherein: n=1-4 and m=2 when the nitrogen-hydrogen reactant is straight chain, and 0 when the nitrogen-hydrogen reactant is cyclic. High purity silicon nitride can be formed from this intermediate product by heating the intermediate product at a temperature of from about 1200.degree.-1700.degree. C. for a period from about 15 minutes up to about 2 hours to form a high purity alpha silicon nitride product. The discovery of the existence of a soluble Si-N-H intermediate enables chemical pathways to be explored previously unavailable in conventional solid state approaches to silicon-nitrogen ceramics.

  2. Powder Processing of Fiber-Reinforced Ceramics: Strengthening of the Powder Matrix Without Shrinkage. Ph.D. Thesis

    SciTech Connect

    Tu, Wen-chiang

    1994-01-01

    Powder processing of fiber-reinforced ceramic matrix composites is limited by constrained densification if the powder matrix is allowed to shrink during heat treatment. This produces large, strength-limiting crack-like voids. The objective of this study was to avoid this damage phenomenon by strengthening the powder matrix without shrinkage by using the cyclic infiltration/pyrolysis of ceramic liquid precursors. The following issues were addressed: (1) liquid precursor infiltration kinetics, (2) microstructural development during heat treatment, and (3) the mechanical properties of the porous bodies thus produced. Si3N4 powder matrices were infiltrated with either Zr(Y)-nitrate, which produces ZrO2, or polysilazane, which converts to Si3N4 during pyrolysis. Infiltration kinetics were shown to depend on the permeability of the powder compact, as well as that of the intruded material developed after heat treatment. The large volume changes during precursor pyrolysis is manifested by the formation of randomly distributed voids, which coalesce at higher temperatures. In this study, the powder matrix cannot be made fully dense; its fracture toughness was found to increase proportionally with the fraction of filled porosity and with the fracture toughness of the intruded material. The fracture strength appeared to follow the same trend. However, relatively strong bodies can be obtained despite high porosity, provided that the strength-limiting flaws are small. Large cracks are introduced in the powder matrix during infiltration if a layer of precursor remains on the surface. Cracks which develop in the precursor layer can extend into the matrix. Fracture mechanisms of thin films-on-substrates under residual thermal stress were used to explain this phenomenon. Matrix damage can be avoided by removing the precursor layer prior to pyrolysis and/or by strengthening the powder compact before infiltration.

  3. Production of High Purity Niobium Ingots at CBMM

    SciTech Connect

    Moura, Lourenco de; Faria Sousa, Clovis Antonio de; Burgos Cruz, Edmundo

    2011-03-31

    CBMM is a fully integrated company, from the mine to the end line of the production chain, supplying different niobium products to the world market: ferroniobium, nickelniobium, niobium pentoxide and high purity metallic niobium. This high purity metallic niobium has long been known to exhibit superconductivity below 9.25 Kelvin. This characteristic has the potential to bring technological benefits for many different areas such as medicine, computing and environment. This paper presents the raw material requirements as well as CBMM experience on producing high purity niobium ingots. The results prove that CBMM material can be the best solution for special applications such as low cost superconductive radiofrequency cavities.

  4. DSC and TG Analysis of a Blended Binder Based on Waste Ceramic Powder and Portland Cement

    NASA Astrophysics Data System (ADS)

    Pavlík, Zbyšek; Trník, Anton; Kulovaná, Tereza; Scheinherrová, Lenka; Rahhal, Viviana; Irassar, Edgardo; Černý, Robert

    2016-03-01

    Cement industry belongs to the business sectors characteristic by high energy consumption and high {CO}2 generation. Therefore, any replacement of cement in concrete by waste materials can lead to immediate environmental benefits. In this paper, a possible use of waste ceramic powder in blended binders is studied. At first, the chemical composition of Portland cement and ceramic powder is analyzed using the X-ray fluorescence method. Then, thermal and mechanical characterization of hydrated blended binders containing up to 24 % ceramic is carried out within the time period of 2 days to 28 days. The differential scanning calorimetry and thermogravimetry measurements are performed in the temperature range of 25°C to 1000°C in an argon atmosphere. The measurement of compressive strength is done according to the European standards for cement mortars. The thermal analysis results in the identification of temperature and quantification of enthalpy and mass changes related to the liberation of physically bound water, calcium-silicate-hydrates dehydration and portlandite, vaterite and calcite decomposition. The portlandite content is found to decrease with time for all blends which provides the evidence of the pozzolanic activity of ceramic powder even within the limited monitoring time of 28 days. Taking into account the favorable results obtained in the measurement of compressive strength, it can be concluded that the applied waste ceramic powder can be successfully used as a supplementary cementing material to Portland cement in an amount of up to 24 mass%.

  5. Method for molding ceramic powders using a water-based gel casting process

    DOEpatents

    Jenny, Mark A.; Omalete, Ogbemi O.

    1992-09-08

    A method for molding ceramic powders comprises forming a slurry mixture including ceramic powder, a dispersant, and a monomer solution. The monomer solution includes at least one monofunctional monomer and at least one difunctional monomer, a free-radical initiator, and a aqueous solvent. The slurry mixture is transferred to a mold, and the mold containing the slurry mixture is heated to polymerize and crosslink the monomer and form a firm polymer-solvent gel matrix. The solid product may be removed from the mold and heated to first remove the solvent and subsequently remove the polymer, whereafter the product may be sintered.

  6. Method for molding ceramic powders using a water-based gel casting

    DOEpatents

    Janney, Mark A.; Omatete, Ogbemi O.

    1991-07-02

    A method for molding ceramic powders comprises forming a slurry mixture including ceramic powder, a dispersant, and a monomer solution. The monomer solution includes at least one monofunctional monomer and at least one difunctional monomer, a free-radical initiator, and a aqueous solvent. The slurry mixture is transferred to a mold, and the mold containing the slurry mixture is heated to polymerize and crosslink the monomer and form a firm polymer-solvent gel matrix. The solid product any be removed from the mold and heated to first remove the solvent and subsequently remove the polymer, whereafter the product may be sintered.

  7. Analysis of trace halocarbon contaminants in ultra high purity helium

    NASA Technical Reports Server (NTRS)

    Fewell, Larry L.

    1994-01-01

    This study describes the analysis of ultra high purity helium. Purification studies were conducted and containment removal was effected by the utilization of solid adsorbent purge-trap systems at cryogenic temperatures. Volatile organic compounds in ultra high purity helium were adsorbed on a solid adsorbent-cryogenic trap, and thermally desorbed trace halocarbon and other contaminants were analyzed by combined gas chromatography-mass spectrometry.

  8. Delta Doping High Purity CCDs and CMOS for LSST

    NASA Technical Reports Server (NTRS)

    Blacksberg, Jordana; Nikzad, Shouleh; Hoenk, Michael; Elliott, S. Tom; Bebek, Chris; Holland, Steve; Kolbe, Bill

    2006-01-01

    A viewgraph presentation describing delta doping high purity CCD's and CMOS for LSST is shown. The topics include: 1) Overview of JPL s versatile back-surface process for CCDs and CMOS; 2) Application to SNAP and ORION missions; 3) Delta doping as a back-surface electrode for fully depleted LBNL CCDs; 4) Delta doping high purity CCDs for SNAP and ORION; 5) JPL CMP thinning process development; and 6) Antireflection coating process development.

  9. Method for producing a compressed body of mix-powder for ceramic

    NASA Technical Reports Server (NTRS)

    Okawa, K.

    1983-01-01

    Under the invented method, a compressed body of mix powder for ceramic is produced by mixing and stirring several raw powder materials with mixing liquid such as water, and, in the process of sending the resulted viscous material pressurized at 5 kg/cm to 7 kg/cm, using 1.5 to 2 times the pressure to filter and dehydrate, adjusting the water content to 10 to 20%.

  10. Continuum-based FEM modeling of ceramic powder compaction using a cap-plasticity constitutive model

    SciTech Connect

    ARGUELLO JR.,JOSE G.; FOSSUM,ARLO F.; ZEUCH,DAVID H.; EWSUK,KEVIN G.

    2000-01-25

    Common ceramic component manufacturing typically involves the processing of the raw materials in powder form. Granulated powder is formed into a green body of the desired size and shape by consolidation, often by simply pressing nominally dry powder. Ceramic powders are commonly pressed in steel dies or rubber bags with the aim of producing a near-net-shape green body for subsequent sintering. Density gradients in these compacts, introduced during the pressing operation, are often severe enough to cause distortions in the shape of the part during sintering due to nonuniform shrinkage. In such cases, green machining or diamond grinding operations may be needed to obtain the desired final shape and size part. In severe cases, nonuniform shrinkage may even cause fracture in the parts during sintering. Likewise, density gradients can result in green bodies that break during ejection from the die or that are too fragile to be handled during subsequent processing. Empirical relationships currently exist to describe powder compaction but provide little understanding of how to control die design or compaction parameters to minimize density gradients thereby forcing the designer to use expensive and time consuming trial and error procedures. For this reason, interest has grown in developing computational tools to address this problem (Aydin et al., 1996 and Coube, 1998). The goal of the present work was to develop a general continuum-based finite element model for ceramic powder compaction that can be used to aid and guide the design and pressing of ceramic powders. Such a model can be used to improve both part and die/bag pressing design, resulting in more efficient and cost effective ways to make better parts.

  11. Fully-Enclosed Ceramic Micro-burners Using Fugitive Phase and Powder-based Processing.

    PubMed

    Do, Truong; Shin, Changseop; Kwon, Patrick; Yeom, Junghoon

    2016-01-01

    Ceramic-based microchemical systems (μCSs) are more suitable for operation under harsh environments such as high temperature and corrosive reactants compared to the more conventional μCS materials such as silicon and polymers. With the recent renewed interests in chemical manufacturing and process intensification, simple, inexpensive, and reliable ceramic manufacturing technologies are needed. The main objective of this paper is to introduce a new powder-based fabrication framework, which is a one-pot, cost-effective, and versatile process for ceramic μCS components. The proposed approach employs the compaction of metal-oxide sub-micron powders with a graphite fugitive phase that is burned out to create internal cavities and microchannels before full sintering. Pure alumina powder has been used without any binder phase, enabling more precise dimensional control and less structure shrinkage upon sintering. The key process steps such as powder compaction, graphite burnout during partial sintering, machining in a conventional machine tool, and final densification have been studied to characterize the process. This near-full density ceramic structure with the combustion chamber and various internal channels was fabricated to be used as a micro-burner for gas sensing applications. PMID:27546059

  12. Fully-Enclosed Ceramic Micro-burners Using Fugitive Phase and Powder-based Processing

    PubMed Central

    Do, Truong; Shin, Changseop; Kwon, Patrick; Yeom, Junghoon

    2016-01-01

    Ceramic-based microchemical systems (μCSs) are more suitable for operation under harsh environments such as high temperature and corrosive reactants compared to the more conventional μCS materials such as silicon and polymers. With the recent renewed interests in chemical manufacturing and process intensification, simple, inexpensive, and reliable ceramic manufacturing technologies are needed. The main objective of this paper is to introduce a new powder-based fabrication framework, which is a one-pot, cost-effective, and versatile process for ceramic μCS components. The proposed approach employs the compaction of metal-oxide sub-micron powders with a graphite fugitive phase that is burned out to create internal cavities and microchannels before full sintering. Pure alumina powder has been used without any binder phase, enabling more precise dimensional control and less structure shrinkage upon sintering. The key process steps such as powder compaction, graphite burnout during partial sintering, machining in a conventional machine tool, and final densification have been studied to characterize the process. This near-full density ceramic structure with the combustion chamber and various internal channels was fabricated to be used as a micro-burner for gas sensing applications. PMID:27546059

  13. Silicon nitride ceramic matrix for CMCs from silane derived Si powders and preceramic polymers

    SciTech Connect

    Rhine, W.E.; Lightfoot, A.; Seyferth, D.; Haggerty, J.S.

    1995-10-01

    Si powders synthesized by the laser pyrolysis of silane can be nitrided at 1,200--1,250 C, producing an improved reaction bonded silicon nitride. This RBSN is a potential matrix for composites since it can be formed at temperatures which do not degrade the strengths of commercially available amorphous ceramic fibers. However, the density of the RBSN matrix has been limited to about 75% using the silane-derived Si powder. Combining Si powders and preceramic polymers offers an approach for increasing the density and mechanical properties of the reaction-formed Si{sub 3}N{sub 4} matrix. The incorporation of polysilazanes inhibited the nitridation oat 1,250 C, but samples could be effectively nitrided at 1,400 C. These higher nitriding temperatures are compatible with SCS-6 and other low-oxygen, crystalline SiC fibers which can be used as reinforcements for ceramic composites.

  14. Characterisation of two AGATA asymmetric high purity germanium capsules

    NASA Astrophysics Data System (ADS)

    Colosimo, S. J.; Moon, S.; Boston, A. J.; Boston, H. C.; Cresswell, J. R.; Harkness-Brennan, L.; Judson, D. S.; Lazarus, I. H.; Nolan, P. J.; Simpson, J.; Unsworth, C.

    2015-02-01

    The AGATA spectrometer is an array of highly segmented high purity germanium detectors. The spectrometer uses pulse shape analysis in order to track Compton scattered γ-rays to increase the efficiency of nuclear spectroscopy studies. The characterisation of two high purity germanium detector capsules for AGATA of the same A-type has been performed at the University of Liverpool. This work will examine the uniformity of performance of the two capsules, including a comparison of the resolution and efficiency as well as a study of charge collection. The performance of the capsules shows good agreement, which is essential for the efficient operation of the γ-ray tracking array.

  15. Overview of transparent optical ceramics for high-energy lasers at NRL.

    PubMed

    Kim, Woohong; Villalobos, Guillermo; Baker, Colin; Frantz, Jesse; Shaw, Brandon; Bayya, Shyam; Bowman, Steven; Sadowski, Bryan; Hunt, Michael; Rock, Benjamin; Aggarwal, Ishwar; Sanghera, Jasbinder

    2015-11-01

    In this review, we present our recent research progress at the Naval Research Laboratory in the development of highly transparent and rugged ceramic window materials such as MgAl2O4 spinel and β-SiC; high-power solid-state laser gain materials based on sesquioxide such as Yb(3+):Y2O3, Yb(3+):Lu2O3, and Ho(3+):Lu2O3; and composite ceramics in the application for high-energy lasers. Various powder synthesis/purification methods and powder post-process techniques necessary to create high-purity powders are described. Ceramic fabrication processes and chemical, morphological, and optical properties of the ceramics developed at the Naval Research Laboratory (NRL) are highlighted. We also report high-efficiency lasing from a hot-pressed rare-earth sesquioxide single layer and composite ceramics made from coprecipitated powder. PMID:26560610

  16. Synthesis of ceramic powders and surface films from laser heated gases

    NASA Technical Reports Server (NTRS)

    Haggerty, J. S.

    1985-01-01

    Two new processes have been developed that are based on laser-heated gases. Both permit unusually precise levels of process control and, thereby, materials having superior properties. The power process yields Si, Si3N4 and SiC powders that are uniform in size, nonagglomerated, small diameter, spherically shaped and high purity. Manufacturing cost analyses show that submicron powders can be made with an energy cost of approximately 2 kWhr/kg and a dollar cost of 2-3.30 $/kg, exclusive of the costs of feed materials. The laser-induced chemical vapor deposition process (LICVD) causes reactant gases to be heated by absorbing IR light from a laser beam that passes parallel to the substrate surface. Laser heating permits independent control of gas and substrate temperatures while operating in a conventional, thermally activated chemical vapor deposition mode. Spin density, hydrogen content, electrical conductivity and mobility gap properties show the LICVD process capable of producing very high quality films.

  17. Ceramic automotive Stirling engine study

    NASA Technical Reports Server (NTRS)

    Musikant, S.; Chiu, W.; Darooka, D.; Mullings, D. M.; Johnson, C. A.

    1985-01-01

    A conceptual design study for a Ceramic Automotive Stirling Engine (CASE) is performed. Year 1990 structural ceramic technology is assumed. Structural and performance analyses of the conceptual design are performed as well as a manufacturing and cost analysis. The general conclusions from this study are that such an engine would be 10-26% more efficient over its performance map than the current metal Automotive Stirling Reference Engine (ASRE). Cost of such a ceramic engine is likely to be somewhat higher than that of the ASRE but engine cost is very sensitive to the ultimate cost of the high purity, ceramic powder raw materials required to fabricate high performance parts. When the design study is projected to the year 2000 technology, substantinal net efficiency improvements, on the order of 25 to 46% over the ASRE, are computed.

  18. Low cost routes to high purity silicon and derivatives thereof

    SciTech Connect

    Laine, Richard M; Krug, David James; Marchal, Julien Claudius; Mccolm, Andrew Stewart

    2013-07-02

    The present invention is directed to a method for providing an agricultural waste product having amorphous silica, carbon, and impurities; extracting from the agricultural waste product an amount of the impurities; changing the ratio of carbon to silica; and reducing the silica to a high purity silicon (e.g., to photovoltaic silicon).

  19. Electrochemical study of aluminum corrosion in boiling high purity water

    NASA Technical Reports Server (NTRS)

    Draley, J. E.; Legault, R. A.

    1969-01-01

    Electrochemical study of aluminum corrosion in boiling high-purity water includes an equation relating current and electrochemical potential derived on the basis of a physical model of the corrosion process. The work involved an examination of the cathodic polarization behavior of 1100 aluminum during aqueous oxidation.

  20. Preparation of high purity copper fluoride by fluorinating copper hydroxyfluoride

    NASA Technical Reports Server (NTRS)

    King, R. B.; Lundquist, J. R.

    1969-01-01

    Copper fluoride containing no more than 50 ppm of any contaminating element was prepared by the fluorination of copper hydroxyfluoride. The impurity content was obtained by spark source mass spectrometry. High purity copper fluoride is needed as a cathode material for high energy density batteries.

  1. Optimization of calcium phosphate fine ceramic powders preparation

    NASA Astrophysics Data System (ADS)

    Sezanova, K.; Tepavitcharova, S.; Rabadjieva, D.; Gergulova, R.; Ilieva, R.

    2013-12-01

    The effect of biomimetic synthesis method, reaction medium and further precursor treatments on the chemical and phase composition, crystal size and morphology of calcium phosphates was examined. Nanosized calcium phosphate precursors were biomimetically precipitated by the method of continuous precipitation in three types of reaction media at pH 8: (i) SBF as an inorganic electrolyte system; (ii) organic (glycerine) modified SBF (volume ratio of 1:1); (iii) polymer (10 g/l xanthan gum or 10 g/l guar gum) modified SBF (volume ratio of 1:1). After maturation (24 h) the samples were lyophilized, calcinated at 300°C for 3 hours, and washed with water, followed by new gelation, lyophilization and step-wise (200, 400, 600, 800, and 1000°C, each for 3 hours) sintering. The reaction medium influenced the chemical composition and particle size but not the morphology of the calcium phosphate powders. In all studied cases bi-phase calcium phosphate fine powders with well-shaped spherical grains, consisting of β-tricalcium phosphate (β-TCP) and hydroxyapatite (HA) with a Ca/P ratio of 1.3 - 1.6 were obtained. The SBF modifiers decreased the particle size of the product in the sequence guar gum ˜ xanthan gum < glycerin < SBF medium.

  2. Evaluation of the behavior of ceramic powders under mechanical vibration and its effect on the mechanics of auto-granulation

    NASA Astrophysics Data System (ADS)

    Ku, Nicholas

    In ceramic powder processing, the correlations between the constituent particles and the product structure-property outcomes are well established. However, the influence of static powder properties on the dynamic bulk powder behavior in such advance powder processes remains elusive. A multi-scale evaluation is necessary to understand the full effects of the particle ensemble on the bulk powder behavior, ranging from the particle micro-scale to the bulk powder macro-scale. Fine powders, with particle size of 10 ?m or less, often exhibit cohesive behavior. Cohesion in powders can cause poor flowability, affect agglomerate formation, as well as induce powder caking, all of which can be detrimental to the processing of the powders and/or final product structure-property outcomes. For this reason, it is critical to correlate the causal properties of the powders to this detrimental behavior. In this study, the bulk behavior of ceramic powders is observed under a simple powder process: harmonic, mechanical vibration. Four powder samples, two titania and two alumina powders, were studied. The main difference between the two powder variants of each material is particle size. The two alumina (Al2O3) powder samples had a primary particle size at 50% less than, or d50 of, 0.5 and 2.3 microm and the titania (TiO2) powder samples had a d 50 particle size of 0.1 and 1 microm. Due to mechanical vibration, the titania powder variant with a primary particle size of 0.1 microm exhibited a clustering behavior known as auto-granulation. Auto-granulation is the growth of particle clusters within a dry, fine powder bed without the addition of any binder or liquid to the system. The amplitude and frequency of the mechanical vibration was varied to view the effect on the equilibrium granule size and density. Furthermore, imaging of cross-sections of the granules was conducted to provide insight into to the internal microstructure and measure the packing fraction of the constituent

  3. A comparison of different powder compaction processes adopted for synthesis of lead-free piezoelectric ceramics

    NASA Astrophysics Data System (ADS)

    Mahesh, M. L. V.; Bhanu Prasad, V. V.; James, A. R.

    2016-04-01

    Barium zirconium titanate, Ba(Zr0.15Ti0.85)O3 nano-crystalline powders were synthesized using high energy ball milling. The calcined powders were compacted adopting two different approaches viz. the conventional uniaxial pressing and cold-isostatic pressing (CIP) and the compacts were sintered at 1350 °C. A single phase perovskite structure was observed in both cases. BZT ceramics compacted using CIP technique exhibited enhanced dielectric and ferroelectric properties compared to ceramics compacted by uniaxial pressing. The polarization current peaks have been used in this paper as an experimental evidence to prove the existence of ferroelectricity in the BZT ceramics under study. The peak polarization current was found to be ~700% higher in case of cold iso-statically compacted ceramics. Similarly electric field induces strain showed a maximum strain ( S max) of 0.08% at an electric field of 28 kV/cm. The dielectric and ferroelectric properties observed are comparable to single crystals of the same material.

  4. Sintering of ceramics using low frequency RF powder

    SciTech Connect

    Caughman, J.B.O.; Hoffman, D.J.; Baity, F.W.; Akerman, M.A.

    1995-12-31

    Sintering with low frequency rf power ({approximately}50 MHz) is a new technique with unique capabilities that has been used to sinter a variety of ceramic materials, including zirconia-toughened alumina, alumina, silicon carbide, and boron carbide. Processing with low frequencies offers many advantages compared to processing with conventional microwave frequencies (915 MHz and 2.45 GHz). Because of the longer wavelength, the rf electric field penetrates materials more than microwaves. This effect allows the processing of a wider variety of materials and allows for an increase in the physical size of the material being processed. In addition, the material is heated in a single mode cavity with a uniform electric field, which reduces the occurrence of hot-spot generation and thermal runaway effects. This technique has been used to sinter large crack-free alumina samples (3 inches square) to >97% density. The sintering and/or annealing of a number of carbide materials has been demonstrated as well, including silicon carbide, boron carbide, tungsten carbide, and titanium carbide.

  5. CDTE CERAMICS BASED ON COMPRESSION OF NANOCRYSTAL POWDER.

    SciTech Connect

    KOLESNIKOV, N.N.; BORISENKO, E.B.; BORISENKO, D.N.; JAMES, R.B.; KVEDER, V.V.; GARTMAN, V.K.; GNESIN, G.A.

    2005-07-01

    Wide-gap II-VI semiconductor crystalline materials are conventionally used in laser optics, light emitting devices, and nuclear detectors. The advances made in the studies of nanocrystals and in the associated technologies have created great interest in the design of semiconductor devices based on these new materials. The objectives of this work are to study the microstructure and the properties of the new material produced through CdTe nanopowder compression and to consider the prospects of its use in the design of ionizing-radiation detectors and in laser optics. Highly dense material produced of 7-10 nm CdTe particles under pressure of 20-600 MPa at temperatures from 20 to 200 C was analyzed using x-ray diffractometry, texture analysis; light and scanning electron microscopy, and optical spectrophotometry. The mechanical and electrical properties of the compacted material were measured and compared with similar characteristics of the conventionally grown single crystals. Phase transformation from metastable to stable crystal structure caused by deformation was observed in the material. Sharp crystallographic texture {l_brace}001{r_brace} that apparently affects specific mechanical, electrical and optical characteristics of compacted CdTe was observed. The specific resistivity calculated from the linear current-voltage characteristics was about 10{sup 10} Ohm x cm, which is a promisingly high value regarding the possibility of using this material in the design of semiconductor radiation detectors. The optical spectra show that the transmittance in the infrared region is sufficient to consider the prospects of possible applications of CdTe ceramics in laser optics.

  6. Sintering stress and microstructure in ceramic powder compacts

    SciTech Connect

    Chu, May-Ying California Univ., Berkeley, CA . Dept. of Materials Science and Mineral Engineering)

    1990-08-01

    The behavior of the sintering stress and microstructure during sintering is studied under various thermal and physical conditions. Specifically, the study includes sintering under isothermal or constant heating rate conditions; and altering the starting compact structure by pre-coarsening to increase the particle size, or by compaction to increase the starting density. Loading dilatometry is used to measure the ratio of the densification strain rate to the creep strain rate and the continuous shrinkage history of the systems. The data show that the ratio of the densification to the creep strain rate is remarkably constant within a wide temperature range for densification, from the earliest stages of densification to at least the onset of the final stage. As a consequence, the sintering stress, which is proportional to the strain rate ratio, is nearly independent of sintered density or of temperature. Analysis leads to a simple method for determining the simultaneous densification strain rate over the creep strain rate ratio. A rigorous densification strain rate equation is derived for a model system. The constant sintering stress allows progress on formulating a sintering equation to predict the densification behavior of powder compacts. Analysis of dilatometry data from compacts sintered at various heating rates, and of numerical computations, indicate the need to include separate coarsening processes with different activation energies. The same model is used to describe the differences in pore spacing evolution between pre-coarsened and as-received systems.

  7. Preparation and properties of high purity Mg-Y biomaterials.

    PubMed

    Peng, Qiuming; Huang, Yuanding; Zhou, Le; Hort, Norbert; Kainer, Karl Ulrich

    2010-01-01

    An effective zone solidification method has been found to prepare high purity Mg-Y biomaterials. The corrosion and mechanical properties of the purified middle region are improved remarkably compared with common casting method. The average gain size and secondary dendrite space decrease from the top layer to the bottom layer of the ingot. The oxides, defects and precipitates are mainly enriched in the top layer of the ingot under the impulsion of high thermal gradient. These results are in agreement with that simulated by finite elemental method using FLOW-3D software. It is confirmed that the mode of scallop symmetric solidification attributes to the purifying process. This zone solidification method not only contributes to high purity Mg-based biomaterials, but also provides a new approach to prepare high performance Mg alloys. PMID:19800117

  8. High-Purity Silicon Seeds for Silane Pyrolysis

    NASA Technical Reports Server (NTRS)

    Hsu, G. C.; Rohatgi, N. K.; Morrison, A.

    1985-01-01

    Seed particles for fluidized-bed production of silicon made by new contamination-free, economical method. In new method, large particles of semiconductor-grade silicon fired at each other by high-speed streams of gas and thereby break up into particles of suitable size for fluidized bed. No foreign materials introduced, and leaching unnecessary. Method used to feed fluidized-bed reactor for continuous production of high-purity silicon.

  9. Ceramics

    NASA Astrophysics Data System (ADS)

    Chen, Song; Zhu, De-Gui; Cai, Xu-Sheng

    2014-08-01

    The dense monoclinic-SrAl2Si2O8 ceramics have been prepared by a two-step sintering process at a sintering temperature of 1173 K (900 °C). Firstly, the pre-sintered monoclinic-SrAl2Si2O8 powders containing small SiO2·Al2O3 crystal phases were obtained by continuously sintering a powder mixture of SrCO3 and kaolin at 1223 K (950 °C) for 6 hours and 1673 K (1400 °C) for 4 hours, respectively. Subsequently, by the combination of the pre-sintered ceramic powders with the composite flux agents, which are composed of a SrO·3B2O3 flux agent and α-Al2O3, the low-temperature densification sintering of the monoclinic-SrAl2Si2O8 ceramics was accomplished at 1173 K (900 °C). The low-temperature sintering behavior and microstructure evolvement of the monoclinic-SrAl2Si2O8 ceramics have been investigated in terms of Al2O3 in addition to the composite flux agents. It shows that due to the low-meting characteristics, the SrO·3B2O3 flux agent can urge the dense microstructure formation of the monoclinic-SrAl2Si2O8 ceramics and the re-crystallization of the grains via a liquid-phase sintering. The introduction of α-Al2O3 to the SrO·3B2O3 flux agent can apparently lead to more dense microstructures for the monoclinic-SrAl2Si2O8 ceramics but also cause the re-precipitation of SiO2·Al2O3 compounds because of an excessive Al2O3 content in the SrO·3B2O3 flux agent.

  10. The use of functionalized monoalkyl phosphates and phosphonates in the colloidal processing of oxide ceramic powders

    NASA Astrophysics Data System (ADS)

    Radsick, Timothy Carl

    The purpose of this study was to develop phosphorous-based chemicals that could be used to modify the interparticle pair potential of several oxide ceramic particles, thereby enabling their use in colloidal processing schemes. Several procedures for the synthesis of 11-12 carbon alpha,o-functionalized monoalkyl phosphates and phosphonates were developed. Because of its simplicity and its use of mild reagents, a procedure based on the Michaelis-Arbuzov rearrangement was selected to produce the bulk of the chemicals used in this study. Carboxyl- and hydroxyl-terminated monoalkyl phosphonates were adsorbed onto alumina and zirconia powders using either aqueous-based or solvent-based methods to produce a monolayer of "brushlike" steric molecules. In the aqueous-based methods, powders were processed at pH values below their isoelectric point in order to produce a positive charge on the powder, thereby attracting the negatively charged phosphate or phosphonate group onto the powder surface to form the steric monolayer. In solvent-based methods, powder was suspended in an acetone solution of the phosphonates, heated at reflux, washed, dried and heat treated at 120°C under vacuum. The zeta potential of the coated powders was measured to quantify the degree of steric layer adsorption and the shift in the isoelectric point. Slurries of coated alumina and zirconia were prepared having 20 vol % powder. Rheological behavior was studied by measuring viscosity as a function of shear rate for slurries of various pH values and counterion concentrations. Slurries with powder processed via the solvent method were the least sensitive to changes in slurry pH and were straightforward to prepare. It is thought that the solvent-based coating procedure produced a stronger, multi-dentate powder-phosphonate bond than that of the aqueous-based procedure. Dispersed and coagulated slurries were able to be prepared over a wide pH range, including at the isoelectric point of the uncoated powders

  11. Tridymite Type Phosphates of Cesium and Divalent Metals: Synthesis and Characterization of Powder and Ceramic Samples

    NASA Astrophysics Data System (ADS)

    Pet'kov, V. I.; Korchemkin, I. V.; Asabina, E. A.; Chuvil'deev, V. N.; Boldin, M. S.

    The phase formation regularities of trydimite-type solid solutions CsMg1-xMexPO4 (Me = Mn, Co, Zn, Cu) were studied, and the dependences of the unit cell parameters on their compositions x were revealed. The thermal expansion of some double phosphates CsMePO4 (Me = Mg, Co, Mn, Zn) was investigated by high-temperature X-ray powder diffraction. The samples expand anisotropically and belong to high-thermal expansion materials. Single- phase stuffed CsMgPO4-based ceramic (density about 95-97% of theoretical value) was obtained. A leaching rate of approximately 3rad 10-4 grad cm-2rad d-1 for Cs was determined with statical leaching of prepared ceramic.

  12. Effect of Sintering Temperature on the Synthesis of High Purity Cordierite

    SciTech Connect

    Choo, Y. P.; Chow, T. Y.; Mohamad, H.

    2008-03-17

    Cordierite is silicate material widely used in ceramic industry. The effect of sintering temperature to the properties of cordierite by sol gel method was studied with utilizing magnesium nitrate, aluminum nitrate, ethanol, and tetraethyl orthosilicate (TEOS) as starting materials. Gels are dried and sintered at different temperature (1000 deg. C, 1200 deg. C, 1300 deg. C and 1350 deg. C) then characterized by varies analysis techniques. XRD analysis shows that spinel, {mu}-cordierite and cristobalite are formed at 1000 deg. C which spinel as predominant phase. At 1200 deg. C, {mu}-cordierite occured as predominant phase, spinel, sapphirine and cristobalite are formed as minor phases. It also confirmed that high purity {alpha}-cordierite formed at 1300 deg. C and clearly observed at 1350 deg. C. Result of EDX analysis proved that magnesium, aluminum, silicon and oxygen was existed in the cordierite.

  13. Numerical Simulation of Sintering Process in Ceramic Powder Injection Moulded Components

    SciTech Connect

    Song, J.; Barriere, T.; Gelin, J. C.

    2007-05-17

    A phenomenological model based on viscoplastic constitutive law is presented to describe the sintering process of ceramic components obtained by powder injection moulding. The parameters entering in the model are identified through sintering experiments in dilatometer with the proposed optimization method. The finite element simulations are carried out to predict the density variations and dimensional changes of the components during sintering. A simulation example on the sintering process of hip implant in alumina has been conducted. The simulation results have been compared with the experimental ones. A good agreement is obtained.

  14. Method and apparatus for producing high purity silicon

    DOEpatents

    Olson, Jerry M.

    1984-01-01

    A method for producing high purity silicon includes forming a copper silie alloy and positioning the alloy within an enclosure. A filament member is also placed within the enclosure opposite the alloy. The enclosure is then filled with a chemical vapor transport gas adapted for transporting silicon. Finally, both the filament member and the alloy are heated to temperatures sufficient to cause the gas to react with silicon at the alloy surface and deposit the reacted silicon on the filament member. In addition, an apparatus for carrying out this method is also disclosed.

  15. The GALATEA test-facility for high purity germanium detectors

    NASA Astrophysics Data System (ADS)

    Abt, I.; Caldwell, A.; Dönmez, B.; Garbini, L.; Irlbeck, S.; Majorovits, B.; Palermo, M.; Schulz, O.; Seitz, H.; Stelzer, F.

    2015-05-01

    GALATEA is a test facility designed to investigate bulk and surface effects in high purity germanium detectors. A vacuum tank houses a cold volume with the detector inside. A system of three precision motorized stages allows an almost complete scan of the detector. The main feature of GALATEA is that there is no material between source and detector. This allows the usage of alpha and beta sources to study surface effects. A 19-fold segmented true-coaxial germanium detector was used for commissioning. A first analysis of data obtained with an alpha source is presented here.

  16. A novel method to synthesize high purity, nanostructured copper

    SciTech Connect

    Hodge, A M; Wang, Y M; Barbee, T W

    2005-08-30

    Nanostructured high purity (99.999%) copper foils, 10 cm in diameter and 22-25 microns thick were produced using nanoscale multilayer technology. The foils were produced using five different layer thicknesses ranging from 1.25 to 43.6 nm (18,000 to 520 layers). This process delivers the ability to produce multiple large-scale samples during a single deposition run with very small residual stresses. Tensile and indentation tests demonstrate that the material produced is a high strength copper ({sigma}{sub y} {approx} 540-690 MPa).

  17. Neutron energy determination with a high-purity germanium detector

    NASA Technical Reports Server (NTRS)

    Beck, Gene A.

    1992-01-01

    Two areas that are related to planetary gamma-ray spectrometry are investigated. The first task was the investigation of gamma rays produced by high-energy charged particles and their secondaries in planetary surfaces by means of thick target bombardments. The second task was the investigation of the effects of high-energy neutrons on gamma-ray spectral features obtained with high-purity Ge-detectors. For both tasks, as a function of the funding level, the experimental work was predominantly tied to that of other researchers, whenever there was an opportunity to participate in bombardment experiments at large or small accelerators for charged particles.

  18. Preparation of high purity doped oxides for fundamental studies

    NASA Astrophysics Data System (ADS)

    Morrissey, Amy L.

    Yttria-stabilized zirconia (YSZ) is an important ceramic and is critical in electrochemical applications. Small amounts of transition metal dopants are shown to influence mechanical and electronic properties of YSZ. In this work, a novel method was used to synthesize 0.01, 0.1, 0.5, and 1.0 mol % NiO, Co3O4, and Fe2O3-doped YSZ from all acetate precursors. The synthesized materials were calcined at temperatures between 600°C and 1000°C to produce powders that were then pressed into compacts and sintered at 1500°C The powders and compacts were evaluated with x-ray diffraction, electron microscopy, and SQUID magnetometry. The particle size was observed to increase with increasing calcination temperature and a correlation between the particle size and formation of NiO was noted. In particular, NiO is absent as a second phase in the finer particle size material (lower calcination temperatures) but present in coarser material (calcination temperature at 1000°C), even when the concentration is well below the known solid solubility limit of NiO in YSZ. The results suggest Ni 2+ ions dissolve readily in nanoscale YSZ, but form NiO once the grains are larger than about 150 nm. When all materials are sintered at 1500°C, NiO dissolves fully into YSZ. Thus, the dissolution of NiO in YSZ occurs in two stages: at temperatures up to 1000°C, Ni2+ ions dissolve only in the grain boundaries of YSZ; at 1500°C, Ni2+ ions dissolve in the bulk YSZ. The results of initial experiments for Co3 O4-10YSZ and Fe2O3-10YSZ systems are reported and show an increased complexity compared with NiO-YSZ, likely because the dopant solubilities are not well-known and the effect of multivalent dopant ions existing simultaneously in YSZ is not well-characterized. This work shows that magnetometry is extremely useful for characterizing the dopant concentration in all stages of processing.

  19. Characterization of high purity Silicon derived from Rice husk through improved Leaching process

    NASA Astrophysics Data System (ADS)

    Yusuf, Gbadebo; Awodugba, Ayodeji; Raimi, Adepoju; Babatola, Babatunde

    2014-03-01

    Rice husk is an abundant source of silicon and silicon compounds. High purity Silicon are required in high technology products such as semiconductors and solar cell. In this work, the possibility of obtaining pure silicon compounds through leaching process was investigated. Mesoporous silica nanoparticles with amorphous morphology have been synthesized from rice husk which was further subjected to improved leaching process to obtain pure silicon. XRD analysis shows the crystal structure of the as-received RHA with major reflections or peaks of crystalline quartz from ICSD powder diffraction occur at Bragg 2 θ angles of 20.856°, 26.636° and 36.541°. The purity of silicon obtained in terms of silica content was improved by leaching in 10 wt% hydrochloric acid. Advance future works on characterizing the electrical properties of the refined Rice Husk will eventually add value to the Rice Husk Silicon product and make it more attractive not only to the Photovoltaic industry but also other industries that require high purity silicon at reasonable cost. We wish to thank the Managements of Osun state Polytechnic-Iree and Ladoke Akintola University of Technology-Ogbomoso for creating enabling environment for this research work.

  20. The compressibility of high purity YbB2.

    PubMed

    Kalkan, B; Suzer, S; Ozdas, E

    2012-08-29

    The compressibility and phase stability of Y bB(2) are investigated under high pressure using high-resolution synchrotron x-ray diffraction in a diamond anvil cell. The bulk modules of high purity Y bB(2) is obtained as ∼182 GPa using the Birch-Murnaghan equation of state. The patterns measured up to 20 GPa and the pressure dependence of normalized lattice parameters, a/a(0) and c/c(0), reveal that the compressibility of Y bB(2) is low and fairly isotropic, and this material can be classified as a hard material. X-ray photoemission studies demonstrate that Yb in Y bB(2) has a mostly trivalent valence state at room temperature. Moreover, sample preparation details provide a new insight into the high purity synthesis of Y bB(2) at ambient pressure and moderate temperatures. The presented structural and compressibility results are in agreement with the available theoretical and experimental data on binary rare-earth borides and can serve as a reliable reference for future studies. PMID:22850355

  1. Hydration of blended cement pastes containing waste ceramic powder as a function of age

    NASA Astrophysics Data System (ADS)

    Scheinherrová, Lenka; Trník, Anton; Kulovaná, Tereza; Pavlík, Zbyšek; Rahhal, Viviana; Irassar, Edgardo F.; Černý, Robert

    2016-07-01

    The production of a cement binder generates a high amount of CO2 and has high energy consumption, resulting in a very adverse impact on the environment. Therefore, use of pozzolana active materials in the concrete production leads to a decrease of the consumption of cement binder and costs, especially when some type of industrial waste is used. In this paper, the hydration of blended cement pastes containing waste ceramic powder from the Czech Republic and Portland cement produced in Argentina is studied. A cement binder is partially replaced by 8 and 40 mass% of a ceramic powder. These materials are compared with an ordinary cement paste. All mixtures are prepared with a water/cement ratio of 0.5. Thermal characterization of the hydrated blended pastes is carried out in the time period from 2 to 360 days. Simultaneous DSC/TG analysis is performed in the temperature range from 25 °C to 1000 °C in an argon atmosphere. Using this thermal analysis, we identify the temperature, enthalpy and mass changes related to the liberation of physically bound water, calcium-silicate-hydrates gels dehydration, portlandite, vaterite and calcite decomposition and their changes during the curing time. Based on thermogravimetry results, we found out that the portlandite content slightly decreases with time for all blended cement pastes.

  2. Optical Coherence Tomography for Inspection of Highly Scattering Ceramic Media: Glass Powders and Plasma-Sprayed Coatings

    NASA Astrophysics Data System (ADS)

    Veilleux, J.; Moreau, C.; Lévesque, D.; Dufour, M.; Boulos, M. I.

    2006-03-01

    Optical coherence tomography (OCT) is used to collect images of spherical glass powders with mean diameter ranging from 10 to 150 microns. Appropriate peak distance measurements on image interferograms provide a good approximation of particle size distribution. The relationship between the light penetration depth inside powders and the particle diameter is also discussed based on Mie theory. Thereafter, OCT images of plasma-sprayed ceramic coatings are presented as well as an approach for establishing light penetration depth inside zirconia coatings.

  3. Optical Coherence Tomography for Inspection of Highly Scattering Ceramic Media: Glass Powders and Plasma-Sprayed Coatings

    SciTech Connect

    Veilleux, J.; Boulos, M. I.; Moreau, C.; Levesque, D.; Dufour, M.

    2006-03-06

    Optical coherence tomography (OCT) is used to collect images of spherical glass powders with mean diameter ranging from 10 to 150 microns. Appropriate peak distance measurements on image interferograms provide a good approximation of particle size distribution. The relationship between the light penetration depth inside powders and the particle diameter is also discussed based on Mie theory. Thereafter, OCT images of plasma-sprayed ceramic coatings are presented as well as an approach for establishing light penetration depth inside zirconia coatings.

  4. Precipitation of hydrides in high purity niobium after different treatments

    SciTech Connect

    Barkov, F.; Romanenko, A.; Trenikhina, Y.; Grassellino, A.

    2013-01-01

    Precipitation of lossy non-superconducting niobium hydrides represents a known problem for high purity niobium in superconducting applications. Using cryogenic optical and laser confocal scanning microscopy we have directly observed surface precipitation and evolution of niobium hydrides in samples after different treatments used for superconducting RF cavities for particle acceleration. Precipitation is shown to occur throughout the sample volume, and the growth of hydrides is well described by the fast diffusion-controlled process in which almost all hydrogen is precipitated at $T=140$~K within $\\sim30$~min. 120$^{\\circ}$C baking and mechanical deformation are found to affect hydride precipitation through their influence on the number of nucleation and trapping centers.

  5. Characteristics of GRIFFIN high-purity germanium clover detectors

    NASA Astrophysics Data System (ADS)

    Rizwan, U.; Garnsworthy, A. B.; Andreoiu, C.; Ball, G. C.; Chester, A.; Domingo, T.; Dunlop, R.; Hackman, G.; Rand, E. T.; Smith, J. K.; Starosta, K.; Svensson, C. E.; Voss, P.; Williams, J.

    2016-06-01

    The Gamma-Ray Infrastructure For Fundamental Investigations of Nuclei, GRIFFIN, is a new experimental facility for radioactive decay studies at the TRIUMF-ISAC laboratory. The performance of the 16 high-purity germanium (HPGe) clover detectors that will make up the GRIFFIN spectrometer is reported. The energy resolution, efficiency, timing resolution, crosstalk and preamplifier properties of each crystal were measured using a combination of analog and digital data acquisition techniques. The absolute efficiency and add-back factors are determined for the energy range of 80-3450 keV. The detectors show excellent performance with an average over all 64 crystals of a FWHM energy resolution of 1.89(6) keV and relative efficiency with respect to a 3 in . × 3 in . NaI detector of 41(1)% at 1.3 MeV.

  6. Secondary emission conductivity of high purity silica fabric

    NASA Technical Reports Server (NTRS)

    Belanger, V. J.; Eagles, A. E.

    1977-01-01

    High purity silica fabrics were proposed for use as a material to control the effects of electrostatic charging of satellites at synchronous altitudes. These materials exhibited very quiet behavior when placed in simulated charging environments as opposed to other dielectrics used for passive thermal control which exhibit varying degrees of electrical arcing. Secondary emission conductivity is proposed as a mechanism for this superior behavior. Design of experiments to measure this phenomena and data taken on silica fabrics are discussed as they relate to electrostatic discharge (ESD) control on geosynchronous orbit spacecraft. Studies include the apparent change in resistivity of the material as a function of the electron beam energy, flux intensity, and the effect of varying electric fields impressed across the material under test.

  7. Springback in Deep Drawn High Purity Niobium for Superconductor Cavities

    SciTech Connect

    Ganapati Rao Myneni; Peter Kneisel

    2005-09-01

    Superconducting radio frequency (SRF) cavities made from deep drawn high-purity niobium have become a popular approach for the design of particle accelerators. A number of current accelerators use this technology and it is a leading candidate for future designs. The development of this technology has required significant advances in many scientific fields including metallurgy, high vacuum physics, surface science, and forming. Recently proposed modifications to the current process for fabrication of these cavities has resulted in increased concern about the distribution of deformation, residual stress patterns, and springback. This presentation will report on the findings of a recently initiated program to study plastic flow and springback in the fabrication of these cavities and the influence of metallurgical variables including grain size and impurity content.

  8. Study on the Properties of High Purity Germanium Crystals

    NASA Astrophysics Data System (ADS)

    Yang, G.; Mei, H.; Guan, Y. T.; Wang, G. J.; Mei, D. M.; Irmscher, K.

    2015-05-01

    In the crystal growth lab of South Dakota University, we are growing high purity germanium (HPGe) crystals and using the grown crystals to make radiation detectors. As the detector grade HPGe crystals, they have to meet two critical requirements: an impurity level of ∼109 to 10 atoms /cm3 and a dislocation density in the range of ∼102 to 104 / cm3. In the present work, we have used the following four characterization techniques to investigate the properties of the grown crystals. First of all, an x-ray diffraction method was used to determine crystal orientation. Secondly, the van der Pauw Hall effect measurement was used to measure the electrical properties. Thirdly, a photo-thermal ionization spectroscopy (PTIS) was used to identify what the impurity atoms are in the crystal. Lastly, an optical microscope observation was used to measure dislocation density in the crystal. All of these characterization techniques have provided great helps to our crystal activities.

  9. Dislocation distribution in large high-purity germanium crystal

    NASA Astrophysics Data System (ADS)

    Mei, Hao; Wang, Guojian; Mei, Dongming; Huang, Mianliang; Yang, Gang; Guan, Yutong; Cubed Collaboration

    2014-03-01

    We investigated the impacts of growth rate, time-temperature profile, thermal gradient on the dislocation distribution in large high-purity germanium crystal (12 cm in diameter) grown via Czochralski along <100>orientation. The time-temperature profiles of the crystal grown at different input power were investigated using direct measurements and computational modeling. The effect of crystallization speed on dislocation density is discussed from the context of thermal gradient during growth. Several samples from the grown crystals were used for this investigation. We measured dislocation density across the entire cross-section of the grown crystal through the microscope. By measuring and calculating the dislocation density, we were able to identify the denseness and the type of dislocation, which allows us to study how the thermal stress impacts the dislocation generation and distribution across the large grown crystals. This work is supported by DOE grant DE-FG02-10ER46709 and the state of South Dakota.

  10. Development of high purity niobium used in SRF accelerating cavity

    NASA Astrophysics Data System (ADS)

    Chen, Lin; Xie, Wei-Ping; Li, Ming-Yang; He, Ji-Lin; Fan, Hui-Ru; Zhang, Bao-Cheng; He, Fei-Si; Zhao, Kui; Chen, Jia-Er; Liu, Ke-Xin

    2008-12-01

    Niobium is widely used in SRF (Superconducting Radio Frequency) cavities due to its excellent superconductivity and workability. With the continuous development of technology, higher demands of material are raised. One of the key issues is that RRR (Residual Resistance Ratio) of the Nb material should be more than 300, which requires that the Nb ingot have even higher RRR. This article introduces the development and the experimental results of high purity niobium in OTIC in Ningxia (Ningxia Orient Tantalum Industry Co. Ltd.), and the test results of the single cell TESLA (Tera Electron volt energy Superconducting Linear Accelerator) shaped cavity manufactured by Peking University using Nb material from OTIC. Supported by National Basic Research Program of China (2002CB713600)

  11. Physical and mechanical metallurgy of high purity Nb accelerator cavities.

    SciTech Connect

    Wright, N. T.; Bieler, T. R.; Pourgoghart , F.; Compton, C.; Hartwig, K. T.; Baars, D.; Zamiri, A.; Chandrasekaran, S.; Darbandi, P.; Jiang, H.; Skoug, E.; Balachandran, S.; Ice, G. E.; Liu, W.; Michigan State Univ.; Texas A & M Univ.; ORNL

    2010-01-01

    In the past decade, high Q values have been achieved in high purity Nb superconducting radio frequency (SRF) cavities. Fundamental understanding of the physical metallurgy of Nb that enables these achievements is beginning to reveal what challenges remain to establish reproducible and cost-effective production of high performance SRF cavities. Recent studies of dislocation substructure development and effects of recrystallization arising from welding and heat treatments and their correlations with cavity performance are considered. With better fundamental understanding of the effects of dislocation substructure evolution and recrystallization on electron and phonon conduction, as well as the interior and surface states, it will be possible to design optimal processing paths for cost-effective performance using approaches such as hydroforming, which minimizes or eliminates welds in a cavity.

  12. Continuum-Based FEM Modeling of Ceramic Powder Compaction Using a Cap-Plasticity Constitutive Model

    SciTech Connect

    ARGUELLO JR.,JOSE G.; FOSSUM,ARLO F.; ZEUCH,DAVID H.; EWSUK,KEVIN G.

    2000-05-01

    Software has been developed and extended to allow finite element (FE) modeling of ceramic powder compaction using a cap-plasticity constitutive model. The underlying, general-purpose FE software can be used to model even the most complex three-dimensional (3D) geometries envisioned. Additionally, specialized software has been developed within this framework to address a general subclass of axisymmetric compacts that are common in industry. The expertise required to build the input deck, run the FE code, and post-process the results for this subclass of compacts is embedded within the specialized software. The user simply responds to a series of prompts, evaluates the quality of the FE mesh that is generated, and analyzes the graphical results that are produced. The specialized software allows users with little or no FE expertise to benefit from the tremendous power and insight that FE analysis can bring to the design cycle. The more general underlying software provides complete flexibility to model more complicated geometries and processes of interest to ceramic component manufacturers but requires significantly more user interaction and expertise.

  13. Preparation and mechanical properties of the MgAl2O4 transparent phosphor ceramics

    NASA Astrophysics Data System (ADS)

    Bai, Xue; Li, Zhen; Lei, Muyun; Pang, Zhenli

    2014-09-01

    MgAl2O4 transparent phosphor ceramics were fabricated by hot-pressing and hot isostatic pressing using high-purity ultrafine MgAl2O4 powder mixed with phosphor. The microstructures of transparent phosphor ceramics were characterized by SEM and EDS. Moreover, the hardness and bending strength of transparent ceramics were measured. Effect of phosphor concentration (0~20%) on microstructure, hardness and bending flexture of transparent ceramics was analyzed. It was found that phosphor doping plays an important role in improving the mechanical property of transparent ceramics. So applying this kind of transparent phosphor ceramic to LED components as packaging material can significantly improve the lifetime and reliability of LED products.

  14. High-purity silica reflecting heat shield development

    NASA Technical Reports Server (NTRS)

    Congdon, W. M.

    1974-01-01

    A high-purity, fused-silica reflecting heat shield for the thermal protection of outer-planet probes was developed. Factors that strongly influence the performance of a silica heat shield were studied. Silica-bonded silica configurations, each prepared by a different technique, were investigated and rated according to its relative merits. Slip-casting was selected as the preferred fabrication method because it produced good reflectivity and good strength, and is relatively easy to scale up for a full-size outer-planet probe. The slips were cast using a variety of different particle sizes: continuous particle-size slips; monodisperse particle-size slips; and blends of monodisperse particle-size slips were studied. In general, smaller particles gave the highest reflectance. The monodisperse slips as well as the blend slips gave a higher reflectance than the continuous particle-size slips. An upgraded and fused natural quartz was used to study the effects of microstructure on reflectance and as the baseline to ascertain the increase in reflectance obtained from using a higher-purity synthetic material.

  15. Observing bulk diamond spin coherence in high-purity nanodiamonds.

    PubMed

    Knowles, Helena S; Kara, Dhiren M; Atatüre, Mete

    2014-01-01

    Nitrogen-vacancy (NV) centres in diamond are attractive for research straddling quantum information science, nanoscale magnetometry and thermometry. Whereas ultrapure bulk diamond NVs sustain the longest spin coherence times among optically accessible spins, nanodiamond NVs exhibit persistently poor spin coherence. Here we introduce high-purity nanodiamonds accommodating record-long NV coherence times, >60 μs, observed through universal dynamical decoupling. We show that the main contribution to decoherence comes from nearby nitrogen impurities rather than surface states. We protect the NV spin free precession, essential to d.c. magnetometry, by driving solely these impurities into the motional narrowing regime. This extends the NV free induction decay time from 440 ns, longer than that in type Ib bulk diamond, to 1.27 μs, which is comparable to that in type IIa (impurity-free) diamond. These properties allow the simultaneous exploitation of both high sensitivity and nanometre resolution in diamond-based emergent quantum technologies. PMID:24270582

  16. High Purity Zirconium Tetrafluoride For Fluoride Glass Applications

    NASA Astrophysics Data System (ADS)

    Withers, Howard P.; Monk, V. A.; Cooper, G. A.

    1989-06-01

    A totally anhydrous process has been developed for the preparation of high purity zirconium tetrafluoride for use in low loss fluoride glass applications. The ZrF4 purityis 99.99997% with respect to all transition elements (excluding HO based on analysis by spark source mass spectrometry (SSMS) and graphite furnace/atomic absorption spectroscopy (GF/AA). The only transition elements detected by these techniques were Fe, Ni and Cr, while Co and Cu were consistently below the detection limits. The anhydrous nature of the process, which is strictly maintained by the choice of reactants, affords product with very low oxide and hydroxide content. Total oxygen concentrations of less than 10 ppm have been measured by the inert gas fusion technique. A ZBLAN glass composition prepared using this ZrF4 showed extremely low UV absorption having an absorption constant of 1 cm-1 at 198 nm. ZrF4 from this process was also used in a ZBLAN glass fiber whose minimum optical loss was measured at 6.3 dB/km over 150 meters of fiber. The process is straightforward to scale up and has also been demonstrated to be useful for the preparation of HfF4, BaF2, A1F3 and LaF3.

  17. Spectroscopic Determination of Trace Contaminants in High Purity Oxygen

    NASA Technical Reports Server (NTRS)

    Hornung, Steven D.

    2011-01-01

    Oxygen used for extravehicular activities (EVA) must be free of contaminants because a difference in a few tenths of a percent of argon or nitrogen content can mean significant reduction in available EVA time. These inert gases build up in the extravehicular mobility unit because they are not metabolized or scrubbed from the atmosphere. Measurement of oxygen purity above 99.5% is problematic, and currently only complex instruments such as gas chromatographs or mass spectrometers are used for these determinations. Because liquid oxygen boil-off from the space shuttle will no longer be available to supply oxygen for EVA use, other concepts are being developed to produce and validate high purity oxygen from cabin air aboard the International Space Station. A prototype optical emission technique capable of detecting argon and nitrogen below 0.1% in oxygen was developed at White Sands Test Facility. This instrument uses a glow discharge in reduced pressure gas to produce atomic emission from the species present. Because the atomic emission lines from oxygen, nitrogen, and argon are discrete and in many cases well-separated, trace amounts of argon and nitrogen can be detected in the ultraviolet and visible spectrum. This is a straightforward, direct measurement of the target contaminants and may lend itself to a device capable of on-orbit verification of oxygen purity. System design and optimized measurement parameters are presented.

  18. Permeation of oxygen through high purity, large grain silver

    NASA Technical Reports Server (NTRS)

    Outlaw, R. A.; Peregoy, W. K.; Hoflund, Gar B.

    1987-01-01

    The permeation of high purity, large grain Ag membranes by oxygen has been studied over the temperature range 400 to 800 C. The permeability was found to be quite linear and repeatable, but the magnitude was 3.2 times smaller than that determined by past research. Since previous investigators studied substantially less pure Ag and conducted experiments within much poorer vacuum environments (which indicates that their grain boundary density was much greater), the data presented here suggest oxygen transport through the membrane is primarily by grain boundary diffusion. The diffusivity measurements were found to exhibit two distinct linear regions, one above and one below a critical temperature of 630 C. The high-temperature data have an activation energy (11.1 kcal/mole) similar to that reported by others, but the low-temperature data have a higher activation energy (15.3 kcal/mole), which can be explained by impurity trapping in the grain boundaries. Vacuum desorption of the oxygen-saturated Ag was found to occur at a threshold of 630 C, which is consistent with the onset of increased mobility within the grain boundaries.

  19. Recent developments in high purity niobium metal production at CBMM

    SciTech Connect

    Abdo, Gustavo Giovanni Ribeiro Sousa, Clovis Antonio de Faria Guimarães, Rogério Contato Ribas, Rogério Marques Vieira, Alaércio Salvador Martins Menezes, Andréia Duarte Fridman, Daniel Pallos Cruz, Edmundo Burgos

    2015-12-04

    CBMM is a global supplier of high quality niobium products including pure niobium, the focus of this paper. CBMM’s position has been consolidated over three decades of producing high purity niobium metal ingots. The company supplies, among other products, commercial and reactor grade niobium ingots. One of the main uses of CBMM’s ingots is for the manufacture of particle accelerators (superconducting radio frequency – SRF – cavities), where the purity and homogeneity of niobium metal is essentially important for good performance. CBMM constantly strives to improve process controls and product quality, and is currently implementing innovations in production, research and development to further improve ingot quality. The main aim is to reduce the content of interstitial elements, such as nitrogen (N), oxygen (O), carbon (C), and hydrogen (H), starting with the raw materials through the final step of ingot production. CBMM held the first trial to produce the world’s largest-diameter niobium ingot (as cast 535 mm). The results of this initial trial presented very low levels of interstitial impurities (N, O, C, H), allowing the achievement of residual resistivity ratio (RRR) values very close to 300 in a six-melt process in an electron beam furnace. These values were reached with 850 ppm of tantalum. SRF cavities will be produced with this material in order to study the effect of low impurities and high RRR on the Q factor and accelerating gradient.

  20. Recent developments in high purity niobium metal production at CBMM

    NASA Astrophysics Data System (ADS)

    Abdo, Gustavo Giovanni Ribeiro; Sousa, Clovis Antonio de Faria; Guimarães, Rogério Contato; Ribas, Rogério Marques; Vieira, Alaércio Salvador Martins; Menezes, Andréia Duarte; Fridman, Daniel Pallos; Cruz, Edmundo Burgos

    2015-12-01

    CBMM is a global supplier of high quality niobium products including pure niobium, the focus of this paper. CBMM's position has been consolidated over three decades of producing high purity niobium metal ingots. The company supplies, among other products, commercial and reactor grade niobium ingots. One of the main uses of CBMM's ingots is for the manufacture of particle accelerators (superconducting radio frequency - SRF - cavities), where the purity and homogeneity of niobium metal is essentially important for good performance. CBMM constantly strives to improve process controls and product quality, and is currently implementing innovations in production, research and development to further improve ingot quality. The main aim is to reduce the content of interstitial elements, such as nitrogen (N), oxygen (O), carbon (C), and hydrogen (H), starting with the raw materials through the final step of ingot production. CBMM held the first trial to produce the world's largest-diameter niobium ingot (as cast 535 mm). The results of this initial trial presented very low levels of interstitial impurities (N, O, C, H), allowing the achievement of residual resistivity ratio (RRR) values very close to 300 in a six-melt process in an electron beam furnace. These values were reached with 850 ppm of tantalum. SRF cavities will be produced with this material in order to study the effect of low impurities and high RRR on the Q factor and accelerating gradient.

  1. Improved scheme for the analysis of high-purity talc.

    PubMed

    Norwitz, G; Gordon, H

    1977-01-01

    An improved method is proposed for the determination of silica, magnesium oxide, R(2)O(3), ferric oxide, calcium oxide, and aluminium oxide in high-purity talc. In the method for silica and magnesium oxide, the sample is fused with sodium carbonate and the cooled melt is dissolved with perchloric acid in such a manner that it floats free from the crucible (in previous schemes for the analysis of talc there are frequently mechanical losses due to the difficulty of removing the magnesium silicate melt from the crucible). The solution is then evaporated to fumes of perchloric acid and the silica is filtered off and ignited. The magnesium oxide is determined in the filtrate by precipitation as magnesium ammonium phosphate and a correction is made for the calcium which is precipitated along with the magnesium ammonium phosphate. R(2)O(3) is determined after treatment of the sample with nitric and hydrofluoric acids and evaporation to fumes of perchloric acid. Iron oxide and calcium oxide are determined by atomic absorption, after treatment with nitric and hydrofluoric acids and evaporation to fumes of perchloric acid. Al(2)O(3) is calculated by difference. PMID:18962055

  2. Modified matrix volatilization setup for characterization of high purity germanium.

    PubMed

    Meruva, Adisesha Reddy; Raparthi, Shekhar; Kumar, Sunil Jai

    2016-01-01

    Modified matrix volatilization (MV) method has been described to characterize high purity germanium material of 7 N (99.99999%) purity. Transport of both, the chlorine gas generated in-situ in this method and the argon gas (carrier) is fine controlled by means of a mass flow controller. This enabled both uniform reaction of chlorine gas with the germanium matrix and smooth removal of germanium matrix as its chloride. This resulted in improvement in the reproducibility of the analytical results. The use of quartz reaction vessel has lead to the reduction in the process blank levels. The combined effect of these modifications in the MV setup has resulted in very consistent and low process blanks and hence improved detection limits of this method. Applicability of the method has been expanded to rare earth elements and other elements after examining their recoveries. The quantification is done by using inductively coupled plasma quadrupole mass spectrometer (ICP-QMS) and continuum source graphite furnace atomic absorption spectrometry (CS-GFAAS). In the absence of certified reference materials for high pure germanium, the accuracy of the method is established by spike recovery tests. The precision of the method has been found to vary from 1 to 30% for concentrations between 1 and 30 ng g(-1). The limits of detection (LOD) for the target analytes are found to be between 18 and 0.033 ng g(-1). PMID:26695261

  3. Boron-Doped Strontium-Stabilized Bismuth Cobalt Oxide Thermoelectric Nanocrystalline Ceramic Powders Synthesized via Electrospinning

    NASA Astrophysics Data System (ADS)

    Koçyiğit, Serhat; Aytimur, Arda; Çınar, Emre; Uslu, İbrahim; Akdemir, Ahmet

    2014-01-01

    Boron-doped strontium-stabilized bismuth cobalt oxide thermoelectric nanocrystalline ceramic powders were produced by using a polymeric precursor technique. The powders were characterized by using x-ray diffraction (XRD), scanning electron microscopy (SEM), and physical properties measurement system (PPMS) techniques. The XRD results showed that these patterns have a two-phase mixture. The phases are face-centered cubic (fcc) and body-centered cubic (bcc). Values of the crystallite size, dislocation density, and microstrain were calculated by using the Scherrer equation. The lattice parameters were calculated for fcc and bcc phases. The SEM results showed that needle-like grains are formed in boron-undoped composite materials, but the needle-like grains changed to the plate-like grains with the addition of boron. The distribution of the nanofiber diameters was calculated and the average diameter of the boron-doped sample is smaller than the boron-undoped one. PPMS values showed that the electrical resistivity values decreased, but the thermal conductivity values, the Seebeck coefficients, and figure of merit ( ZT) increased with increasing temperature for the two samples.

  4. Application of a Barrier Filter at a High Purity Synthetic Graphite Plant, CRADA 99-F035, Final Report

    SciTech Connect

    National Energy Technology Laboratory

    2000-08-31

    Superior Graphite Company and the US Department of Energy have entered into a Cooperative Research and Development Agreement (CRADA) to study the application of ceramic barrier filters at its Hopkinsville, Kentucky graphite plant. Superior Graphite Company is a worldwide leader in the application of advanced thermal processing technology to produce high purity graphite and carbons. The objective of the CRADA is to determine the technical and economic feasibility of incorporating the use of high-temperature filters to improve the performance of the offgas treatment system. A conceptual design was developed incorporating the ceramic filters into the offgas treatment system to be used for the development of a capital cost estimate and economic feasibility assessment of this technology for improving particulate removal. This CRADA is a joint effort of Superior Graphite Company, Parsons Infrastructure and Technology Group, and the National Energy Technology Laboratory (NETL) of the US Department of Energy (DOE).

  5. Influence of Barium Hexaferrite on Magnetic Properties of Hydroxyapatite Ceramics.

    PubMed

    Jarupoom, P; Jaita, P

    2015-11-01

    Hydroxyapatite (HA) powders was derived from natural bovine bone by sequence of thermal processes. The barium hexaferrite (BF) find magnetic powders were added into HA powders in ratio of 1-3 vol.%. The HA-BF ceramics were prepared by a solid state reaction method and sintered at 1250 degrees C for 2 h. Effects of BF additive on structural, physical and magnetic properties of HA ceramics were investigated. X-ray diffraction revealed that all HA-BF samples showed a main phase of high purity hydroxyapatite [Ca10(PO4)6(OH)2] with calcium and phosphate molar ratio of 1.67. The addition of BF into HA inhibited grain growth and caused an improvement of mechanical properties. The M-H hysteresis loops also showed an improvement in magnetic behavior for higher content of BF. Moreover, in vitro bioactivity test indicated that the 2-3 vol.% sample may be suitable for biological applications. PMID:26726671

  6. Synthesis of nano-bioactive glass-ceramic powders and its in vitro bioactivity study in bovine serum albumin protein

    NASA Astrophysics Data System (ADS)

    Nabian, Nima; Jahanshahi, Mohsen; Rabiee, Sayed Mahmood

    2011-07-01

    Bioactive glasses and ceramics have proved to be able to chemically bond to living bone due to the formation of an apatite-like layer on its surface. The aim of this work was preparation and characterization of bioactive glass-ceramic by sol-gel method. Nano-bioglass-ceramic material was crushed into powder and its bioactivity was examined in vitro with respect to the ability of hydroxyapatite layer to form on the surface as a result of contact with bovine serum albumin (BSA) protein. The obtained nano-bioactive glass-ceramic was analyzed before and after contact with BSA solution. This study used scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray powder diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) analysis to examine its morphology, crystallinity and composition. The TEM images showed that the NBG particles size were 10-40 nm. Bioactivity of nanopowder was confirmed by SEM and XRD due to the presence of a rich bone-like apatite layer. Therefore, this nano-BSA-bioglass-ceramic composite material is promising for medical applications such as bone substitutes and drug carriers.

  7. Electrolytic production of high purity aluminum using inert anodes

    DOEpatents

    Ray, Siba P.; Liu, Xinghua; Weirauch, Jr., Douglas A.

    2001-01-01

    A method of producing commercial purity aluminum in an electrolytic reduction cell comprising inert anodes is disclosed. The method produces aluminum having acceptable levels of Fe, Cu and Ni impurities. The inert anodes used in the process preferably comprise a cermet material comprising ceramic oxide phase portions and metal phase portions.

  8. The influence of ZrB2-SiC powders mechanical treatment on the structure of sintered ceramic composites

    NASA Astrophysics Data System (ADS)

    Buyakova, S.; Burlachenko, A.; Mirovoi, Yu; Sevostiyanova, I.; Kulkov, S.

    2016-07-01

    The effect of mechanical treatment by planetary ball milling on the properties of hot pressed ZrB2 - SiC ceramics was studied. It was shown that material densification after mechanical treatment is finished at initial stages of sintering process. Addition of SiC leads to an essential increase of sample density to 99% of theoretically achievable for powder with 2% of SiC, as compared with ZrB2 with the density less than 76%. It was demonstrated that all defects that were accumulated during mechanical treatment are annealed during hot pressing, and there are no changes of CDD values in sintered ceramics.

  9. Traction characteristics of high-temperature powder-lubricated ceramics (Si3N4/alpha SiC)

    SciTech Connect

    Heshmat, Hooshang; Dill, J.F. )

    1992-04-01

    As part of a development program for a high-temperature, dry-lubricated bearing technology and lubricant system, a high-speed high-temperature disk-on-disk tribometer was utilized and a matrix of traction data covering a range of load, speed, and temperature was obtained. The influence of dry powder lubricants, TiO2 and MoS2, on the traction coefficients between two ceramic materials, Si3N4 and SiC, was investigated. The results of this investigation are characteristic curves for the traction coefficient vs the slide/roll ratio with dry powders which are reminiscent of fluids, and the observation of dry powder lubricants' lower traction coefficients and wear. Measured tractions are found to be a strong function of powder-lubricant type, and values decrease moderately with slide-to-roll ration and load. The data show a weak sensitivity to temperature. 9 refs.

  10. Synthesis of high purity metal oxide nanoparticles for optical applications

    NASA Astrophysics Data System (ADS)

    Baker, C.; Kim, W.; Friebele, E. J.; Villalobos, G.; Frantz, J.; Shaw, L. B.; Sadowski, B.; Fontana, J.; Dubinskii, M.; Zhang, J.; Sanghera, J.

    2014-09-01

    In this paper we present our recent research results in synthesizing various metal oxide nanoparticles for use as laser gain media (solid state as well as fiber lasers) and transparent ceramic windows via two separate techniques, co-precipitation and flame spray pyrolysis. The nanoparticles were pressed into ceramic discs that exhibited optical transmission approaching the theoretical limit and showed very high optical-to-optical lasing slope efficiency. We have also synthesized sesquioxide nanoparticles using a Flame Spray Pyrolysis (FSP) technique that leads to the synthesis of a metastable phase of sesquioxide which allows fabricating excellent optical quality transparent windows with very fine grain sizes. Finally, we present our research in the synthesis of rare earth doped boehmite nanoparticles where the rareearth ion is encased in a cage of aluminum and oxygen to prevent ion-ion proximity and energy transfer. The preforms have been drawn into fibers exhibiting long lifetimes and high laser efficiencies.

  11. The Hydrometallurgical Extraction and Recovery of High-Purity Silver

    NASA Astrophysics Data System (ADS)

    Hoffmann, James E.

    2012-06-01

    -bearing inputs, will be described in detail to demonstrate how typical chemical engineering unit process and unit operations have supplanted classic smelting and fire refining techniques. The Kennecott Copper Company, which has operated a hydrometallurgical circuit successfully for the recovery of high-purity silver from the slimes wet chlorination residue, has permitted me to provide some operation information and results using the technology. Both Phelps Dodge and Kennecott should be recognized for their forward-looking attitude in undertaking the conversion of conceptual chemistry into successful, full-scale plants. The process as employed at Phelps Dodge is discussed at length in reference (J.E. Hoffmann and B. Wesstrom: Hydrometallurgy, 1994, vol. 94, pp. 69-105).

  12. Emission spectra of LiYNbO 3:RE 3+ (=Sm 3+ or Dy 3+) ceramic powders

    NASA Astrophysics Data System (ADS)

    Bhaskar Kumar, G.; Buddhudu, S.

    2008-12-01

    Sm 3+ or Dy 3+:LiYNbO 3 ceramic powders have been synthesized by a solid-state reaction method to study their photoluminescence properties in order to evaluate emission performance. Upon exposure to the UV lamp, these luminescent ceramic powders have displayed a bright reddish-orange ( 4G 5/2→ 6H 7/2) (Sm 3+) and an yellow ( 4F 9/2→ 6H 13/2) (Dy 3+) color emissions, respectively. In addition, these phosphors have also been characterized for their structures and morphology from the measurement of X-ray diffraction (XRD), Fourier transform-infrared (FTIR), scanning electron microscope (SEM), EDAX, thermogravimetry (TG) and differential thermal analysis (DTA) results.

  13. Large-scale fabrication of boron nitride nanotubes with high purity via solid-state reaction method

    PubMed Central

    2014-01-01

    An effective solid-state reaction method is reported for synthesizing boron nitride nanotubes (BNNTs) in large scale and with high purity by annealing amorphous boron powder and ferric chloride (FeCl3) catalyst in ammonia atmosphere at elevated temperatures. FeCl3 that has rarely been utilized before is introduced not only as a catalyst but also as an efficient transforming agent which converts boron powder into boron chloride (BCl3) vapor in situ. The nanotubes are bamboo in shape and have an average diameter of about 90 nm. The effect of synthetic temperatures on nanotube morphology and yield is investigated. The photoluminescence (PL) measurement shows emission bands of the nanotubes at 354, 423, 467, and 666 nm. A combined growth mechanism of vapor–liquid-solid (VLS) and solid–liquid-solid (SLS) model is proposed for the formation of the BNNTs. PMID:25313303

  14. Defect structural evolution in high purity tungsten irradiated with electrons using high voltage electron microscope

    NASA Astrophysics Data System (ADS)

    Fukuzumi, S.; Yoshiie, T.; Satoh, Y.; Xu, Q.; Mori, H.; Kawai, M.

    2005-08-01

    Four types of high purity tungsten were irradiated with 2 MeV electrons to 5 dpa using a high voltage electron microscope, and defect structural evolutions were examined as a function of the irradiation temperature and the concentration of impurity atoms. Three of materials were made by sintering of tungsten powder with purity of 99.999% (5N-W), 99.99% (PF-W) and 99.95% (N-W), and one was a chemical vapor deposited tungsten of 99.9999% (CVD-W) purity. The formation of interstitial type dislocation loops is observed above room temperature by electron irradiation. In sintered tungsten, the number density of loops increases with increasing density of impurity atoms, i.e., N-W > PF-W > 5N-W. The density of loops in CVD-W is relatively high, contrary to its purity. In CVD-W, a heterogeneous formation of loops is observed at above 573 K. Loops are aligned on layers, and no loops are formed between the layers. All four types of specimens have a change in slop of the temperature dependence of loop number density at around 500 K which is caused by impurity atoms. Results of radioactivation analysis and hardness testing are also presented.

  15. Preparation of metal-ceramic composites by sonochemical synthesis of metallic nano-particles and in-situ decoration on ceramic powders.

    PubMed

    Poulia, A; Sakkas, P M; Kanellopoulou, D G; Sourkouni, G; Legros, C; Argirusis, Chr

    2016-07-01

    Copper and nickel nanoparticles were synthesized using reducing agents in the presence of direct high energy ultra-sonication. The metallic nanoparticles were decorated on various ceramic substrates (e.g. α-Al2O3, and TiO2) leading to metal reinforced ceramics with up to 45% metallic content. Different parameters, such as the amount of precursor material or the substrate, as well as the intensity of ultrasound were examined, in order to evaluate the percentage of final metallic decoration on the composite materials. All products were characterized by means of Inductively Coupled Plasma Spectroscopy in order to investigate the loading with metallic particles. X-ray Diffraction and Scanning Electron Microscopy were also used for further sample characterization. Selected samples were examined using Transmission Electron Microscopy, while finally, some of the powders synthesized, were densified by means of Spark Plasma Sintering, followed by a SEM/EDX examination and an estimation of their porosity. PMID:26964967

  16. The Powdering Process with a Set of Ceramic Mills for Green Tea Promoted Catechin Extraction and the ROS Inhibition Effect.

    PubMed

    Fujioka, Kouki; Iwamoto, Takeo; Shima, Hidekazu; Tomaru, Keiko; Saito, Hideki; Ohtsuka, Masaki; Yoshidome, Akihiro; Kawamura, Yuri; Manome, Yoshinobu

    2016-01-01

    For serving green tea, there are two prominent methods: steeping the leaf or the powdered leaf (matcha style) in hot water. The purpose of the present study was to reveal chemical and functional differences before and after the powdering process of green tea leaf, since powdered green tea may contribute to expanding the functionality because of the different ingesting style. In this study, we revealed that the powdering process with a ceramic mill and stirring in hot water increased the average extracted concentration of epigallocatechin gallate (EGCG) by more than three times compared with that in leaf tea using high-performance liquid chromatography (HPLC) and liquid chromatography-tandem mass Spectrometry (LC-MS/MS) analyses. Moreover, powdered green tea has a higher inhibition effect of reactive oxygen species (ROS) production in vitro compared with the same amount of leaf tea. Our data suggest that powdered green tea might have a different function from leaf tea due to the higher catechin contents and particles. PMID:27077834

  17. Low temperature synthesis of high purity monoclinic celsian using topaz

    SciTech Connect

    Talmy, I.G.; Haught, D.A.

    1991-02-19

    This patent describes a process for preparing monoclinic BaO {center dot} Al{sub 2}O{sub 3} {center dot} 2SiO{sub 2}. It comprises: forming an intimate reaction mixture of powders of topaz and BaCO{sub 3} wherein the molar ratio of topaz to BaCO{sub 3} is from 2:1 to 4:1; and heating the reaction mixture to initiate a celsian formation reaction, in an atmosphere of gases generated by the celsian formation reaction, at a temperature in the range of from 900{degrees} C. to less than 1590{degrees} C. until the monoclinic celsian is produced.

  18. A Dilatometric Study of Sintering of Composite Ceramics Manufactured from Ultrafine Zro2(Y)-Al2O3 Powders Under Different Thermal-Temporal Firing Conditions

    NASA Astrophysics Data System (ADS)

    Surzhikov, A. P.; Frangulyan, T. S.; Ghyngazov, S. A.; Vasiliev, I. P.

    2014-07-01

    Using dilatometry, kinetic principles of sintering of composite ZrO2(Y)-Al2O3 ceramic material made from ultrafine powders synthesized at the Siberian Chemical Integrated Works are investigated. It is shown that under heating conditions, sintering of the composite ceramics under study occurs within a few stages that are closely related to the structural-phase transformations taking place in the composite powder mixture. At the firing temperatures Т > 1500 С and during long isothermal times, negative phenomena develop in the ceramic material, which give rise to its undesired dilatation and cracking in the course of cooling.

  19. Synthesis of lead-free piezoelectric powders by ultrasonic-assisted hydrothermal method and properties of sintered (K0.48Na0.52)NBO3 ceramics.

    PubMed

    Isobe, Gaku; Maeda, Takafumi; Bornmann, Peter; Hemsel, Tobias; Morita, Takeshi

    2014-02-01

    (K,Na)NbO3 ceramics have attracted much attention as lead-free piezoelectric materials with high piezoelectric properties. High-quality (K,Na)NbO3 ceramics can be sintered using KNbO3 and NaNbO3 powders synthesized by a hydrothermal method. In this study, to enhance the quality factor of the ceramics, high-power ultrasonic irradiation was employed during the hydrothermal method, which led to a reduction in the particle size of the resultant powders. PMID:24474129

  20. Functionalization of Ceramic Metal Oxide Powders and Ceramic Membranes by Perfluoroalkylsilanes and Alkylsilanes Possessing Different Reactive Groups: Physicochemical and Tribological Properties.

    PubMed

    Kujawa, Joanna; Kujawski, Wojciech

    2016-03-23

    The functionalization of ceramic materials, metal oxide powders (TiO2 and ZrO2), and ceramic membranes (5 kD TiO2 and 300 kD TiO2) was performed and thoroughly discussed. The objective of the functionalization was to change the natively hydrophilic character to the hydrophobic. The hydrophilic character of the ceramics generates limitations in wider application of such materials. Material functionalization was performed using perfluoroalkylsilanes and trifunctional(octyl)silanes possessing three different reactive functional groups: -Cl, -OMe, and -OEt. The characterization of functionalized metal oxide powders and ceramic membranes was assessed by a combination of various analytical methods and techniques: NMR, TGA, HR-TEM, FT-IR, SEM-EDX, AFM, and contact goniometry. The impact of molecular structure of grafting agents (type of reactive group), time of functionalization process (5-15 min), and type of membrane morphology on the material, physicochemical, and tribological properties was studied. Effectiveness of hydrophobization was confirmed by HR-TEM technique. The thickness of the attached hydrophobic nanolayer on the surface of ceramics was around 2.2 nm. It was found that the stable hydrophobic surfaces were obtained by functionalization with both fluorinated and nonfluorinated modifiers. The materials modified with perfluoroalkylsilanes (FC6OEt3) and trichloro(octyl)silanes (C6Cl3) during 15 min hydrophobization possess comparable properties: contact angle (CA) equal to 130° and 133°; roughness RMS of 10.2 and 12 nm; adhesive force of 4.1 and 5.7 nN; and Young modulus of 135 and 130 GPa, respectively. The relation between hydrophobicity level and ceramic membrane roughness was discussed applying the Kao diagram concept. (29)Si NMR results show that type of modifier has an important influence on grafting efficiency and on the mode of the grafting molecules attachment. In case of grafting with n-octyltrichlorosilane (C6OCl3) and n-octyltrimethoxysilane (C6

  1. Dielectric Performance of a High Purity HTCC Alumina at High Temperatures - a Comparison Study with Other Polycrystalline Alumina

    NASA Technical Reports Server (NTRS)

    Chen, Liangyu

    2014-01-01

    A very high purity (99.99+%) high temperature co-fired ceramic (HTCC) alumina has recently become commercially available. The raw material of this HTCC alumina is very different from conventional HTCC alumina, and more importantly there is no glass additive in this alumina material for co-firing processing. Previously, selected HTCC and LTCC (low temperature co-fired ceramic) alumina materials were evaluated at high temperatures as dielectric and compared to a regularly sintered 96% polycrystalline alumina (96% Al2O3), where 96% alumina was used as the benchmark. A prototype packaging system based on regular 96% alumina with Au thickfilm metallization successfully facilitated long term testing of high temperature silicon carbide (SiC) electronic devices for over 10,000 hours at 500 C. In order to evaluate this new high purity HTCC alumina for possible high temperature packaging applications, the dielectric properties of this HTCC alumina substrate were measured and compared with those of 96% alumina and a previously tested LTCC alumina from room temperature to 550 C at frequencies of 120 Hz, 1 KHz, 10 KHz, 100 KHz, and 1 MHz. A parallel-plate capacitive device with dielectric of the HTCC alumina and precious metal electrodes were used for measurements of the dielectric constant and dielectric loss of the co-fired alumina material in the temperature and frequency ranges. The capacitance and AC parallel conductance of the capacitive device were directly measured by an AC impedance meter, and the dielectric constant and parallel AC conductivity of the dielectric were calculated from the capacitance and conductance measurement results. The temperature and frequency dependent dielectric constant, AC conductivity, and dissipation factor of the HTCC alumina substrate are presented and compared to those of 96% alumina and a selected LTCC alumina. Other technical advantages of this new co-fired material for possible high packaging applications are also discussed.

  2. A cleaner two-step synthesis of high purity diallyldimethylammonium chloride monomers for flocculant preparation.

    PubMed

    Tian, Bing-hui; Fan, Bin; Peng, Xian-jia; Luan, Zhao-kun

    2005-01-01

    In order to improve the flocculation efficiency of polydiallyldimethylammonium chloride (PDADMAC), high molecular weight PDADMAC should be prepared from high purity diallyldimethylammonium chloride(DADMAC) monomers. In this paper, a cleaner method with microwave irradiation and alkali solidification was proposed for preparing high pure DADMAC by selective heating under low temperature, and the prepared high purity DADMAC is characterized using FTIR and atomic absorption spectrometry. The new method provides a solution to the key technical problem of PDADMAC synthesis. Comparing with the conventional methods, the results showed that the advantages of the novel synthesis include: (a) high purity DADMAC is improved from 57% to 71%; (b) reaction time of tertiary amine preparation is shortened from 6 h to 7 min; (c) water instead of acetone was used as reaction medium; (d) toxic by-products, wastewater and waste gas are eliminated. Flocculant made from the synthesized high purity DADMAC monomers was proved more efficient in flocculation tests. PMID:16313006

  3. High purity germanium crystal growth at the University of South Dakota

    NASA Astrophysics Data System (ADS)

    Wang, Guojian; Mei, Hao; Mei, Dongming; Guan, Yutong; Yang, Gang

    2015-05-01

    High-purity germanium crystal growth is challenging work, requiring the control of individual crystal properties such as the impurity distribution, the dislocation density, and the crystalline structure. Currently, we grow high-purity germanium crystals by the Czochralski method in our laboratory in order to understand the details of the growing process, especially for large diameter crystals. In this paper, we report the progress of detector-grade germanium crystal growth at the University of South Dakota.

  4. Optical and laser characterization of Nd:YAG ceramics elements

    NASA Astrophysics Data System (ADS)

    Librant, Zdzisław; Węglarz, Helena; Wajler, Anna; Tomaszewski, Henryk; Łukasiewicz, Tadeusz; Jabczyński, Jan K.; Zendzian, Waldemar; Kwiatkowski, Jacek

    2008-12-01

    The Nd:YAG ceramics of nominal 1% and 2% Nd dopant were produced by a solid-state reaction of high-purity (4N) nanometric oxides powders i.e. Al2O3, Y2O3 and Nd2O3. Yttrium oxide nanopowder (XRD crystallite size of 79 nm) was produced by precipitation from water solution of high-purity hydrated nitrate, by means of ammonia hydro-carbonate. The cold isostatic pressing method was applied to densify granulated powder. Further the sintering and annealing processes were deployed to produce the final Nd:YAG ceramic samples. Mean grain sizes of about 20 µm and grain boundaries less than 10 nm of elaborated Nd:YAG ceramic samples were evaluated in SEM and TEM measurements. Thus, in microscale the quality of obtained ceramic was quite satisfactory. However, in macroscale, the samples had unacceptable level of voids and pores observed in visual inspection, which resulted in low 76% transmission, corresponding to extinction coefficient of 0.32 cm-1 at 1064-nm wavelength. The sizes of defects, pores and inclusions were of several dozens of micrometer. The active elements of rod and slab shape were fabricated and characterized in two diode pumping laser set ups. In end pumping configuration as a pump source 20-W fiber coupled laser diode was deployed. For the low duty cycle pumping (1 ms/20 Hz) above 30% slope efficiency was achieved. In the best case, 3.7 W of output power for 18 W of pump power, with M2 <1.4 were demonstrated for uncoated ceramics rod of φ4x3mm size. We have used uncoated elements, thus we can expect increase in laser parameters for optimized pumping conditions and samples with anti-reflective coatings. The parameters of elaborated ceramic material at this stage of work are unsatisfactory for laser application. However, the results of TEM measurements and laser characterizations seems to be quite promising..

  5. Characterization of high-purity niobium structures fabricated using the electron beam melting process

    NASA Astrophysics Data System (ADS)

    Terrazas Najera, Cesar Adrian

    Additive Manufacturing (AM) refers to the varied set of technologies utilized for the fabrication of complex 3D components from digital data in a layer-by-layer fashion. The use of these technologies promises to revolutionize the manufacturing industry. The electron beam melting (EBM) process has been utilized for the fabrication of fully dense near-net-shape components from various metallic materials. This process, catalogued as a powder bed fusion technology, consists of the deposition of thin layers (50 - 120microm) of metallic powder particles which are fused by the use of a high energy electron beam and has been commercialized by Swedish company Arcam AB. Superconducting radio frequency (SRF) cavities are key components that are used in linear accelerators and other light sources for studies of elemental physics. Currently, cavity fabrication is done by employing different forming processes including deep-drawing and spinning. In both of the latter techniques, a feedstock high-purity niobium sheet with a thickness ranging from 3-4 mm is mechanically deformed and shaped into the desired geometry. In this manner, half cavities are formed that are later joined by electron beam welding (EBW). The welding step causes variability in the shape of the cavity and can also introduce impurities at the surface of the weld interface. The processing route and the purity of niobium are also of utmost importance since the presence of impurities such as inclusions or defects can be detrimental for the SRF properties of cavities. The focus of this research was the use of the EBM process in the manufacture of high purity niobium parts with potential SRF applications. Reactor grade niobium was plasma atomized and used as the precursor material for fabrication using EBM. An Arcam A2 system was utilized for the fabrication. The system had all internal components of the fabrication chamber replaced and was cleaned to prevent contamination of niobium powder. A mini-vat, developed at

  6. Characterization of high-purity niobium structures fabricated using the electron beam melting process

    NASA Astrophysics Data System (ADS)

    Terrazas Najera, Cesar Adrian

    Additive Manufacturing (AM) refers to the varied set of technologies utilized for the fabrication of complex 3D components from digital data in a layer-by-layer fashion. The use of these technologies promises to revolutionize the manufacturing industry. The electron beam melting (EBM) process has been utilized for the fabrication of fully dense near-net-shape components from various metallic materials. This process, catalogued as a powder bed fusion technology, consists of the deposition of thin layers (50 - 120microm) of metallic powder particles which are fused by the use of a high energy electron beam and has been commercialized by Swedish company Arcam AB. Superconducting radio frequency (SRF) cavities are key components that are used in linear accelerators and other light sources for studies of elemental physics. Currently, cavity fabrication is done by employing different forming processes including deep-drawing and spinning. In both of the latter techniques, a feedstock high-purity niobium sheet with a thickness ranging from 3-4 mm is mechanically deformed and shaped into the desired geometry. In this manner, half cavities are formed that are later joined by electron beam welding (EBW). The welding step causes variability in the shape of the cavity and can also introduce impurities at the surface of the weld interface. The processing route and the purity of niobium are also of utmost importance since the presence of impurities such as inclusions or defects can be detrimental for the SRF properties of cavities. The focus of this research was the use of the EBM process in the manufacture of high purity niobium parts with potential SRF applications. Reactor grade niobium was plasma atomized and used as the precursor material for fabrication using EBM. An Arcam A2 system was utilized for the fabrication. The system had all internal components of the fabrication chamber replaced and was cleaned to prevent contamination of niobium powder. A mini-vat, developed at

  7. Electrical Properties of BaTiO3-Based Multilayer Ceramic Capacitors Sintered with Plasma-Treated Glass Powder

    NASA Astrophysics Data System (ADS)

    Jeong, Dae-Yong; Lee, Soon-il; Lee, Heun-Young; Kim, Min-Kee; Yoon, Jung-Rag

    2013-10-01

    The influence of glass power morphology on the electrical and microstructural properties of BaTiO3-based multilayer ceramic capacitors (MLCCs) was investigated to enhance the reliability of MLCCs. For a sintering additive, glass particles of different sizes and shapes were prepared by jet-milling and RF plasma treatment. Plasma treatment decreased the glass particle size and transformed the irregular shape of glass particles into homogeneous spherical shapes. It was found that MLCCs sintered with plasma-treated glass powder have a more homogeneous microstructure, a clear core-shell structure, a more stable capacitance against voltage and temperature changes, and a higher degradation resistance. It is inferred that nanosized spherical glass powder prepared by plasma treatment helps so-called magic dopants such as rare-earth elements to be distributed homogeneously around the BaTiO3 particles.

  8. Direct use of celestite to prepare presintered SrFe 12O 19 powders

    NASA Astrophysics Data System (ADS)

    Mozaffari, Mortaza; Amighian, Jamshid

    2002-08-01

    Mineral celestite was directly used to prepare presintered single-phase Sr-ferrite powders for fabrication of sintered permanent magnets. The starting materials were high-purity domestic celestite, modified iron oxide and sodium carbonate. The role of sodium carbonate is firstly to promote the displacement solid-state reaction and secondly to lower the temperature during calcining stage. A vibrating sample magnetometer was used to measure magnetic parameters of the powders. The results were compared with those of the powders prepared by conventional ceramic process. Lower reaction temperature of 1000°C and low-cost celestite show that this process is more economical for production of presintered SrFe 12O 19 powders than the conventional one.

  9. Microstructural changes in NiFe2O4 ceramics prepared with powders derived from different fuels in sol-gel auto-combustion technique

    NASA Astrophysics Data System (ADS)

    Chauhan, Lalita; Bokolia, Renuka; Sreenivas, K.

    2016-05-01

    Structural properties of Nickel ferrite (NiFe2O4) ceramics prepared from powders derived from sol gel auto-combustion method using different fuels (citric acid, glycine and Dl-alanine) are compared. Changes in the structural properties at different sintering temperatures are investigated. X-ray diffraction (XRD) confirms the formation of single phase material with cubic structure. Ceramics prepared using the different powders obtained from different fuels show that that there are no significant changes in lattice parameters. However increasing sintering temperatures show significant improvement in density and grain size. The DL-alanine fuel is found to be the most effective fuel for producing NIFe2O4 powders by the sol-gel auto combustion method and yields highly crystalline powders in the as-burnt stage itself at a low temperature (80 °C). Subsequent use of the powders in ceramic manufacturing produces dense NiFe2O4 ceramics with a uniform microstructure and a large grain size.

  10. Preparation and dielectric properties of the lead-free BaFe1/2Nb1/2O3 ceramics obtained from mechanically triggered powder

    NASA Astrophysics Data System (ADS)

    Bochenek, Dariusz; Niemiec, Przemysław; Szafraniak-Wiza, Izabela; Adamczyk, Małgorzata; Skulski, Ryszard

    2015-10-01

    In the paper the influence of mechanical activation of the powder on the final dielectric properties lead-free Ba(Fe1/2Nb1/2)O3 (BFN) ceramic was examined. The BFN ceramics were obtained by 3-steps route. Firstly, the substrates were pre-homogenized in a planetary ball mill. Than, the powder was activated in vibratory mill (the shaker type SPEX 8000 Mixer Mill) for different duration between 25 h and 100 h. The influence of the milling time on the BFN powder was monitored by X-ray diffraction. The diffraction data confirmed that the milling process of the starting components is accompanied by partial synthesis of the BFN materials. The longer of the high-energy milling duration the powders results in increasing the amount of amorphous/nanocrystalline content. The mechanically activated materials were sintered in order to obtain the ceramic samples. During this temperature treatment the final crystallisation of the powder appeared what was confirmed by XRD studies. The performed dielectric measurements have revealed the reduction of the dielectric loss of the BFN ceramics compared to materials obtained by classic methods.

  11. Synthesis and Characterization of Ba(Zr0.15Ti0.85)O3 Nano Powders by Oxalate Precipitation Method

    NASA Astrophysics Data System (ADS)

    Chen, Lei; Wang, Xiaohui; Qiao, Bin; Gui, Zhilun; Li, Longtu

    2006-08-01

    Barium zirconate titanate (BZT) is considered to be an important dielectric material for the fabrication of multilayer ceramic capacitors (MLCCs). The synthesis of nanocrystalline powders of high purity is the key to improving the performance of BZT-based ceramics. In this study, we developed Ba(Zr0.15Ti0.85)O3 nano powders with a perovskite structure and a homogeneous granularity through the oxalate precipitation method. The average particle size of the powders can be controlled from 30 to 100 nm at different calcining temperatures. The sintering property of the powders is superior to that of powders prepared by the conventional solid-state method, such that the more compact ceramics with a smaller grain size can be obtained at a sintering temperature of 1250 °C. The dielectric property of the ferroelectric-powder-based ceramics was so excellent for the development of dielectric materials for base-metal electrode multilayer ceramic capacitors (BME MLCCs) with a large capacitance.

  12. Impurity distribution in high purity germanium crystal and its impact on the detector performance

    NASA Astrophysics Data System (ADS)

    Wang, Guojian; Amman, Mark; Mei, Hao; Mei, Dongming; Irmscher, Klaus; Guan, Yutong; Yang, Gang

    High-purity germanium crystals were grown in a hydrogen atmosphere using the Czochralski method. The axial and radial distributions of impurities in the crystals were measured by Hall effect and Photo-thermal ionization spectroscopy (PTIS). Amorphous semiconductor contacts were deposited on the germanium crystals to make detectors. Three planar detectors were fabricated from three crystals with different net carrier concentrations (1.7, 7.9 and 10x1010 cm-3). We evaluated the electrical and spectral performance of three detectors. Measurements of gamma-ray spectra from 137Cs, 241Am and 60Co sources demonstrate that the detectors have excellent energy resolution. The relationship between the impurities and detector's energy resolution was analyzed. Keywords: High-purity germanium crystal, High-purity germanium detector This work is supported by DOE grant DE-FG02-10ER46709 and the state of South Dakota..

  13. [Preparation and optical properties of MgAl2O4/Ce:YAG transparent ceramics].

    PubMed

    He, Long-Fei; Fan, Guang-Han; Lei, Mu-Yun; Lou, Zai-Liang; Chen, Zhi-Wu; Xiao, Yao; Zheng, Shu-Wen; Zhang, Tao

    2013-05-01

    High-purity ultrafine MgAl2O4 powder was synthesized by metal-alkoxide method and calcining for 2-4 h. And then MgAl2O4/Ce:YAG transparent ceramics were fabricated by hot-pressed sintering and hot isostatic pressed sintering technique with YAG:Ce powder and MgAl2O4 powder. The transparent ceramics were characterized by XRD, SEM, EDS and fluorescence spectrometer, respectively. The results show that the crystal phase of the transparent ceramic was composed of MgAl2O4 and YAG,and the YAG phase dispersed well in the matrix of MgAl2O4. The excitation spectra had a weak band at 345 nm and a strong band at 475 nm. The broad emission peaks at about 533 nm were attributed to 5d-->4f transition of Ce3+ ions. Decay curves for the fluorescence of MgAl2O4/Ce:YAG transparent ceramic test show that the lifetime of the Ce:YAG glass ceramic was 59.74 ns. All results show that MgAl2O4/Ce:YAG transparent ceramic may be a promising fluorescent material for white LED applications. PMID:23905313

  14. Structure and properties of the ceramics based on quasicrystal powders processed by plasma coating method

    NASA Astrophysics Data System (ADS)

    Ekimov, E. A.; Ivanov, A. S.; Pal, A. F.; Petrzhik, M. I.; Ryabinkin, A. N.; Serov, A. O.

    2015-11-01

    Homogeneous incorporation of a small amount of binding material or modifying agent in the batch consisting of micron size particles is a problem of a composite material production process. In this work the problem is solved by deposition of a thin coating consisting of binding material on the initial powder particles by means of high-rate magnetron sputtering. The confinement of dusty particles in plasma was used in fine powder processing procedure. Composite powders based on the Al-Cu-Fe quasicrystalline particles with nickel coating were obtained. Their investigation showed that the method provides uniform incorporation of small quantities of additives (at concentration of about 3 wt. %) to fine powders. The powders were pressed at room temperature under quasi-hydrostatic conditions at high pressures. After pressing the samples were sintered in hydrogen at normal pressure. Structure and mechanical properties of the sintered samples were studied. The conditions of sintering the composite powder, which provide producing compacts with improved performance data, were established.

  15. Thermoluminescence (TL) properties and x-ray diffraction (XRD) analysis of high purity CaSO4:Dy TL material

    NASA Astrophysics Data System (ADS)

    Kamarudin, Nadira; Abdullah, Wan Saffiey Wan; Hamid, Muhammad Azmi Abdul; Dollah, Mohd Taufik

    2014-09-01

    This paper presents the characterization and TL properties of dysprosium (Dy) doped calcium sulfate (CaSO4) TL material produced by co-precipitation technique with 0.5mol% concentration of dopant. The morphology of the produced TL material was studied using scanning electron microscope (SEM) and the micrograph shows that rectangular parallelepiped shaped crystal with the average of 150 μm in length were produced. The crystallinity of the produced powder was studied using x-ray powder diffraction (XRD). The XRD spectra show that the TL material produced is high purity anhydrite CaSO4 with average crystallite size of 74 nm with orthorhombic crystal system. The TL behavior of produced CaSO4:Dy was studied using a TLD reader after exposure to gamma ray by Co60 source with the doses of 1,5 and 10 Gy. The glow curve shows linear response with glow peak around 230°C which is desired development in the field of radiation dosimetry.

  16. A simple dissolved metals mixing method to produce high-purity MgTiO{sub 3} nanocrystals

    SciTech Connect

    Pratapa, Suminar E-mail: suminar-pratapa@physics.its.ac.id; Baqiya, Malik A. E-mail: suminar-pratapa@physics.its.ac.id; Istianah, E-mail: suminar-pratapa@physics.its.ac.id; Lestari, Rina E-mail: suminar-pratapa@physics.its.ac.id; Angela, Riyan E-mail: suminar-pratapa@physics.its.ac.id

    2014-02-24

    A simple dissolved metals mixing method has been effectively used to produce high-purity MgTiO{sub 3} (MT) nanocrystals. The method involves the mixing of independently dissolved magnesium and titanium metal powders in hydrochloric acid followed by calcination. The phase purity and nanocrystallinity were determined by making use of laboratory x-ray diffraction data, to which Rietveld-based analyses were performed. Results showed that the method yielded only one type magnesium titanate powders, i.e. MgTiO{sub 3}, with no Mg{sub 2}TiO{sub 4} or MgTi{sub 2}O{sub 5} phases. The presence of residual rutile or periclase was controlled by adding excessive Mg up to 5% (mol) in the stoichiometric mixing. The method also resulted in MT nanocrystals with estimated average crystallite size of 76±2 nm after calcination at 600°C and 150±4 nm (at 800°C). A transmission electron micrograph confirmed the formation of the nanocrystallites.

  17. Low temperature recombination and trapping analysis in high purity gallium arsenide by microwave photodielectric techniques

    NASA Technical Reports Server (NTRS)

    Khambaty, M. B.; Hartwig, W. H.

    1972-01-01

    Some physical theories pertinent to the measurement properties of gallium arsenide are presented and experimental data are analyzed. A model for explaining recombination and trapping high purity gallium arsenide, valid below 77 K is assembled from points made at various places and an appraisal is given of photodielectric techniques for material property studies.

  18. Production of High-purity Radium-223 from Legacy Actinium-Beryllium Neutron Sources

    SciTech Connect

    Z. Soderquist, Chuck; K. McNamara, Bruce; R. Fisher, Darrell

    2012-06-01

    Radium-223 is a short-lived alpha-particle-emitting radionuclides with potential applications in cancer treatment. Research to develop new radiopharmaceuticals employing 223Ra has been hindered by poor availability due to the small quantities of parent actinium-227 available world-wide. The purpose of this study was to develop innovative and cost-effective methods to obtain high-purity 223Ra from 227Ac. We obtained 227Ac from two surplus actinium-beryllium neutron generators. We retrieved the actinium/beryllium buttons from the sources and dissolved them in a sulfuric-nitric acid solution. A crude actinium solid was recovered from the solution by coprecipitation with thorium fluoride, leaving beryllium in solution. The crude actinium was purified to provide about 40 milligrams of actinium nitrate using anion exchange in methanol-water-nitric acid solution. The purified actinium was then used to generate high-purity 223Ra. We extracted 223Ra using anion exchange in a methanol-water-nitric acid solution. After the radium was separated, actinium and thorium were then eluted from the column and dried for interim storage. This single-pass separation produces high purity, carrier-free 223Ra product, and does not disturb the 227Ac/227Th equilibrium. A high purity, carrier-free 227Th was also obtained from the actinium using a similar anion exchange in nitric acid. These methods enable efficient production of 223Ra for research and new alpha-emitter radiopharmaceutical development.

  19. Structure and texture of electrolytic superconducting coatings of high-purity niobium

    NASA Astrophysics Data System (ADS)

    Kolosov, V. N.; Shevyrev, A. A.

    2014-08-01

    Modes of epitaxial growth of electrolytic superconducting coatings of high-purity niobium on substrates of niobium, molybdenum, and tungsten have been investigated. The dynamics of changes in the structure and texture of the coatings depending on the method of treatment of substrates, cathode current density, and thickness of the deposited niobium layer has been studied.

  20. Production of high-purity radium-223 from legacy actinium-beryllium neutron sources.

    PubMed

    Soderquist, Chuck Z; McNamara, Bruce K; Fisher, Darrell R

    2012-07-01

    Radium-223 is a short-lived alpha-particle-emitting radionuclide with potential applications in cancer treatment. Research to develop new radiopharmaceuticals employing (223)Ra has been hindered by poor availability due to the small quantities of parent actinium-227 available world-wide. The purpose of this study was to develop innovative and cost-effective methods to obtain high-purity (223)Ra from (227)Ac. We obtained (227)Ac from two surplus actinium-beryllium neutron generators. We retrieved the actinium/beryllium buttons from the sources and dissolved them in a sulfuric-nitric acid solution. A crude actinium solid was recovered from the solution by coprecipitation with thorium fluoride, leaving beryllium in solution. The crude actinium was purified to provide about 40 milligrams of actinium nitrate using anion exchange in methanol-water-nitric acid solution. The purified actinium was then used to generate high-purity (223)Ra. We extracted (223)Ra using anion exchange in a methanol-water-nitric acid solution. After the radium was separated, actinium and thorium were then eluted from the column and dried for interim storage. This single-pass separation produces high purity, carrier-free (223)Ra product, and does not disturb the (227)Ac/(227)Th equilibrium. A high purity, carrier-free (227)Th was also obtained from the actinium using a similar anion exchange in nitric acid. These methods enable efficient production of (223)Ra for research and new alpha-emitter radiopharmaceutical development. PMID:22697483

  1. Influence of citrate-nitrate reaction mixture packing on ceramic powder properties

    NASA Astrophysics Data System (ADS)

    Zupan, Klementina; Kolar, Drago; Marinšek, Marjan

    Lanthanum chromite-based materials have a good prospect for use in various high temperature applications, as well as an SOFC separator. A citrate-nitrate gel combustion reaction was used for the preparation of submicron crystalline strontium-substituted lanthanum chromite (LSC). The effect of the fuel-oxidant molar ratio and sample form prior to combustion was investigated in terms of reaction period, phase formation, particle size, morphology and agglomerate formation. Several characterization methods including scanning electron microscopy, mercury porosimetry, BET measurement, X-ray powder diffraction and thermal analysis were used to evaluate the influence of reaction mixture packing on powder characteristics for different citrate-nitrate (c/n) ratios. It was shown that the reaction period depends on the fuel/oxidant ratio and reaction mixture packing. The LSC powders prepared via the combustion route exhibited surface areas of about 12 m 2/g for the loose packed layer prepared samples and 7 to 11 m 2/g for samples prepared from a pellet. The nature of the agglomerates was studied from the pore size distribution in the green compacts pressed at different pressures. The sintering behaviour of powders and some of the electrical properties of sintered samples are reported. Sintering tests on LSC powders prepared via the combustion route showed that the sintering process started at about 900°C and proceeded in two steps in the presence of a liquid phase.

  2. ESEEM of industrial silica-bearing powders: reactivity of defects during wet processing in the ceramics production

    NASA Astrophysics Data System (ADS)

    Romanelli, Maurizio; Di Benedetto, Francesco; Fornaciai, Gabriele; Innocenti, Massimo; Montegrossi, Giordano; Pardi, Luca A.; Zoleo, Alfonso; Capacci, Fabio

    2015-05-01

    A study is undertaken to ascertain whether changes in the speciation of inorganic radicals are occurring during the ceramic industrial production that involves abundant silica powders as raw material. Industrial dusts were sampled in two ceramic firms, immediately after the wet mixing stage, performed with the aid of a relevant pressure. The dusts were then characterised by means of X-ray diffraction, analysis of the trace elements through chemical methods, granulometry, continuous-wave electron paramagnetic resonance (EPR) and pulsed electron spin echo envelope modulation (ESEEM) spectroscopies. The results of the characterisation point to a relevant change in the speciation of the two samples; namely, a prevailing contribution due to an inorganic radical different from that pertaining to pure quartz is pointed out. The combined interpretation of EPR and ESEEM data suggests the attribution of the main paramagnetic contribution to the A-centre in kaolinite, a constituent that is added to pure quartz at the initial stage of the ceramic production. In one of the two samples, a second weak EPR signal is attributed to the quartz's hAl species. By taking into account the relative quantities of quartz and kaolinite mixed in the two samples, and the relative abundances of the two radical species, we propose that the partial or complete suppression of the hAl species in favour of the A-centre of kaolinite has occurred. Although this change is apparently fostered by the mixture between quartz and another radical-bearing raw material, kaolinite, the suppression of the hAl centre of quartz is ascribed to the role played by the pressure and the wet environment during the industrial mixing procedure. This suppression provides a net change of radical speciation associated with quartz, when this phase is in contact with workers' respiratory system.

  3. Method of making metal oxide ceramic powders by using a combustible amino acid compound

    DOEpatents

    Pederson, L.R.; Chick, L.A.; Exarhos, G.J.

    1992-05-19

    This invention is directed to the formation of homogeneous, aqueous precursor mixtures of at least one substantially soluble metal salt and a substantially soluble, combustible co-reactant compound, typically an amino acid. This produces, upon evaporation, a substantially homogeneous intermediate material having a total solids level which would support combustion. The homogeneous intermediate material essentially comprises highly dispersed or solvated metal constituents and the co-reactant compound. The intermediate material is quite flammable. A metal oxide powder results on ignition of the intermediate product which combusts same to produce the product powder.

  4. Method of making metal oxide ceramic powders by using a combustible amino acid compound

    DOEpatents

    Pederson, Larry R.; Chick, Lawrence A.; Exarhos, Gregory J.

    1992-01-01

    This invention is directed to the formation of homogeneous, aqueous precursor mixtures of at least one substantially soluble metal salt and a substantially soluble, combustible co-reactant compound, typically an amino acid. This produces, upon evaporation, a substantially homogeneous intermediate material having a total solids level which would support combustion. The homogeneous intermediate material essentially comprises highly dispersed or solvated metal constituents and the co-reactant compound. The intermediate material is quite flammable. A metal oxide powder results on ignition of the intermediate product which combusts same to produce the product powder.

  5. Ceramics

    NASA Astrophysics Data System (ADS)

    Yao, Lichun; Yang, Jian; Qiu, Tai

    2014-09-01

    The effects of CuO addition on phase composition, microstructure, sintering behavior, and microwave dielectric properties of 0.80Sm(Mg0.5Ti0.5)O3-0.20 Ca0.8Sr0.2TiO3(8SMT-2CST) ceramics prepared by a conventional solid-state ceramic route have been studied. CuO addition shows no obvious influence on the phase of the 8SMT-2CST ceramics and all the samples exhibit pure perovskite structure. Appropriate CuO addition can effectively promote sintering and grain growth, and consequently improve the dielectric properties of the ceramics. The sintering temperature of the ceramics decreases by 50°C by adding 1.00 wt.%CuO. Superior microwave dielectric properties with a ɛ r of 29.8, Q × f of 85,500 GHz, and τ f of 2.4 ppm/°C are obtained for 1.00 wt.%CuO doped 8SMT-2CST ceramics sintered at 1500°C, which shows dense and uniform microstructure as well as well-developed grain growth.

  6. Laser hearth melt processing of ceramic materials

    NASA Astrophysics Data System (ADS)

    Richard Weber, J. K.; Felten, J. J.; Nordine, Paul C.

    1996-02-01

    A new technique for synthesizing small batches of oxide-based ceramic and glass materials from high purity powders is described. The method uses continuous wave CO2 laser beam heating of material held on a water-cooled copper hearth. Contamination which would normally result during crucible melting is eliminated. Details of the technique are presented, and its operation and use are illustrated by results obtained in melting experiments with a-aluminum oxide, Y-Ba-Cu-O superconductor material, and the mixtures, Al2O3-SiO2, Bi2O3-B2O3, Bi2O3-CuO. Specimen masses were 0.05-1.5 g.

  7. Dielectric Performance of High Purity HTCC Alumina at High Temperatures - A Comparison Study with Other Polycrystalline Alumina

    NASA Technical Reports Server (NTRS)

    Chen, Liang-Yu

    2012-01-01

    A very high purity (99.99+) high temperature co-fired ceramic (HTCC) alumina has recently become commercially available. The raw material of this HTCC alumina is very different from conventional HTCC alumina, and more importantly there is no glass additive in this co-fired material. Previously, selected HTCC and LTCC (low temperature co-fired ceramic) alumina materials were evaluated at high temperatures as dielectric and compared to a regularly sintered 96 polycrystalline alumina (96 Al2O3), where 96 alumina was used as the benchmark. A prototype packaging system based on regular 96 alumina with Au thick-film metallization successfully facilitated long term testing of high temperature silicon carbide (SiC) electronic devices for over 10,000 hours at 500C. In order to evaluate this new HTCC alumina for possible high temperature packaging applications, the dielectric properties of this HTCC alumina substrate were measured and compared with those of 96 alumina and a LTCC alumina from room temperature to 550C at frequencies of 120 Hz, 1 KHz, 10 KHz, 100 KHz, and 1 MHz. A parallel-plate capacitive device with dielectric of the HTCC alumina and precious metal electrodes were used for measurements of the dielectric constant and dielectric loss of the co-fired alumina material in the temperature and frequency ranges. The capacitance and AC parallel conductance of the capacitive device were directly measured by an AC impedance meter, and the dielectric constant and parallel AC conductivity of the dielectric were calculated from the capacitance and conductance measurement results. The temperature and frequency dependent dielectric constant, AC conductivity, and dissipation factor of the HTCC alumina substrate are presented and compared to those of 96 alumina. Other technical advantages of this new co-fired material for possible high packaging applications are also discussed.

  8. Comparison of Deformation in High-Purity Single/Large Grain and Polycrystalline Niobium Superconducting Cavities

    SciTech Connect

    Ganapati Rao Myneni; Peter Kneisel

    2005-07-10

    The current approach for the fabrication of superconducting radio frequency (SRF) cavities is to roll and deep draw sheets of polycrystalline high-purity niobium. Recently, a new technique was developed at Jefferson Laboratory that enables the fabrication of single-crystal high-purity Nb SRF cavities. To better understand the differences between SRF cavities fabricated out of fine-grained polycrystalline sheet in the standard manner and single crystal cavities fabricated by the new technique, two half-cells were produced according to the two different procedures and compared using a variety of analytical techniques including optical microscopy, scanning laser confocal microscopy, profilometry, and X-ray diffraction. Crystallographic orientations, texture, and residual stresses were determined in the samples before and after forming and this poster presents the results of this ongoing study.

  9. An improved procedure for high purity gaseous peroxyacyl nitrate production: Use of heavy lipid solvents

    NASA Astrophysics Data System (ADS)

    Gaffney, J. S.; Fajer, R.; Senum, G. I.

    An improved procedure is described for the production of peroxyacyl nitrates (PAN's) in the gas phase. The method of Nielsen et al. (1982) has been modified to yield PAN's of high purity with no further Chromatographic purification required. Extraction of PAN's from the nitration of the peracids is accomplished by use of a heavy lipid solvent ( n-tridecane). This solvent's low vapor pressure allows the simple separation and preparation of high purity gaseous PAN's (> 98 %) as determined by Fourier transform infrared spectroscopy (FTIR). Using this method infrared integrated band strengths are reported for peroxyacetyl nitrate (PAN) perdeutero-peroxyacetyl nitrate (PAN-D 3) and peroxyproprionyl nitrate (PPN). The method allows facile production of large amounts of gaseous PAN's for smog chamber and laboratory studies, lexicological and health effects research, as well as for calibration of PAN analyses.

  10. Crystal growth and detector performance of large size high-purity Ge crystals

    NASA Astrophysics Data System (ADS)

    Wang, Guojian; Amman, Mark; Mei, Hao; Mei, Dongming; Irmscher, Klaus; Guan, Yutong; Yang, Gang

    2015-03-01

    High-purity germanium crystals with 12 cm in diameter were grown in a hydrogen atmosphere using the Czochralski method. The dislocation density of the crystals was determined to be in the range of 2000 - 4200 cm-2, which meets a requirement for use as a radiation detector. The axial and radial distributions of impurities in the crystals were measured by Hall effect and Photo-thermal ionization spectroscopy (PTIS). Two detectors were also fabricated from one of the crystals with different techniques and then evaluated for electrical and spectral performance. Measurements of gamma-ray spectra from 137Cs, 241Am and 60Co sources demonstrate that the detectors have excellent energy resolution. Keywords: High-purity germanium crystal, Czochralski method This work is supported by DOE grant DE-FG02-10ER46709 and the state of South Dakota.

  11. Characterization of a high-purity germanium detector for small-animal SPECT

    PubMed Central

    Johnson, Lindsay C; Campbell, Desmond L; Hull, Ethan L; Peterson, Todd E

    2011-01-01

    We present an initial evaluation of a mechanically-cooled, high-purity germanium double-sided strip detector as a potential gamma camera for small-animal SPECT. It is 90 mm in diameter and 10 mm thick with two sets of 16 orthogonal strips that have a 4.5 mm width with a 5 mm pitch. We found an energy resolution of 0.96% at 140 keV, an intrinsic efficiency of 43.3% at 122 keV and a FWHM spatial resolution of approximately 1.5 mm. We demonstrated depth-of-interaction estimation capability through comparison of pinhole acquisitions with a point source on and off axis. Finally, a flood-corrected-flood image exhibited a strip-level uniformity of less than 1%. This high-purity germanium offers many desirable properties for small-animal SPECT. PMID:21852723

  12. Fabrication of novel cryomill for synthesis of high purity metallic nanoparticles

    NASA Astrophysics Data System (ADS)

    Kumar, Nirmal; Biswas, Krishanu

    2015-08-01

    The successful preparation of free standing metal nanoparticles with high purity in bulk quantity is the pre-requisite for any potential application. This is possible by using ball milling at cryogenic temperature. However, the most of ball mills available in the market do not allow preparing high purity metal nanoparticles by this route. In addition, it is not possible to carry out in situ measurements of process parameters as well as diagnostic of the process. In the present investigation, we present a detailed study on the fabrication of a cryomill, which is capable of avoiding contaminations in the product. It also provides in situ measurements and diagnostic of the low temperature milling process. Online monitoring of the milling temperature and observation of ball motion are the important aspects in the newly designed mill. The nanoparticles prepared using this fabricated mill have been found to be free standing and also free from contaminations.

  13. Aluminium. II - A review of deformation properties of high purity aluminium and dilute aluminium alloys.

    NASA Technical Reports Server (NTRS)

    Reed, R. P.

    1972-01-01

    The elastic and plastic deformation behavior of high-purity aluminum and of dilute aluminum alloys is reviewed. Reliable property data, including elastic moduli, elastic coefficients, tensile, creep, fatigue, hardness, and impact are presented. Single crystal tensile results are discussed. Rather comprehensive reference lists, containing publications of the past 20 years, are included for each of the above categories. Defect structures and mechanisms responsible for mechanical behavior are presented. Strengthening techniques (alloys, cold work, irradiation, quenching, composites) and recovery are briefly reviewed.

  14. High purity liquid phase epitaxial GaAs for radiation detectors

    SciTech Connect

    Wynne, D.I.; Haller, E.E.; Rossington Tull, C.S.

    1998-12-31

    The authors report on the growth of high purity n-GaAs using Liquid Phase Epitaxy (LPE) and the fabrication of room temperature p-i-n radiation detectors. The epilayers are grown from a Ga solvent in a graphite boat in a pure hydrogen atmosphere. Growth is started at a temperature of approximately 800 C. The best epilayers show a net-residual-donor concentration of 2 {times} 10{sup 13} cm{sup {minus}3}, confirmed by Hall effect measurements. The residual donors have been analyzed by far infrared spectroscopy and found to be sulfur and silicon. Epilayers with thicknesses of up to 120 {micro}m have been deposited on 650 {micro}m thick semi-insulating GaAs substrates and on 500 {micro}m thick n{sup +}-type GaAs substrates. The authors report the results obtained with Schottky barrier diodes fabricated from these high purity n-type GaAs epilayers and operated as X-ray detectors. The Schottky barrier contacts consisted of evaporated circular gold contacts on epilayers on n{sup +} substrates. The ohmic contacts were formed by evaporated and alloyed Ni-Ge-Au films on the back of the substrate. Several of the diodes exhibit currents of the order of 1 to 10 nA at reverse biases depleting approximately 50 {micro}m of the epilayer. This very encouraging result, demonstrating the possibility for fabricating GaAs p-i-n diodes with depletion layers in high purity GaAs instead of semi-insulating GaAs, is supported by similar results obtained by several other groups. The consequences of using high purity instead of semi-insulating GaAs will be much reduced charge carrier trapping. Diode electrical characteristics and detector performance results using {sup 55}Fe and {sup 241}Am radiation will be discussed.

  15. Integration of High-Purity Carbon Nanotube Solution into Electronic Devices

    NASA Astrophysics Data System (ADS)

    Tulevski, George; IBM TJ Watson Reserach Center Team

    Due to their exceptional electronic properties, carbon nanotubes (cnt) are leading candidates to be employed as channel materials in future nanoelectronic devices. A key bottleneck to realizing device integration is the sorting of carbon nanotubes, namely the isolation of high-purity, semiconducting cnt solutions. This talk will describe our efforts in using polymer-based sorting methods to isolate high-density and high-purity semiconducting cnt solutions. We explore the dependence of starting material and polymer to cnt ratio on the effectiveness of the separation. We confirm optically and electrically that the semiconducting purity is >99.99% through several thousand individual device measurements. In addition to single-cnt devices, thin-film transistors were also fabricated and tested. Due to the high purity of the solutions, device switching (~105 ION/IOFF) was observed at channel lengths below the percolation threshold (<500 nm). Operating below the percolation threshold allows for devices with much higher current densities and effective mobilities as transport is now the result of direct transport as opposed to hopping between cnts.

  16. Synthesis and Characterization of High-Purity Tellurium Nanowires via Self-seed-Assisted Growth Approach

    NASA Astrophysics Data System (ADS)

    Li, Ying; Zhao, Wen-yu; Mu, Xin; Liu, Xing; He, Dan-qi; Zhu, Wan-ting; Zhang, Qing-jie

    2016-03-01

    Nanowires have attracted intense attention in recent years due to their novel physical properties. In this work, we prepare high-purity tellurium nanowires through the self-seed-assisted growth method previously developed by us. The tellurium seeds were firstly synthesized by reducing Na2TeO3 in the ice water with NaBH4. The high-purity tellurium nanowires with a diameter of 40-50 nm and a length of several tens of micrometers were then grown on tellurium seeds by reducing Na2TeO3 with hydrazine hydrate. X-ray diffraction, scanning electron microscopy and transmission electron microscopy were employed to characterize the crystal structure, microstructure, and growth direction of tellurium seeds and nanowires. The effects of temperature, time, surfactant and tellurium seeds on microstructures of tellurium nanowires has also been investigated. The synthesis conditions of tellurium seeds and nanowires was optimized. The selected area electron diffraction pattern confirms that the growth direction of tellurium nanowires is parallel to [0001] direction. It was discovered that high-purity tellurium nanowires with high aspect ratio can be synthesized by precisely controlling the temperature to adjust the nucleation rate of the tellurium nuclei, selecting the appropriate surfactant to induce the coordination along the macromolecular chain, and using tellurium seeds as the templates of the epitaxial growth of tellurium nuclei.

  17. Synthesis and Characterization of High-Purity Bismuth Nanowires via Seed-Assisted Growth Approach

    NASA Astrophysics Data System (ADS)

    Mu, Xin; Zhao, Wen-Yu; He, Dan-Qi; Zhou, Hong-Yu; Zhu, Wan-Ting; Zhang, Qing-Jie

    2015-06-01

    Nanowires are considered as high-performance thermoelectric materials with large Seebeck coefficients due to quantum confinement and low thermal conductivity because of enhanced boundary scattering of phonons. In this work, a seed-assisted growth method has been developed to synthesize high-purity bismuth nanowires. The bismuth seeds were first synthesized by reducing BiCl3 in the ice water with NaBH4. The high-purity bismuth nanowires about 40-50 nm in diameter and several tens of micrometers in length were then grown on bismuth seeds by reducing NaBiO3 with ethylene glycol. X-ray diffraction, scanning electron microscopy, and transmission electron microscopy were employed to characterize the crystal structure, microstructure, and growth direction of the bismuth seeds and nanowires. The effects of temperature, reductant, and bismuth seeds template on the microstructures of the bismuth nanowires were also investigated. The synthesis conditions of bismuth seeds and nanowires were optimized. The selected area electron diffraction pattern confirms that the growth direction of bismuth nanowires is parallel to [] direction. It was discovered that high-purity bismuth nanowires with high aspect ratio can be synthesized by precisely controlling the temperature to adjust the nucleation rate of the bismuth nuclei, selecting the appropriate reductant to maintain a low nucleation rate, and using bismuth seeds as the template of the epitaxial growth of the bismuth nuclei.

  18. Dense and Homogeneous Compaction of Fine Ceramic and Metallic Powders: High-Speed Centrifugal Compaction Process

    NASA Astrophysics Data System (ADS)

    Suzuki, Hiroyuki Y.

    2008-02-01

    High-Speed Centrifugal Compaction Process (HCP) is a variation of colloidal compacting method, in which the powders sediment under huge centrifugal force. Compacting mechanism of HCP differs from conventional colloidal process such as slip casting. The unique compacting mechanism of HCP leads to a number of characteristics such as a higher compacting speed, wide applicability for net shape formation, flawless microstructure of the green compacts, etc. However, HCP also has several deteriorative characteristics that must be overcome to fully realize this process' full potential.

  19. Dense and Homogeneous Compaction of Fine Ceramic and Metallic Powders: High-Speed Centrifugal Compaction Process

    SciTech Connect

    Suzuki, Hiroyuki Y.

    2008-02-15

    High-Speed Centrifugal Compaction Process (HCP) is a variation of colloidal compacting method, in which the powders sediment under huge centrifugal force. Compacting mechanism of HCP differs from conventional colloidal process such as slip casting. The unique compacting mechanism of HCP leads to a number of characteristics such as a higher compacting speed, wide applicability for net shape formation, flawless microstructure of the green compacts, etc. However, HCP also has several deteriorative characteristics that must be overcome to fully realize this process' full potential.

  20. Cobalt(I) Olefin Complexes: Precursors for Metal-Organic Chemical Vapor Deposition of High Purity Cobalt Metal Thin Films.

    PubMed

    Hamilton, Jeff A; Pugh, Thomas; Johnson, Andrew L; Kingsley, Andrew J; Richards, Stephen P

    2016-07-18

    We report the synthesis and characterization of a family of organometallic cobalt(I) metal precursors based around cyclopentadienyl and diene ligands. The molecular structures of the complexes cyclopentadienyl-cobalt(I) diolefin complexes are described, as determined by single-crystal X-ray diffraction analysis. Thermogravimetric analysis and thermal stability studies of the complexes highlighted the isoprene, dimethyl butadiene, and cyclohexadiene derivatives [(C5H5)Co(η(4)-CH2CHC(Me)CH2)] (1), [(C5H5)Co(η(4)-CH2C(Me)C(Me)CH2)] (2), and [(C5H5)Co(η(4)-C6H8)] (4) as possible cobalt metal organic chemical vapor deposition (MOCVD) precursors. Atmospheric pressure MOCVD was employed using precursor 1, to synthesize thin films of metallic cobalt on silicon substrates under an atmosphere (760 torr) of hydrogen (H2). Analysis of the thin films deposited at substrate temperatures of 325, 350, 375, and 400 °C, respectively, by scanning electron microscopy and atomic force microscopy reveal temperature-dependent growth features. Films grown at these temperatures are continuous, pinhole-free, and can be seen to be composed of hexagonal particles clearly visible in the electron micrograph. Powder X-ray diffraction and X-ray photoelectron spectroscopy all show the films to be highly crystalline, high-purity metallic cobalt. Raman spectroscopy was unable to detect the presence of cobalt silicides at the substrate/thin film interface. PMID:27348614

  1. Purity analyses of high-purity organic compounds with nitroxyl radicals based on the Curie–Weiss law

    SciTech Connect

    Matsumoto, Nobuhiro Shimosaka, Takuya

    2015-05-07

    This work reports an attempt to quantify the purities of powders of high-purity organic compounds with stable nitroxyl radicals (namely, 2,2,6,6-tetramethylpiperidine 1-oxyl (TEMPO), 1-oxyl-2,2,6,6-tetramethyl-4-hydroxypiperidine (TEMPOL), and 4-hydroxy-2,2,6,6-tetramethylpiperidine 1-oxyl benzoate (4-hydroxy-TEMPO benzoate)) in terms of mass fractions by using our “effective magnetic moment method,” which is based on both the Curie–Weiss law and a fundamental equation of electron paramagnetic resonance (ESR). The temperature dependence of the magnetic moment resulting from the radicals was measured with a superconducting quantum interference device magnetometer. The g value for each compound was measured with an X-band ESR spectrometer. The results of the purities were (0.998 ± 0.064) kg kg{sup −1} for TEMPO, (1.019 ± 0.040) kg kg{sup −1} for TEMPOL, and (1.001 ± 0.048) kg kg{sup −1} for 4-hydroxy-TEMPO benzoate. These results demonstrate that this analytical method as a future candidate of potential primary direct method can measure the purities with expanded uncertainties of approximately 5%.

  2. Investigations of Ba{sub x}Sr{sub 1−x}TiO{sub 3} ceramics and powders prepared by direct current arc discharge technique

    SciTech Connect

    Li, Shuangbin; Wang, Xiaohan; Yao, Ying Jia, Yongzhong; Xie, Shaolei; Jing, Yan; Yuzyuk, Yu. I.

    2014-09-01

    Ba{sub x}Sr{sub 1−x}TiO{sub 3} ceramics with x ranging from 0 to 1 were prepared by direct current arc discharge technique and studied by means of x-ray diffraction (XRD) and Raman spectroscopy. The cubic-tetragonal ferroelectric phase transition in Ba{sub x}Sr{sub 1−x}TiO{sub 3} ceramics was found to occur at x ≈ 0.75. XRD investigation of as-grown BaTiO{sub 3} ceramics revealed co-existence of tetragonal and hexagonal modifications with a small amount of impurity phase BaTi{sub 4}O{sub 9}. No evidences of hexagonal phase were observed in Raman spectra of as-grown BaTiO{sub 3} ceramics, while Raman peaks related to hexagonal phase were clearly observed in the spectrum of fine-grain powders prepared from the same ceramics. A core-shell model for BaTiO{sub 3} ceramics prepared by direct current arc discharge technique is proposed. Absence of the hexagonal phase in any Ba{sub x}Sr{sub 1−x}TiO{sub 3} solid solution with x < 1 is discussed in the frame of specific atomic arrangement.

  3. The crystallization of the nanometersized amorphous ceramic powders by ball milling

    SciTech Connect

    Fan, G.J.; Song, X.P.; Li, Y.L.

    1995-12-31

    The nanometersized amorphous Si{sub 3}N{sub 4} and Si-N-C powders are subjected by high-energy ball milling in order to induce a crystallization process. It was found that after initial 4 seconds of milling a-Si{sub 3}N{sub 4} may rapidly crystallize into a mixture of {alpha}-Si{sub 3}N{sub 4} and {beta}-Si{sub 3}N{sub 4} whereas amorphous Si-N-C powders remain in the amorphous state. These results cannot be interpreted with the local effective temperature rise at the collision sites and the increase of the impurity levels which drive the crystallization. The observed structural changes occurring in a-Si{sub 3}N{sub 4} can be attributed to the mechanical deformation which alters the bonding nature of a-Si{sub 3}N{sub 4}. It was concluded that ball milling is an effective tool to induce the crystallization of some amorphous metallic systems.

  4. Interdisciplinary research on the nature and properties of ceramic materials

    NASA Technical Reports Server (NTRS)

    1980-01-01

    Several investigations concerning the properties and processing of brittle ceramic materials as related to design considerations are briefly described. Surface characterization techniques, fractography, high purity materials, creep properties, impact and thermal shock resistance, and reaction bonding are discussed.

  5. Ceramics

    NASA Astrophysics Data System (ADS)

    Bin, Tang; Feng, Si; Ying-xiang, Li; He-tuo, Chen; Xiao, Zhang; Shu-ren, Zhang

    2014-11-01

    The effects of Ta2O5/Y2O3 codoping on the microstructure and microwave dielectric properties of Ba(Co0.56Zn0.40)1/3Nb2/3O3- xA- xB (A = 0.045 wt.% Ta2O5; B = 0.113 wt.% Y2O3) ceramics ( x = 0, 1, 2, 4, 8, 16, 32) prepared according to the conventional solid-state reaction technique were investigated. The x-ray diffraction (XRD) results showed that the main crystal phase in the sintered ceramics was BaZn0.33Nb0.67O3-Ba3CoNb2O9. The additional surface phase of Ba8CoNb6O24 and trace amounts of Ba5Nb4O15 second phase were present when Ta2O5/Y2O3 was added to the ceramics. The 1:2 B-site cation ordering was affected by the substitution of Ta5+ and Y3+ in the crystal lattice, especially for x = 4. Scanning electron microscopy (SEM) images of the optimally doped ceramics sintered at 1340°C for 20 h showed a compact microstructure with crystal grains in dense contact. Though the dielectric constant increased with the x value, appropriate addition would result in a tremendous modification of the Q × f and τ f values. Excellent microwave dielectric properties ( ɛ r = 35.4, Q × f = 62,993 GHz, and τ f = 2.6 ppm/°C) were obtained for the ceramic with x = 0.4 sintered in air at 1340°C for 20 h.

  6. Selection of different sintering aids and heat-treatment of Y2O3 raw powders for Yb3+:Y3Al5O12 transparent ceramics

    NASA Astrophysics Data System (ADS)

    Chen, Chong; Zhou, Shengming; Lin, Hui; Yi, Qing

    2011-11-01

    La2O3, Y2O3, ZrO2, and MgO+TEOS were added as the sintering aid to prepare Yb3+:Y3Al5O12 transparent ceramics. Pre-calcination was adopted to improve the crystalline quality and morphology of the commercially available Y2O3 raw powders. The non-stoichiometricaly doped La2O3, Y2O3, and ZrO2 enhanced the grain boundary mobility so fast that abnormal grain growth occurred and pores tended to be enclosed in these grains. It was found that MgO+TEOS had a positive effect on full densification of the Yb:YAG ceramics. The grain boundaries moved moderately so that pores could be eliminated well and meanwhile the grains would not get too large. Laser output experiment was also carried out for the Yb:YAG transparent ceramics.

  7. Selection of different sintering aids and heat-treatment of Y2O3 raw powders for Yb3+:Y3Al5O12 transparent ceramics

    NASA Astrophysics Data System (ADS)

    Chen, Chong; Zhou, Shengming; Lin, Hui; Yi, Qing

    2012-01-01

    La2O3, Y2O3, ZrO2, and MgO+TEOS were added as the sintering aid to prepare Yb3+:Y3Al5O12 transparent ceramics. Pre-calcination was adopted to improve the crystalline quality and morphology of the commercially available Y2O3 raw powders. The non-stoichiometricaly doped La2O3, Y2O3, and ZrO2 enhanced the grain boundary mobility so fast that abnormal grain growth occurred and pores tended to be enclosed in these grains. It was found that MgO+TEOS had a positive effect on full densification of the Yb:YAG ceramics. The grain boundaries moved moderately so that pores could be eliminated well and meanwhile the grains would not get too large. Laser output experiment was also carried out for the Yb:YAG transparent ceramics.

  8. Ceramics

    NASA Astrophysics Data System (ADS)

    Li, Enzhu; Zou, Mengying; Duan, Shuxin; Xu, Ning; Yuan, Ying; Zhou, Xiaohua

    2014-11-01

    The effects of excess Li content on the phase structure and microwave dielectric properties, especially on the temperature coefficient, of LiNb0.6 Ti0.5O3 (LNT) ceramics were studied. The results show that small amounts of Li effectively enhanced the sintering process due to the compensation of high volatility of Li, leading to a densification and homogenous microstructure, and therefore enhanced the dielectric properties. However, too much Li leads to a secondary phase and cause abnormal grain growth. The LNT + 5 wt.% Li ceramic sintered at 1075°C in the air shows the best properties of ɛ r = 69.73, Q × f = 5543 GHz, and τ f = -4.4 ppm/°C.

  9. Silicon nitride/silicon carbide composite powders

    DOEpatents

    Dunmead, Stephen D.; Weimer, Alan W.; Carroll, Daniel F.; Eisman, Glenn A.; Cochran, Gene A.; Susnitzky, David W.; Beaman, Donald R.; Nilsen, Kevin J.

    1996-06-11

    Prepare silicon nitride-silicon carbide composite powders by carbothermal reduction of crystalline silica powder, carbon powder and, optionally, crystalline silicon nitride powder. The crystalline silicon carbide portion of the composite powders has a mean number diameter less than about 700 nanometers and contains nitrogen. The composite powders may be used to prepare sintered ceramic bodies and self-reinforced silicon nitride ceramic bodies.

  10. Characterization of high-purity arsine and gallium arsenide epilayers grown by MOCVD

    NASA Astrophysics Data System (ADS)

    Feng, Jun; Clement, Ryan; Raynor, Mark

    2008-11-01

    Impurities present in the metal organic chemical vapor deposition (MOCVD) process gases and precursors can have a significant effect on the performance of III-V compound semiconductor devices. High-purity arsine purified using chemical, adsorption and distillation techniques, has been characterized for impurities by using high sensitivity gas analysis methods and low temperature photoluminescence (PL) of GaAs epilayers. Permanent gas, hydrocarbon and dopant impurities can all be removed using these purification methods to below the detection limit of instrumentation (low nmol mol -1-pmol mol -1, depending on method). Capability to remove water vapor to single digit nmol mol -1 levels is also demonstrated and cylinder depletion studies show that gas-phase arsine, with consistently low H 2O, can be delivered from the cylinder, even well after phase break. Low temperature PL measurements are made on 10 μm GaAs/GaAs grown with three different arsine sources. Well-resolved near-band emission characteristics of high-purity n-type GaAs is obtained with high-purity distilled arsine. PL of epilayers grown with less pure arsine show the presence of Ge as well as elevated levels of Mg and Zn, incorporated from the trimethylgallium. The incorporation of O from an arsine cylinder containing H 2O at 200 nmol mol -1 results in reduced full width at half maximum (FWHM) of the near-band emission and decreased ( D0, X) and ( F, X) intensity, highlighting the importance of minimizing H 2O impurity.

  11. High Purity Americium-241 for Fuel Cycle R&D Program

    SciTech Connect

    Dr. Paul A. Lessing

    2011-07-01

    Previously the U.S. Department of Energy released Am-241 for various applications such as smoke detectors and Am-Be neutron sources for oil wells. At this date there is a shortage of usable, higher purity Am-241 in metal and oxide form available in the United States. Recently, the limited source of Am-241 has been from Russia with production being contracted to existing customers. The shortage has resulted in the price per gram rising dramatically over the last few years. DOE-NE currently has need for high purity Am-241 metal and oxide to fabricate fuel pellets for reactor testing in the Fuel Cycle R&D program. All the available high purity americium has been gathered from within the DOE system of laboratories. However, this is only a fraction of the projected needs of FCRD over the next 10 years. Therefore, FCR&D has proposed extraction and purification concepts to extract Am-241 from a mixed AmO2-PuO2 feedstock stored at the Savannah River Site. The most simple extraction system is based upon high temperature reduction using lanthanum metal with concurrent evaporation and condensation to produce high purity Am metal. Metallic americium has over a four order of magnitude higher vapor pressure than plutonium. Results from small-scale reduction experiments are presented. These results confirm thermodynamic predictions that at 1000 deg C metallic lanthanum reduces both PuO2 and AmO2. Faster kinetics are expected for temperatures up to about 1500 deg C.

  12. Effects of annealing on texture evolution of cross shear rolled high-purity Al foils

    NASA Astrophysics Data System (ADS)

    Wang, L.; Liu, Y.; Song, X.; He, J.; Zuo, L.

    2015-04-01

    The effects of annealing on recrystallization texture of cross shear rolled high-purity Al foil were investigated by orientation distribution functions (ODFs) and electron backscattered diffraction (EBSD). The results show that the intermediate annealing is beneficial to the development of the cube texture. The cube texture can be promoted by annealing, and the critical annealing temperature is about 280 °C. The cubic orientation grains firstly nucleate, and then expand into other grains with a high growth speed, and large angle grain boundary ratio increases, finally can swallow up most of the original grains, which results in the cube texture

  13. Formation and evolution of tweed structures on high-purity aluminum polycrystalline foils under cyclic tension

    SciTech Connect

    Kuznetsov, P. V.; Vlasov, I. V.; Sklyarova, E. A.; Smekalina, T. V.

    2015-10-27

    Peculiarities of formation and evolution of tweed structures on the surface of high-purity aluminum polycrystalline foils under cyclic tension were studied using an atom force microscope and a white light interferometer. Tweed structures of micron and submicron sizes were found on the foils at different number of cycles. In the range of 42,000 < N < 95,000 cycles destruction of tweed patterns is observed, which leads to their disappearance from the surface of the foils. Formation of tweed structures of various scales is discussed in terms of the Grinfeld instability.

  14. Formation of High-Purity Indium Oxide Nanoparticles and Their Application to Sensitive Detection of Ammonia

    PubMed Central

    Bhardwaj, Sanjeev K.; Bhardwaj, Neha; Kukkar, Manil; Sharma, Amit L.; Kim, Ki-Hyun; Deep, Akash

    2015-01-01

    High-purity In2O3 nanoparticles were recovered from scrap indium tin oxide substrates in a stepwise process involving acidic leaching, liquid-liquid extraction with a phosphine oxide extractant, and combustion of the organic phase. The morphological and structural parameters of the recovered nanoparticles were investigated to support the formation of the desired products. These In2O3 nanoparticles were used for sensitive sensing of ammonia gas using a four-probe electrode device. The proposed sensor offered very quick response time (around 10 s) and highly sensitive detection of ammonia (at a detection limit of 1 ppm). PMID:26694415

  15. Corrosion behavior of surface films on boron-implanted high purity iron and stainless steels

    NASA Technical Reports Server (NTRS)

    Kim, H. J.; Carter, W. B.; Hochman, R. F.; Meletis, E. I.

    1985-01-01

    Boron (dose, 2 x 10 to the 17th ions/sq cm) was implanted into high purity iron, AISI 316 austenitic stainless steel, and AISI 440C martensitic stainless steel, at 40 keV. The film structure of implanted samples was examined and characterized by contrast and diffraction analyses utilizing transmission electron microscopy. The effect of B(+) ion implantation on the corrosion behavior was studied using the potentiodynamic polarization technique. Tests were performed in deaerated 1 N H2SO4 and 0.1 M NaCl solutions. Scanning electron microscopy was used to examine the morphology of the corroded surfaces after testing.

  16. Method for growing low defect, high purity crystalline layers utilizing lateral overgrowth of a patterned mask

    NASA Technical Reports Server (NTRS)

    Morrison, Andrew D. (Inventor); Daud, Taher (Inventor)

    1986-01-01

    A method for growing a high purity, low defect layer of semiconductor is described. This method involves depositing a patterned mask of a material impervious to impurities of the semiconductor on a surface of a blank. When a layer of semiconductor is grown on the mask, the semiconductor will first grow from the surface portions exposed by the openings in the mask and will bridge the connecting portions of the mask to form a continuous layer having improved purity, since only the portions overlying the openings are exposed to defects and impurities. The process can be iterated and the mask translated to further improve the quality of grown layers.

  17. High-purity separation of cancer cells by optically induced dielectrophoresis.

    PubMed

    Chen, Hsiu-Hsiang; Lin, Mai-Wei; Tien, Wan-Ting; Lai, Chin-Pen; Weng, Kuo-Yao; Ko, Ching-Huai; Lin, Chun-Chuan; Chen, Jyh-Chern; Tiao, Kuo-Tung; Chen, Tse-Ching; Chen, Shin-Cheh; Yeh, Ta-Sen; Cheng, Chieh-Fang

    2014-04-01

    Detecting and concentrating cancer cells in peripheral blood is of great importance for cancer diagnosis and prognosis. Optically induced dielectrophoresis (ODEP) can achieve high resolution and low optical intensities, and the electrode pattern can be dynamically changed by varied light patterns. By changing the projected light pattern, it is demonstrated to separate high-purity gastric cancer cell lines. Traditionally, the purity of cancer cell isolation by negative selection is 0.9% to 10%; by positive selection it is 50% to 62%. An ODEP technology is proposed to enhance the purity of cancer cell isolation to about 77%. PMID:24723112

  18. Enhanced microwave dielectric properties of Ba{sub 0.4}Sr{sub 0.6}TiO{sub 3} ceramics doping by metal Fe powders

    SciTech Connect

    Zhang Qiwei; Zhai Jiwei; Yao Xi; Ben Qianqian; Yu Xian

    2012-11-15

    Ba{sub 0.4}Sr{sub 0.6}TiO{sub 3} ceramics by adding mental Fe powders have been fabricated via the solid-state reaction method. The microstructures and optical properties of samples are systematically studied in order to establish the effects of Fe powder additives on microwave dielectric properties of Ba{sub 0.4}Sr{sub 0.6}TiO{sub 3} ceramics by x-ray diffraction, x-ray photoelectron spectroscopy, and optical reflective spectrum. The results show the coexistence of Fe{sup 2+} and Fe{sup 3+} in Ba{sub 0.4}Sr{sub 0.6}TiO{sub 3} ceramics, the decrease of O vacancy concentrations, and their incorporation into the B-site (Ti) of the Ba{sub 0.4}Sr{sub 0.6}TiO{sub 3} host lattice give rise to excellent microwave dielectric properties. All samples have a higher Q value above 290 while maintaining relatively high tunability above 16.6%. In particular, the sample with the composition of x = 0.035 mol has the dielectric constant of 889, Q Multiplication-Sign f value of 826 (at 1.370 GHz), and tunability of 24%, which are very promising for high power tunable devices. In comparison, Fe{sub 2}O{sub 3} oxide doped Ba{sub 0.4}Sr{sub 0.6}TiO{sub 3} ceramics with the same molar ratios of Fe exhibit inferior microwave properties. It indicates that additives of the metal Fe powders can more effectively improve dielectric properties of Ba{sub x}Sr{sub 1-x}TiO{sub 3} system than Fe{sub 2}O{sub 3} oxide.

  19. In-line System to Produce High-Purity Acid Solutions.

    PubMed

    Masunaga, Hiroto; Higo, Yuji; Ishii, Mizuo; Maruyama, Noboru; Yamazaki, Shigeo

    2016-01-01

    Herein, we report a new device that generates a high-purity acid solution. It comprises three compartments divided by anion-exchange membranes and filled with ion-exchange resins. Fluorochemical cation-exchange membranes, which tolerate electrochemical wear and permit bulk flow, are inserted between each electrode and the anion-exchange resin. A bipolar boundary is a composite boundary comprising anion and cation exchangers. This device has four bipolar boundaries to separate the location of acid generation from the location where water is electrolyzed. It can tolerate high pressures, resist degradation due to electrolysis at the electrodes, and produce high-purity acid solutions that are free from gases and cationic impurities. The acid solution is generated on the basis of an electrokinetic phenomenon at the surfaces of ion-exchange resins and membranes in an electric field; its concentration can be controlled at rates from 0.01 to 100 μmol/min by adjusting the electrical current applied to the device. PMID:27302592

  20. The behavior of high-purity, low-density air plasma sprayed thermal barrier coatings

    SciTech Connect

    Helminiak, Yanar NM

    2009-12-01

    Research on the behavior of high-purity, low-density (85%) air plasma sprayed (APS) thermal barrier coatings (TBC) with NiCoCrAlY bond coats deposited by argon-shrouded plasma spraying is described. The microstructure of the APS topcoats is one variable in this study intended to maximize the coating thicknesses that can be applied without spallation and to minimize the thermal conduction through the YSZ layer. The specimens were evaluated using cyclic oxidation tests and important properties of the TBCs, such as resistance to sintering and phase transformation, were determined. The high purity resulted in top coats which are highly resistant to sintering and transformation from the metastable tetragonal phase to the equilibrium mixture of monoclinic and cubic phases. The porous topcoat microstructure also resulted in significant durability during thermal cycling. The actual failure mechanisms of the APS coatings were found to depend on topcoat thickness, CTE of the superalloy substrate and the nature of the thermal exposure.

  1. Recyclable Strategy for the Production of High-Purity Galacto-oligosaccharides by Kluyveromyces lactis.

    PubMed

    Sun, Huaisheng; You, Shengping; Wang, Mengfan; Qi, Wei; Su, Rongxin; He, Zhimin

    2016-07-20

    A recyclable strategy for the production of high-purity (>95%) galacto-oligosaccharides (GOS) was developed using Kluyveromyces lactis in both the synthesis and purification steps. For the synthesis of GOS, ethanol-permeabilized cells (p-cells) of K. lactis were used because the enhanced permeability facilitated the mass transfer of the substrate and the release of oligosaccharide products. For the purification of GOS, non-permeabilized K. lactis cells (np-cells) were preferred as a result of their intrinsic cell membrane barrier toward GOS, which led to the selective consumption of carbohydrate. In this way, undesired glucose, galactose, and lactose in the raw GOS solution can be completely removed. This strategy is recyclable not only because of the high stability and reusability of p-cells and np-cells but also because the ethanol, which is simultaneously generated during the purification, can be reused for the preparation of p-cells. The strategy proposed in this study is a promising candidate for the efficient production of high-purity GOS. PMID:27366924

  2. Secondary electron emission characteristics of ion-textured copper and high-purity isotropic graphite surfaces

    NASA Technical Reports Server (NTRS)

    Curren, A. N.; Jensen, K. A.

    1984-01-01

    Experimentally determined values of true secondary electron emission and relative values of reflected primary electron yield for untreated and ion textured oxygen free high conductivity copper and untreated and ion textured high purity isotropic graphite surfaces are presented for a range of primary electron beam energies and beam impingement angles. This investigation was conducted to provide information that would improve the efficiency of multistage depressed collectors (MDC's) for microwave amplifier traveling wave tubes in space communications and aircraft applications. For high efficiency, MDC electrode surfaces must have low secondary electron emission characteristics. Although copper is a commonly used material for MDC electrodes, it exhibits relatively high levels of secondary electron emission if its surface is not treated for emission control. Recent studies demonstrated that high purity isotropic graphite is a promising material for MDC electrodes, particularly with ion textured surfaces. The materials were tested at primary electron beam energies of 200 to 2000 eV and at direct (0 deg) to near grazing (85 deg) beam impingement angles. True secondary electron emission and relative reflected primary electron yield characteristics of the ion textured surfaces were compared with each other and with those of untreated surfaces of the same materials. Both the untreated and ion textured graphite surfaces and the ion treated copper surface exhibited sharply reduced secondary electron emission characteristics relative to those of untreated copper. The ion treated graphite surface yielded the lowest emission levels.

  3. Recycling of high purity selenium from CIGS solar cell waste materials.

    PubMed

    Gustafsson, Anna M K; Foreman, Mark R StJ; Ekberg, Christian

    2014-10-01

    Copper indium gallium diselenide (CIGS) is a promising material in thin film solar cell production. To make CIGS solar cells more competitive, both economically and environmentally, in comparison to other energy sources, methods for recycling are needed. In addition to the generally high price of the material, significant amounts of the metals are lost in the manufacturing process. The feasibility of recycling selenium from CIGS through oxidation at elevated temperatures was therefore examined. During oxidation gaseous selenium dioxide was formed and could be separated from the other elements, which remained in solid state. Upon cooling, the selenium dioxide sublimes and can be collected as crystals. After oxidation for 1h at 800°C all of the selenium was separated from the CIGS material. Two different reduction methods for reduction of the selenium dioxide to selenium were tested. In the first reduction method an organic molecule was used as the reducing agent in a Riley reaction. In the second reduction method sulphur dioxide gas was used. Both methods resulted in high purity selenium. This proves that the studied selenium separation method could be the first step in a recycling process aimed at the complete separation and recovery of high purity elements from CIGS. PMID:24472714

  4. Preparation and Evaluation of High-Purity La2O3

    NASA Astrophysics Data System (ADS)

    Lee, Gwang Seop; Uchikoshi, Masahito; Mimura, Kouji; Isshiki, Minoru

    2010-06-01

    A separation procedure based on extraction chromatography using the di(2-ethylhexyl) phosphoric acid (D2EHPA) impregnated resin, anion exchange with DIAION SA 10 resin, and oxalate precipitation has been developed for the preparation of high-purity La2O3 in hydrochloric acid media at a high La concentration. The metallic impurities Ce, Pr, Nd, Sm, K, Mg, Ca, Zn, Cu, Co, Mn, Pb, Al, In, and Fe, but not Bi, were removed efficiently from La by extraction chromatography using a D2EHPA impregnated resin. The Bi was separated from the La by anion exchange (DIAION SA 10) separation. Thus, a high-purity LaCl3 solution was obtained by anion exchange separation and extraction chromatography. La2O3 was prepared from the purified LaCl3 solution by oxalate precipitation. Glow discharge mass spectrometry was applied for purity evaluation of the prepared La2O3. The purity of the prepared La2O3 was more than 99.9998 pct total rare earth oxide.

  5. Process for producing high purity isoolefins and dimers thereof by dissociation of ethers

    DOEpatents

    Smith, Jr., Lawrence A.; Jones, Jr., Edward M.; Hearn, Dennis

    1984-01-01

    Alkyl tertiary butyl ether or alkyl tertiary amyl ether is dissociated by vapor phase contact with a cation acidic exchange resin at temperatures in the range of 150.degree. to 250.degree. F. at LHSV of 0.1 to 20 to produce a stream consisting of unreacted ether, isobutene or isoamylene and an alcohol corresponding to the alkyl radical. After the alcohol is removed, the ether/isoolefin stream may be fractionated to obtain a high purity isoolefin (99+%) or the ether/isoolefin stream can be contacted in liquid phase with a cation acidic exchange resin to selectively dimerize the isoolefin in a highly exothermic reaction, followed by fractionation of the dimerization product to produce high purity diisoolefin (97+%). In the case where the alkyl is C.sub.3 to C.sub.6 and the corresponding alcohol is produced on dissociation of the ether, combined dissociation-distillation may be carried out such that isoolefin is the overhead product and alcohol the bottom.

  6. Process for producing high purity isoolefins and dimers thereof by dissociation of ethers

    DOEpatents

    Smith, L.A. Jr.; Jones, E.M. Jr.; Hearn, D.

    1984-05-08

    Alkyl tertiary butyl ether or alkyl tertiary amyl ether is dissociated by vapor phase contact with a cation acidic exchange resin at temperatures in the range of 150 to 250 F at LHSV of 0.1 to 20 to produce a stream consisting of unreacted ether, isobutene or isoamylene and an alcohol corresponding to the alkyl radical. After the alcohol is removed, the ether/isoolefin stream may be fractionated to obtain a high purity isoolefin (99+%) or the ether/isoolefin stream can be contacted in liquid phase with a cation acidic exchange resin to selectively dimerize the isoolefin in a highly exothermic reaction, followed by fractionation of the dimerization product to produce high purity diisoolefin (97+%). In the case where the alkyl is C[sub 3] to C[sub 6] and the corresponding alcohol is produced on dissociation of the ether, combined dissociation-distillation may be carried out such that isoolefin is the overhead product and alcohol the bottom. 2 figs.

  7. Isolation of high-purity anthocyanin mixtures and monomers from blueberries using combined chromatographic techniques.

    PubMed

    Wang, Erlei; Yin, Yongguang; Xu, Caina; Liu, Jingbo

    2014-01-31

    Research on the isolation and preparation of anthocyanins has intensified in recent years because of the requirements of quantitative and bioactive analyses. However, simple and effective methods for the scale purification of pure anthocyanins from natural products are rarely reported. In this study, high-purity anthocyanin mixtures and monomers were successfully isolated from wild blueberries using a combination of column chromatography and semi-preparative HPLC. We established an effective elution system to separate high-purity anthocyanin mixtures with aqueous ethanol containing 0.01% HCl first in an Amberlite XAD-7HP column (ethanol/H2O=35:65) and then in a Sephadex LH-20 column (ethanol/H2O=25:75). Crude anthocyanin extracts were isolated using the Amberlite column, and a purity of 32% was obtained based on UV-vis analysis. Three fractions of anthocyanin mixtures were isolated from the crude extracts using the Sephadex column with purities ranging from 59% to 68%. Three pure monomeric anthocyanins of malvidin-3-O-glucoside, petunidin-3-O-glucoside, and delphinidin-3-O-glucoside were also isolated by semi-preparative HPLC and identified by HPLC-DAD-ESI-MS/MS. The purities of these anthocyanins were determined by analytical HPLC and estimated to be 97.7%, 99.3%, and 95.4%, respectively. The results of this study may help promote the purification of anthocyanins from most blueberry varieties as well as from other plant materials. PMID:24433700

  8. High-purity Cu nanocrystal synthesis by a dynamic decomposition method

    NASA Astrophysics Data System (ADS)

    Jian, Xian; Cao, Yu; Chen, Guozhang; Wang, Chao; Tang, Hui; Yin, Liangjun; Luan, Chunhong; Liang, Yinglin; Jiang, Jing; Wu, Sixin; Zeng, Qing; Wang, Fei; Zhang, Chengui

    2014-12-01

    Cu nanocrystals are applied extensively in several fields, particularly in the microelectron, sensor, and catalysis. The catalytic behavior of Cu nanocrystals depends mainly on the structure and particle size. In this work, formation of high-purity Cu nanocrystals is studied using a common chemical vapor deposition precursor of cupric tartrate. This process is investigated through a combined experimental and computational approach. The decomposition kinetics is researched via differential scanning calorimetry and thermogravimetric analysis using Flynn-Wall-Ozawa, Kissinger, and Starink methods. The growth was found to be influenced by the factors of reaction temperature, protective gas, and time. And microstructural and thermal characterizations were performed by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and differential scanning calorimetry. Decomposition of cupric tartrate at different temperatures was simulated by density functional theory calculations under the generalized gradient approximation. High crystalline Cu nanocrystals without floccules were obtained from thermal decomposition of cupric tartrate at 271°C for 8 h under Ar. This general approach paves a way to controllable synthesis of Cu nanocrystals with high purity.

  9. Investigation of active slip systems in high purity single crystal niobium

    NASA Astrophysics Data System (ADS)

    Baars, Derek

    The superconducting radio-frequency (SRF) community uses high purity niobium to manufacture SRF cavities for a variety of accelerator applications. Cavities are either made from large-grain sheets cut directly from the ingot and formed, or the ingot microstructure is broken down to form polycrystalline sheets or tubes. Reducing the number of costly electron beam welds to assemble the cavities is also desired. A greater understanding of the active slip systems and their relation to subsequent dislocation substructure would be of use in all these areas, to better understand how large grain niobium deforms and to develop more accurate computational models that will aid in the design and use of more cost-effective forming methods. Studies of slip in high-purity niobium suggest that temperature, material purity, and crystal orientation affect which slip systems are active during deformation, though have not examined the somewhat lesser purity niobium used for SRF cavities. As a step toward these goals, two sets of SRF-purity single crystal niobium samples were deformed to 40% strain in tension at room temperature. The first set was cut and welded back together. The second set consisted of deliberately orientated samples that resolved shear stress onto desired slip systems to evaluate different combinations of slip. Determining likely active slip systems was complex, though the evidence suggests that {112} slip may be dominant at yield at room temperature as suggested by theory, though {110} slip could not be ruled out.

  10. Device to generate high purity hydroxide solution in-line for ion chromatography.

    PubMed

    Masunaga, Hiroto; Higo, Yuji; Ishii, Mizuo; Maruyama, Noboru; Yamazaki, Shigeo

    2016-05-01

    Herein, we report a new device that generates a high-purity hydroxide solution in line. The device's container has three compartments that are isolated from each other by two cation exchange (CE) membranes. In each end of the container, an electrode is installed. The three compartments are filled with ion exchange resins. A bipolar boundary is a composite boundary comprising anion- and cation-exchangers. This device has two bipolar boundaries, which are used to separate the location of hydroxide solution generation from the location where water is electrolyzed. Therefore, it can produce high-purity hydroxide solutions that are free from gases and anionic impurities. The hydroxide solution is generated on the basis of an electrokinetic phenomenon at the surfaces of ion-exchange resins and membranes in an electric field; NaOH concentration can be controlled at rates from 0.01 to 100mM per 1mL/min by adjusting the electrical current (0-200mA) applied to the device. As the generated solution is used as an eluent for a suppressed anion chromatography, the electrical conductivity of the effluent from the suppressor is as low as that of ultra-pure water. Thus, the noise of the base-line electrical conductivity is improved, and so the detection limit of anions on the sub-ng/mL order can be achieved. PMID:27063368

  11. Tertiarybutylarsine for Metalorganic Chemical Vapor Deposition Growth of High Purity, High Uniformity Films

    NASA Astrophysics Data System (ADS)

    Chui, H. C.; Biefeld, R. M.; Hammons, B. E.; Breiland, W. G.; Brennan, T. M.; Jones, E. D.; Moffat, H. K.; Kim, M. H.; Grodzinski, P.; Chang, K. H.; Lee, H. C.

    1997-12-01

    We have performed an extensive study of GaAs, Al0.22Ga0.78As, and In0.16Ga0.84As grown using tertiarybutylarsine (TBA) in an ultra-high purity metalorganic chemical vapor deposition multi-wafer reactor. Key results include: high purity TBA AlGaAs layers with the lowest p-type carrier concentrations (4 × 1014 cm-3) reported to date; 4K photoluminescence bound exciton linewidths as narrow as 4.3 meV; C, O. Si, and S concentrations below the secondary ion mass spectrometry detection limit; and InGaAs/GaAs quantum wells with 20K PL linewidths as narrow as 3.5 meV. We also observe a strong dependence of growth rates and doping efficiency on group-V partial pressure, possibly due to a competition between excess group-V species and group-Ill or Si species for group-Ill surface sites. Finally, we demonstrate record uniformity using TBA with an AlGaAs thickness variation of only ±1.4% across a 4 inch wafer.

  12. New nano-sized Al2O3-BN coating 3Y-TZP ceramic composites for CAD/CAM-produced all-ceramic dental restorations. Part I. Fabrication of powders.

    PubMed

    Yang, Se Fei; Yang, Li Qiang; Jin, Zhi Hao; Guo, Tian Wen; Wang, Lei; Liu, Hong Chen

    2009-06-01

    Partially sintered 3 mol % yttria-stabilized tetragonal zirconium dioxide (ZrO(2), zirconia) polycrystal (3Y-TZP) ceramics are used in dental posterior restorations with computer-aided design-computer-aided manufacturing (CAD/CAM) techniques. High strength is acquired after sintering, but shape distortion of preshaped compacts during their sintering is inevitable. The aim of this study is to fabricate new machinable ceramic composites with strong mechanical properties that are fit for all-ceramic dental restorations. Aluminum oxide (Al(2)O(3))-coated 3Y-TZP powders were first prepared by the heterogeneous precipitation method starting with 3Y-TZP, Al(NO(3))(3) . 9H(2)O, and ammonia, then amorphous boron nitride (BN) was produced and the as-received composite powders were coated via in situ reaction with boric acid and urea. Transmission electron microscopy (TEM) and X-ray diffraction (XRD) were used to analyze the status of Al(2)O(3)-BN on the surface of the 3Y-TZP particles. TEM micrographs show an abundance of Al(2)O(3) particles and amorphous BN appearing uniformly on the surface of the 3Y-TZP particles after the coating process. The size of the Al(2)O(3) particles is about 20 nm. The XRD pattern shows clearly the peak of amorphous BN among the peaks of ZrO(2). PMID:19223246

  13. SIMULTANEOUS PRODUCTION OF HIGH-PURITY HYDROGEN AND SEQUESTRATION-READY CO2 FROM SYNGAS

    SciTech Connect

    Linda Denton; Hana Lorethova; Tomasz Wiltowski; Court Moorefield; Parag Kulkarni; Vladimir Zamansky; Ravi Kumar

    2003-12-01

    This final report summarizes the progress made on the program ''Simultaneous Production of High-Purity Hydrogen and Sequestration-Ready CO{sub 2} from Syngas (contract number DE-FG26-99FT40682)'', during October 2000 through September of 2003. GE Energy and Environmental Research (GE-EER) and Southern Illinois University (SIU) at Carbondale conducted the research work for this program. This program addresses improved methods to efficiently produce simultaneous streams of high-purity hydrogen and separated carbon dioxide from synthesis gas (syngas). The syngas may be produced through either gasification of coal or reforming of natural gas. The process of production of H{sub 2} and separated CO{sub 2} utilizes a dual-bed reactor and regenerator system. The reactor produces hydrogen and the regenerator produces separated CO{sub 2}. The dual-bed system can be operated under either a circulating fluidized-bed configuration or a cyclic fixed-bed configuration. Both configurations were evaluated in this project. The experimental effort was divided into lab-scale work at SIU and bench-scale work at GE-EER. Tests in a lab-scale fluidized bed system demonstrated the process for the conversion of syngas to high purity H{sub 2} and separated CO{sub 2}. The lab-scale system generated up to 95% H{sub 2} (on a dry basis). Extensive thermodynamic analysis of chemical reactions between the syngas and the fluidized solids determined an optimum range of temperature and pressure operation, where the extent of the undesirable reactions is minimum. The cycling of the process between hydrogen generation and oxygen regeneration has been demonstrated. The fluidized solids did not regenerate completely and the hydrogen purity in the reuse cycle dropped to 70% from 95% (on a dry basis). Changes in morphology and particle size may be the most dominant factor affecting the efficiency of the repeated cycling between hydrogen production and oxygen regeneration. The concept of simultaneous

  14. Improved performance of silicon nitride-based high temperature ceramics

    NASA Technical Reports Server (NTRS)

    Ashbrook, R. L.

    1977-01-01

    Recent progress in the production of Si3N4 based ceramics is reviewed: (1) high temperature strength and toughness of hot pressed Si3N4 were improved by using high purity powder and a stabilized ZrO2 additive, (2) impact resistance of hot pressed Si3N4 was increased by the use of a crushable energy absorbing layer, (3) the oxidation resistance and strength of reaction sintered Si3N4 were increased by impregnating reaction sintered silicon nitride with solutions that oxidize to Al2O3 or ZrO2, (4) beta prime SiA1ON compositions and sintering aids were developed for improved oxidation resistance or improved high temperature strength.

  15. A Rapid and Cost-Effective Laser Based Synthesis of High Purity Cadmium Selenide Quantum Dots.

    PubMed

    Gondall, M A; Qahtan, Talal F; Dastageer, M A; Yamani, Z H; Anjum, D H

    2016-01-01

    A rapid and cost effective method is developed to synthesize high purity cadmium Selenide (CdSe) quantum dots in acetone medium using second harmonic of Nd:YAG nanosecond pulsed laser of 532 nm wavelength. The thermal agglomeration due the nanosecond pulse duration of the laser was successfully eliminated by using unfocussed laser beam and thereby providing a favorable conditions for the synthesis of quantum dots having the grain size of 3 nm. The morphological and optical characterizations like XRD, HRTEM, optical absorption of the synthesized CdSe quantum dots, reveal that the material possesses the similar characteristics of the one synthesized through cumbersome wet chemical methods. Relative to the CdSe bulk material, the synthesized CdSe quantum dots showed a blue shift in the measured band gap energy from near infrared spectral region to visible region, making this material very attractive for many solar energy harvesting applications like photo-catalysis and solar cells. PMID:27398538

  16. Observation of Impact Ionization of Shallow States in Sub-Kelvin, High-Purity Germanium

    NASA Astrophysics Data System (ADS)

    Phipps, A.; Sadoulet, B.; Sundqvist, K. M.

    2016-01-01

    We report on the observation of impact ionization processes involving shallow impurity states in a sub-Kelvin, high-purity n-type germanium detector similar to those used by direct detection dark matter experiments such as the Cryogenic Dark Matter Search. An optical fiber is used to generate packets of charge carriers near one surface of the detector. The charge carriers drift to the opposite surface by application of an electric field. The resulting drift current is measured by a high-speed charge amplifier. The onset of impact ionization for both electron and hole transport is clearly observed in the drift current as the applied electric field is increased above ≈ 5 V/cm. We present the effective charge collection efficiency and trapping length as a function of applied electric field for electrons and holes. We estimate the impact ionization cross section to be on the order of 5× 10^{-13} {cm}^2.

  17. Formation of recrystallization cube texture in high purity face-centered cubic metal sheets

    SciTech Connect

    Mao, W.

    1999-10-01

    An investigation on recrystallization textures in high purity face-centered cubic (fcc) aluminum, copper, and nickel indicated that the cube texture is a unique dominant final texture. In a macroview of rolling deformation, a balanced activation of four slip systems can result in certain stability of some substructure with cube orientation in the deformed matrix. In the stable substructure the dislocation density is very low, and the dislocation configuration is rather simple in comparison to other orientations so that the cube substructure can easily be transformed into cube recrystallization nuclei by a recovery process. A high orientation gradient and correspondingly high angle boundaries to the deformed matrix are usually expected around the cube nuclei, which, therefore, grow rapidly. After the primary recrystallization, the size of cube grains is much larger than the grains with other orientations, which will be expensed as the cube grains grow further, so that the cube texture can finally become a dominant texture component.

  18. Map showing high-purity silica sand of Middle Ordovician age in the Midwestern states

    USGS Publications Warehouse

    Ketner, Keith B.

    1979-01-01

    Certain quartz sands of Middle Ordovician age in the Midwestern States are well known for their purity and are exploited for a wide variety of industrial uses. The principal Middle Ordovician formations containing high-purity sands are the St. Peter Sandstone which crops out extensively from Minnesota to Arkansas; the Everton Formation principally of Arkansas; and the Oil Creek, McLish, and Tulip Creek Formations (all of the Simpson Group) of Oklahoma. The St. Peter and sandy beds in the other formations are commonly called "sandstones," but a more appropriate term is "sands" for in most fresh exposures they are completely uncemented or very weakly cemented. On exposure to air, uncemented sands usually become "case hardened" where evaporating ground water precipitates mineral matter at the surface; but this is a surficial effect. This report summarizes the available information on the extent of exposures, range of grain size, and chemical composition of the Middle Ordovician sands.

  19. The relationship between induction time for pitting and pitting potential for high purity aluminum.

    SciTech Connect

    Wall, Frederick Douglas; Vandenavyle, Justin J.; Martinez, Michael A.

    2003-08-01

    The objective of this study was to determine if a distribution of pit induction times (from potentiostatic experiments) could be used to predict a distribution of pitting potentials (from potentiodynamic experiments) for high-purity aluminum. Pit induction times were measured for 99.99 Al in 50 mM NaCl at potentials of -0.35, -0.3, -0.25, and -0.2 V vs. saturated calomel electrode. Analysis of the data showed that the pit germination rate generally was an exponential function of the applied potential; however, a subset of the germination rate data appeared to be mostly potential insensitive. The germination rate behavior was used as an input into a mathematical relationship that provided a prediction of pitting potential distribution. Good general agreement was found between the predicted distribution and an experimentally determined pitting potential distribution, suggesting that the relationships presented here provide a suitable means for quantitatively describing pit germination rate.

  20. Diffusion Resistant, High-Purity Wafer Carriers For SI Semiconductor Production

    SciTech Connect

    Tiegs, T.N.; Leaskey, L.

    2000-10-01

    The Cooperative Research and Development Agreement (CRADA) was directed towards development of diffusion resistant, high-purity wafer carriers for Si semiconductor production with improved properties compared to current materials. The determination of the infiltration behavior is important for controlling the fabrication process to. obtain consistent high-quality products. Ammonium molybdate or molybdenum carbide were found to be suitable as a precursor to produce SiC-MoSi{sub 2}-Si composites by Si infiltration into carbon preforms. Experiments on the pyrolysis of the preforms showed variable infiltration behavior by the molten Si (within the range of conditions in the present study). Further research is required to reproducibly and consistently fabricate flaw-free articles. The strength of the composites fabricated to-date was 325{+-}124 MPa, which is higher than current commercial products. Better process control should result in higher average strengths and reduce the variability.

  1. The importance of Soret transport in the production of high purity silicon for solar cells

    NASA Technical Reports Server (NTRS)

    Srivastava, R.

    1985-01-01

    Temperature-gradient-driven diffusion, or Soret transport, of silicon vapor and liquid droplets is analyzed under conditions typical of current production reactors for obtaining high purity silicon for solar cells. Contrary to the common belief that Soret transport is negligible, it is concluded that some 15-20 percent of the silicon vapor mass flux to the reactor walls is caused by the high temperature gradients that prevail inside such reactors. Moreover, since collection of silicon is also achieved via deposition of silicon droplets onto the walls, the Soret transport mechanism becomes even more crucial due to size differences between diffusing species. It is shown that for droplets in the 0.01 to 1 micron diameter range, collection by Soret transport dominates both Brownian and turbulent mechanisms.

  2. In-growth of an electrically active defect in high-purity silicon after proton irradiation

    SciTech Connect

    Nylandsted Larsen, A.; Juul Pedersen, H.; Christian Petersen, M.; Privitera, V.; Gurimskaya, Y.; Mesli, A.

    2013-12-14

    Defect-related energy levels in the lower half of the band gap of silicon have been studied with transient-capacitance techniques in high-purity, carbon and oxygen lean, plasma-enhanced chemical-vapor deposition grown, n-and p-type silicon layers after 2-MeV proton irradiations at temperatures at or just below room temperature. The in-growth of a distinct line in deep-level transient spectroscopy spectra, corresponding to a level in the band gap at E{sub V} + 0.357 eV where E{sub V} is the energy of the valence band edge, takes place for anneal temperatures at around room temperature with an activation energy of 0.95 ± 0.08 eV. The line disappears at an anneal temperature of around 450 K. The corresponding defect is demonstrated not to contain boron, carbon, oxygen, or phosphorus. Possible defect candidates are discussed.

  3. URANIUM RECOVERY AND PURIFICATION PROCESS AND PRODUCTION OF HIGH PURITY URANIUM TETRAFLUORIDE

    DOEpatents

    Bailes, R.H.; Long, R.S.; Grinstead, R.R.

    1957-09-17

    A process is described wherein an anionic exchange technique is employed to separate uramium from a large variety of impurities. Very efficient and economical purification of contamimated uranium can be achieved by treatment of the contaminated uranium to produce a solution containing a high concentration of chloride. Under these conditions the uranium exists as an aniomic chloride complex. Then the uranium chloride complex is adsorbed from the solution on an aniomic exchange resin, whereby a portion of the impurities remain in the solution and others are retained with the uramium by the resin. The adsorbed impurities are then removed by washing the resin with pure concentrated hydrochloric acid, after which operation the uranium is eluted with pure water yielding an acidic uranyl chloride solution of high purity.

  4. Hot working of high purity Fe-C alloys in the α-range

    NASA Astrophysics Data System (ADS)

    Montheillet, F.; Le Coze, J.

    2010-07-01

    The influence of carbon in solid solution on the stress-strain curves of α-iron was investigated using model alloys prepared from high purity iron. Uniaxial compression tests were carried out within the ferritic domain at temperatures between 700 and 880 °C. Oscillating stress-strain curves observed at high temperatures and low strain rates indicate that discontinuous dynamic recrystallization takes place. The macroscopic strain rate sensitivities m and apparent activation energies Q associated with the flow stress are not significantly modified by carbon additions. By contrast, the "mesoscopic" parameters h and r associated with strain hardening and dynamic recovery, respectively, are strongly dependent on the carbon content. Finally, an estimation of the grain boundary mobilities during dynamic recrystallization was carried out from the above rheological data.

  5. Observation of Impact Ionization of Shallow States in Sub-Kelvin, High-Purity Germanium

    NASA Astrophysics Data System (ADS)

    Phipps, A.; Sadoulet, B.; Sundqvist, K. M.

    2016-07-01

    We report on the observation of impact ionization processes involving shallow impurity states in a sub-Kelvin, high-purity n-type germanium detector similar to those used by direct detection dark matter experiments such as the Cryogenic Dark Matter Search. An optical fiber is used to generate packets of charge carriers near one surface of the detector. The charge carriers drift to the opposite surface by application of an electric field. The resulting drift current is measured by a high-speed charge amplifier. The onset of impact ionization for both electron and hole transport is clearly observed in the drift current as the applied electric field is increased above ≈ 5 V/cm. We present the effective charge collection efficiency and trapping length as a function of applied electric field for electrons and holes. We estimate the impact ionization cross section to be on the order of 5× 10^{-13} mathrm {cm}^2.

  6. Observation of Impact Ionization of Shallow States in Sub-Kelvin, High-Purity Germanium

    NASA Astrophysics Data System (ADS)

    Phipps, A.; Sadoulet, B.; Sundqvist, K. M.

    2016-07-01

    We report on the observation of impact ionization processes involving shallow impurity states in a sub-Kelvin, high-purity n-type germanium detector similar to those used by direct detection dark matter experiments such as the Cryogenic Dark Matter Search. An optical fiber is used to generate packets of charge carriers near one surface of the detector. The charge carriers drift to the opposite surface by application of an electric field. The resulting drift current is measured by a high-speed charge amplifier. The onset of impact ionization for both electron and hole transport is clearly observed in the drift current as the applied electric field is increased above ≈ 5 V/cm. We present the effective charge collection efficiency and trapping length as a function of applied electric field for electrons and holes. We estimate the impact ionization cross section to be on the order of 5× 10^{-13} {cm}^2.

  7. Characterization of dislocation and defects for large high purity Ge crystals

    NASA Astrophysics Data System (ADS)

    Mei, Hao; Wang, Guojian; Guan, Yutong; Yang, Gang; Mei, Dongming; Cubed Collaboration

    2015-03-01

    Large diameter (~10 cm) high purity Germanium (HP-Ge) crystals have been growing via Czochralski method at University of South Dakota. We investigate the impacts of growth rate, time-temperature profile, and thermal gradient on the dislocation and defects distribution in HP-Ge crystals along <100>orientation. The dislocation density across the entire cross-section of a grown crystal is measured using microscope. Utilizing X-Ray Diffraction method, we obtain the rocking curves from the same crystal samples. We analyze the correlation between the full width at half maximum (FWHM) of the rocking curves and the dislocation densities from the optical observations (etch pits distribution). A model that describes the correlation of dislocation density, along the HP-Ge crystal, with the FWHM of the rock curves for XRD is established. We report these analytic results. This work is supported by DOE Grant DE-FG02-10ER46709 and the state of South.

  8. Effect of Rest Periods on Fatigue of High-Purity Aluminum

    NASA Technical Reports Server (NTRS)

    Berry, J. W.; Lemaitre, J.; Valluri, S. R.

    1958-01-01

    The effect of rest periods on the fatigue life of high-purity aluminum was investigated under two conditions. In one the specimens were tested at elevated temperatures and the rest periods were given at room temperature; in the second the specimens were tested at room temperature and the rest periods were given at elevated temperature. The results obtained indicated that the increase of life was negligible in the first condition, but an increase of life may be obtained in the second. In order to check this increase in fatigue life a second series of tests has been carried out on a different lot of specimens and again an increase in life was found. This increase of life appeared to be from 30 to 60 percent from the average of the results of 20 tests for each test condition.

  9. High Strain-Rate Response of High Purity Aluminum at Temperatures Approaching Melt

    SciTech Connect

    Grunschel, S E; Clifton, R J; Jiao, T

    2010-01-28

    High-temperature, pressure-shear plate impact experiments were conducted to investigate the rate-controlling mechanisms of the plastic response of high-purity aluminum at high strain rates (10{sup 6} s{sup -1}) and at temperatures approaching melt. Since the melting temperature of aluminum is pressure dependent, and a typical pressure-shear plate impact experiment subjects the sample to large pressures (2 GPa-7 GPa), a pressure-release type experiment was used to reduce the pressure in order to measure the shearing resistance at temperatures up to 95% of the current melting temperature. The measured shearing resistance was remarkably large (50 MPa at a shear strain of 2.5) for temperatures this near melt. Numerical simulations conducted using a version of the Nemat-Nasser/Isaacs constitutive equation, modified to model the mechanism of geometric softening, appear to capture adequately the hardening/softening behavior observed experimentally.

  10. Application of Thermodynamic Calculations to the Pyro-refining Process for Production of High Purity Bismuth

    NASA Astrophysics Data System (ADS)

    Mezbahul-Islam, Mohammad; Belanger, Frederic; Chartrand, Patrice; Jung, In-Ho; Coursol, Pascal

    2016-04-01

    The present work has been performed with the aim to optimize the existing process for the production of high purity bismuth (99.999 pct). A thermo-chemical database including most of the probable impurities of bismuth (Bi-X, X = Ag, Au, Al, Ca, Cu, Fe, Mg, Mn, Na, Ni, Pb, S, Sb, Sn, Si, Te, Zn) has been constructed to perform different thermodynamic calculations required for the refining process. Thermodynamic description for eight of the selected binaries, Bi-Ca, Cu, Mn, Ni, Pb, S, Sb, and Sn, has been given in the current paper. Using the current database, different thermodynamic calculations have been performed to explain the steps involved in the bismuth refining process.

  11. Production of carbon monoxide-free hydrogen and helium from a high-purity source

    DOEpatents

    Golden, Timothy Christopher; Farris, Thomas Stephen

    2008-11-18

    The invention provides vacuum swing adsorption processes that produce an essentially carbon monoxide-free hydrogen or helium gas stream from, respectively, a high-purity (e.g., pipeline grade) hydrogen or helium gas stream using one or two adsorber beds. By using physical adsorbents with high heats of nitrogen adsorption, intermediate heats of carbon monoxide adsorption, and low heats of hydrogen and helium adsorption, and by using vacuum purging and high feed stream pressures (e.g., pressures of as high as around 1,000 bar), pipeline grade hydrogen or helium can purified to produce essentially carbon monoxide -free hydrogen and helium, or carbon monoxide, nitrogen, and methane-free hydrogen and helium.

  12. Crystallographic Analysis of Nucleation at Hardness Indentations in High-Purity Aluminum

    NASA Astrophysics Data System (ADS)

    Xu, Chaoling; Zhang, Yubin; Lin, Fengxiang; Wu, Guilin; Liu, Qing; Juul Jensen, Dorte

    2016-08-01

    Nucleation at Vickers hardness indentations has been studied in high-purity aluminum cold-rolled 12 pct. Electron channeling contrast was used to measure the size of the indentations and to detect nuclei, while electron backscattering diffraction was used to determine crystallographic orientations. It is found that indentations are preferential nucleation sites. The crystallographic orientations of the deformed grains affect the hardness and the nucleation potentials at the indentations. Higher hardness gives increased nucleation probabilities. Orientation relationships between nuclei developed at different indentations within one original grain are analyzed and it is found that the orientation distribution of the nuclei is far from random. It is suggested that it relates to the orientations present near the indentation tips which in turn depend on the orientation of the selected grain in which they form. Finally, possible nucleation mechanisms are briefly discussed.

  13. Experimental research of phase transition's kinetics in a liquid melt of high-purity aluminum

    NASA Astrophysics Data System (ADS)

    Vorontsov, V. B.; Zhuravlev, D. V.; Cherepanov, A. S.

    2015-08-01

    This scientific work is devoted to the studying of the genetic connection structures of solid and liquid phases. Fourier analysis of signals of acoustic emission (AE) accompanying melting high purity aluminum from the melting point up to t = 860°C was performed. Based on the results of previous studies cluster formations in the melt - the micro-regions, those retain crystallinity (areas with short-range order of symmetry) were considered as the source of AE. The experimental data allowed to follow the dynamics of disorder zones range order in the melt with increasing melt temperature up to their complete destruction. The presented results of spectral analysis of the signals were analyzed from the standpoint of the theory of cluster melting metals.

  14. Physical and mechanical metallurgy of high purity Nb for accelerator cavities

    SciTech Connect

    Bieler, T. R.; Wright, N. T.; Pourboghrat, F.; Compton, C.; Hartwig, K. T.; Baars, D.; Zamiri, A.; Chandrasekaran, S.; Darbandi, P.; Jiang, H.; Skoug, E.; Balachandran, S.; Ice, Gene E; Liu, W.

    2010-01-01

    In the past decade, high Q values have been achieved in high purity Nb superconducting radio frequency (SRF) cavities. Fundamental understanding of the physical metallurgy of Nb that enables these achievements is beginning to reveal what challenges remain to establish reproducible and cost-effective production of high performance SRF cavities. Recent studies of dislocation substructure development and effects of recrystallization arising from welding and heat treatments and their correlations with cavity performance are considered. With better fundamental understanding of the effects of dislocation substructure evolution and recrystallization on electron and phonon conduction, as well as the interior and surface states, it will be possible to design optimal processing paths for cost-effective performance using approaches such as hydroforming, which minimizes or eliminates welds in a cavity.

  15. Preparation and characterization of (10)B boric acid with high purity for nuclear industry.

    PubMed

    Zhang, Weijiang; Liu, Tianyu; Xu, Jiao

    2016-01-01

    Boric acid is often added into coolant as neutron capture agent for pressurized water reactor, whose amount is influenced by its abundance and purity. Therefore, the preparation of enriched (10)B boric acid with high purity is beneficial to nuclear industry. (10)B is also used in developing tumor-specific boronated drugs in boron neutron capture therapy. The boronated drug can be administered to patient intravenously, intratumorally, or deposited at tumor site in surgical excision. Thus, enriched (10)B boric acid is of practical significance in the field of medicine. Self-made boron trifluoride-methanol-complex solution was selected as one of the experimental reagents, and the preparation of (10)B acid was realized by one-step reaction for the complexes with water and calcium chloride. The determination of electrical conductivity in reaction process proves that the optimum reaction time was 16-20 h. Furthermore, the effect of reaction time, ratio of calcium chloride to complex as well as the amount of water on the purity and yield of boric acid was investigated. Finally, the optimum reaction time was 20 h, the optimal solid-liquid ratio (molar ratio) was 3:1, and the amount of water was 1 L of deionized water for each mol of the complex. H2O2 was added in the reaction process to remove Fe(2+). After recrystallization, IR spectra of (10)B boric acid was measured and compared with standard to verify the product of boric acid. The feasibility of the preparation method was determined by the detection of XRD of boric acid. To observe the morphology by polarizing microscope, crystal structure was obtained. The purity of the final product is 99.95 %, and the yield is 96.47 %. The ion concentration of boric acid accords with the national standard of high purity, which was determined by ICP. PMID:27516940

  16. Recycling of high purity selenium from CIGS solar cell waste materials

    SciTech Connect

    Gustafsson, Anna M.K. Foreman, Mark R.StJ.; Ekberg, Christian

    2014-10-15

    Highlights: • A new method for recycling of selenium from CIGS solar cell materials is presented. • Separation of selenium as selenium dioxide after heating in oxygen atmosphere. • Complete selenium separation after oxidation of <63 μm particles at 800 °C for 1 h. • After reduction of selenium dioxide the selenium purity was higher than 99.999 wt%. - Abstract: Copper indium gallium diselenide (CIGS) is a promising material in thin film solar cell production. To make CIGS solar cells more competitive, both economically and environmentally, in comparison to other energy sources, methods for recycling are needed. In addition to the generally high price of the material, significant amounts of the metals are lost in the manufacturing process. The feasibility of recycling selenium from CIGS through oxidation at elevated temperatures was therefore examined. During oxidation gaseous selenium dioxide was formed and could be separated from the other elements, which remained in solid state. Upon cooling, the selenium dioxide sublimes and can be collected as crystals. After oxidation for 1 h at 800 °C all of the selenium was separated from the CIGS material. Two different reduction methods for reduction of the selenium dioxide to selenium were tested. In the first reduction method an organic molecule was used as the reducing agent in a Riley reaction. In the second reduction method sulphur dioxide gas was used. Both methods resulted in high purity selenium. This proves that the studied selenium separation method could be the first step in a recycling process aimed at the complete separation and recovery of high purity elements from CIGS.

  17. Strong upconversion from Er{sub 3}Al{sub 5}O{sub 12} ceramic powders prepared by low temperature direct combustion synthesis

    SciTech Connect

    Maciel, Glauco S.; Rakov, Nikifor; Fokine, Michael; Carvalho, Isabel C. S.; Pinheiro, Carlos B.

    2006-08-21

    Crystalline ceramic powders of Er{sub 3}Al{sub 5}O{sub 12} were obtained by low temperature direct combustion synthesis. Irradiating the sample with a low-power continuous-wave infrared (1.48 {mu}m) diode laser led to ultraviolet, violet, blue, green, and red (380, 410, 456, 495, 525, 550, and 660 nm) emissions. The strong upconversion luminescence appeared to the eyes as an intense green color. The presence of efficient four- and three-photon frequency upconversion processes makes this material an excellent candidate for use in photonic devices based on upconverter phosphors.

  18. Influence of strain rate and temperature on the structure/property behavior of high-purity titanium

    SciTech Connect

    Gray, G.T. III

    1997-05-01

    The effect of strain rate, temperature, grain size, and texture on the substructure and mechanical response of high-purity polycrystalline titanium is presented. The compressive stress-strain response of 20 and 240 {mu}m grain size high-purity Ti was found to depend on both the applied strain rate; 0.001 {le} {epsilon} {le} 7500 s{sup -1}, and the test temperature; 77 {le} T {le} 873 K. The rate of strain hardening in Ti is seen to increase with increasing strain rate. The substructure of high-purity Ti deformed at high-strain-rate or quasi-statically at 77K displayed a higher incidence of deformation twinning than during quasi-static deformation at 298K.

  19. Analysis of ceramic layer for solid oxide fuel cells by LA-ICP-MS

    SciTech Connect

    Westheide, J.; Becker, J.S.; Dietze, H.J.; Broekaert, J.A.C.

    1996-09-01

    Among the different analytical techniques, laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is well established as a solid-state mass spectrometric method for the trace analysis of conducting and nonconducting material. Furthermore, LA-ICP-MS enables ceramic layers with thickness > few {mu}m and a lateral resolution of >10 {mu}m to be analyzed. In this paper, trace analysis on the ceramic layers of solid oxide fuel cells (SOFC) (e.g., La{sub y{center_dot}x}Sr{sub x}MnO{sub 3}, yttrium-stabilized ZrO{sub 2}) is described. Due to a lack of standard reference materials for the analysis of perovskites, the quantification of analytical results can be facilitated by the use of prepared synthetic standards. The synthetic standard samples were prepared by mixing powdered inorganic compounds of ultra-high-purity (e.g., preparation of a stoichiometric mixture of high-purity La{sub 2}(CO{sub 3}){sub 3}, SrCO{sub 3} and MnO{sub 2} mixed with ultrapure graphite as binder). In order to determine the relative sensitivity coefficients (RSC) or calibration curves elemental spikes (high-purity compounds of 30 elements in the concentration range of 50-2000 ppm) were added to these mixtures. The use of UV laser (frequency-quadrupled Nd:YAG laser) improved the laser ablation process in regard to better reproducibility and accuracy in comparison with an infrared system. Results of quantitative measurements of trace elements of sintered La{sub y{center_dot}x}Sr{sub x}MnO{sub 3} and yttrium-stabilized zirconia layers are presented and compared with those of other methods.

  20. Mechanical properties of yttria-stabilized zirconia ceramics

    NASA Astrophysics Data System (ADS)

    Shirooyeh A, Mahmood R.

    Superplasticity is a well-known characteristic of Y2O 3-stabilized tetragonal zirconia (3Y-TZP) ceramic composites at elevated temperatures. The present investigation was originated to evaluate the potential of producing zirconia ceramics suitable for achieving superplasticity. High purity 3 mol% Y2O3-stabilized tetragonal zirconia (3Y-TZP) ceramic composites containing 20 wt% alumina were successfully consolidated by application of Cold Isostatic Pressing (CIP) followed by a subsequent sintering process. Constant-stress tensile creep experiments at elevated temperatures were conducted in order to examine plastic deformation behavior of the material. In addition to mechanical testing data, the microstructure observations confirmed superplastic properties of the ceramic composite. It is also known that in order to attain High Strain Rate Superplasticity (HSRS) in zirconia ceramics, it is essential to retain a stable fine-grained microstructure at high temperatures. Experiments have confirmed that adding a second soft phase such as spinel can facilitate to reach high strain-rate superplasticity in zirconia ceramics by suppressing grain growth during sintering process and enhancing cation diffusion. In the present investigation, homogenous 3Y-TZP ceramic composite powders containing 30 vol% MgAl2O4 spinel were successfully prepared through both physical-based and chemical-based methods. An electric current-activated method known as Spark Plasma Sintering (SPS) was employed for powder consolidation process. This is a very rapid electric current-activated sintering technique having a heating rate of 300 K/min. The powder preparation and consolidation steps were carried out over a wide range of conditions to ensure a homogenous nanocomposite. The experiments showed that fully-dense zirconia ceramics with an average initial grain size of the order of ˜100 nm can be sintered at the relatively low processing temperature of 1373 K in 10 min. In order to study the

  1. Construction of a Bacillus amyloliquefaciens strain for high purity levan production.

    PubMed

    Feng, Jun; Gu, Yanyan; Han, Lifang; Bi, Kexin; Quan, Yufeng; Yang, Chao; Zhang, Wei; Cao, Mingfeng; Wang, Shufang; Gao, Weixia; Sun, Yang; Song, Cunjiang

    2015-06-01

    Bacillus amyloliquefaciens NK-1 has the potential to produce levan and poly-gamma-glutamic acid (γ-PGA) simultaneously. However, it is not possible to purify each single product from the same strain because the extraction process is identical. We deleted the pgs cluster (for γ-PGA synthesis) from the NK-1 strain and constructed a γ-PGA-deficient NK-ΔLP strain. Nuclear magnetic results showed that the NK-ΔLP strain could produce high purity levan product. However, its levan titer was only 1.96 g L(-1) in the basal medium. Single-factor experimental and response surface methodology was used to optimize the culture condition, leading to levan titer of 13.9 and 22.6 g L(-1) in flask culture and in a 5-L bioreactor, respectively. The levan purity can reach to 92.7% after 48 h cultivation. Furthermore, the relationship between levanase (LevB) and levan molecular weight was studied. The results showed that LevB resulted in the production of low molecular weight levan and its expression level determined the ratio of high and low molecular weight levan. We also deleted the sac cluster (for levan synthesis) from the NK-1 strain and constructed a levan-deficient NK-L strain. The NK-L strain exhibited increased purity of γ-PGA product from 79.5 to 91.2%. PMID:25953857

  2. Determination of nitrogen monoxide in high purity nitrogen gas with an atmospheric pressure ionization mass spectrometer

    NASA Technical Reports Server (NTRS)

    Kato, K.

    1985-01-01

    An atmospheric pressure ionization mass spectrometric (API-MS) method was studied for the determination of residual NO in high purity N2 gas. The API-MS is very sensitive to NO, but the presence of O2 interferes with the NO measurement. Nitrogen gas in cylinders as sample gas was mixed with NO standard gas and/or O2 standard gas, and then introduced into the API-MS. The calibration curves of NO and O2 has linearity in the region of 0 - 2 ppm, but the slopes changed with every cylinder. The effect of O2 on NO+ peak was additive and proportional to O2 concentration in the range of 0 - 0.5 ppm. The increase in NO+ intensity due to O2 was (0.07 - 0.13)%/O2, 1 ppm. Determination of NO and O2 was carried out by the standard addition method to eliminate the influence of variation of slopes. The interference due to O2 was estimated from the product of the O2 concentration and the ratio of slope A to Slope B. Slope A is the change in the NO+ intensity with the O2 concentration. Slope B is the intensity with O2 concentration.

  3. Improving axion detection sensitivity in high purity germanium detector based experiments

    NASA Astrophysics Data System (ADS)

    Xu, Wenqin; Elliott, Steven

    2015-04-01

    Thanks to their excellent energy resolution and low energy threshold, high purity germanium (HPGe) crystals are widely used in low background experiments searching for neutrinoless double beta decay, e.g. the MAJORANA DEMONSTRATOR and the GERDA experiments, and low mass dark matter, e.g. the CDMS and the EDELWEISS experiments. A particularly interesting candidate for low mass dark matter is the axion, which arises from the Peccei-Quinn solution to the strong CP problem and has been searched for in many experiments. Due to axion-photon coupling, the postulated solar axions could coherently convert to photons via the Primakeoff effect in periodic crystal lattices, such as those found in HPGe crystals. The conversion rate depends on the angle between axions and crystal lattices, so the knowledge of HPGe crystal axis is important. In this talk, we will present our efforts to improve the HPGe experimental sensitivity to axions by considering the axis orientations in multiple HPGe crystals simultaneously. We acknowledge the support of the U.S. Department of Energy through the LANL/LDRD Program.

  4. GELATIO: a general framework for modular digital analysis of high-purity Ge detector signals

    NASA Astrophysics Data System (ADS)

    Agostini, M.; Pandola, L.; Zavarise, P.; Volynets, O.

    2011-08-01

    GELATIO is a new software framework for advanced data analysis and digital signal processing developed for the GERDA neutrinoless double beta decay experiment. The framework is tailored to handle the full analysis flow of signals recorded by high purity Ge detectors and photo-multipliers from the veto counters. It is designed to support a multi-channel modular and flexible analysis, widely customizable by the user either via human-readable initialization files or via a graphical interface. The framework organizes the data into a multi-level structure, from the raw data up to the condensed analysis parameters, and includes tools and utilities to handle the data stream between the different levels. GELATIO is implemented in C++. It relies upon ROOT and its extension TAM, which provides compatibility with PROOF, enabling the software to run in parallel on clusters of computers or many-core machines. It was tested on different platforms and benchmarked in several GERDA-related applications. A stable version is presently available for the GERDA Collaboration and it is used to provide the reference analysis of the experiment data.

  5. Evaluation of Electric Load Following Capability on Fuel Cell System Fueled by High-Purity Hydrogen

    NASA Astrophysics Data System (ADS)

    Doi, Yusuke; Park, Deaheum; Ishida, Masayoshi; Fujisawa, Akitoshi; Miura, Shinichi

    This paper describes the electrical response in load change concerning a fuel cell system fueled by high-purity hydrogen. The purpose of this study is that the fuel cell system is applied to make up for unstable electrical output of a photovoltaic system as a renewable energy. As an alternative method of secondary battery, the fuel cell system, which is able to continuously generate power as long as fuel is supplied, is expected to provide power with high reliability and stability. To evaluate the load-following capability of a polymer electrolyte fuel cell (PEFC) system, an experimental equipment was constructed with a 200W PEFC stack (number of cells: 20, cell area: 200cm2) which was supplied with hydrogen from a compressed hydrogen cylinder and a metal hydride canister. We measured the transient phenomenon of current and cell voltage when the PEFC stack was inputted step-up current loads that changed in the range of 0∼300mA/cm2. As a result, we have found that the PEFC system with both hydrogen supply sources is able to response at a time constant of 6.6∼11.6μsec under enough oxygen supply and a load below the PEFC rated power.

  6. Influence of Ta content in high purity niobium on cavity performance

    SciTech Connect

    P. Kneisel; G. Ciovati; G. R. Myneni; W. Singer; X. Singer; D. Proch; T. Carneiro

    2005-05-01

    In a previous paper [1] we have reported about initial tests of single cell 1500 MHz cavities made from high purity niobium with three different Ta contents of 160 ppm , {approx}600 ppm and {approx}1400 ppm. These cavities had been treated by buffered chemical polishing several times and 100 {micro}m, 200 {micro}m and 300 {micro}m of material had been removed from the surfaces. This contribution reports about subsequent tests following post purification heat treatments with Ti and ''in situ'' baking. As a result, all cavities exhibited increased quench fields due to the improved thermal conductivity after the heat treatment. After the ''in situ'' baking at 120 C for {approx} 40 hrs the always present Q-drop at high fields disappeared and further improvements in accelerating gradient could be realized. Gradients as high as E{sub acc} = 35 MV/m were achieved and there were no clear indications that the cavity performance was influenced by the Ta content in the material. A multi-cell cavity from the high Ta content material has been fabricated and initial results are reported.

  7. Formation process of high-purity Ge-on-insulator layers by Ge-condensation technique

    NASA Astrophysics Data System (ADS)

    Nakaharai, S.; Tezuka, T.; Hirashita, N.; Toyoda, E.; Moriyama, Y.; Sugiyama, N.; Takagi, S.

    2009-01-01

    Formation process of Ge-on-insulator (GOI) layers by Ge condensation with very high purity of Ge is clarified in terms of diffusion behaviors of Si and Ge in a SiGe layer. It is shown that the diffusion behavior affects the Ge condensation process, and the purity of GOI layer can be determined by the relation between oxidation and diffusion of Si. Experimental results support a model of GOI formation that the selective oxidation of Si in SiGe continues until the formation of a GOI layer with the residual Si fraction of less than 0.01%. Based on this model, we quantitatively clarify the reason why GOI layers can reach very low residual Si fraction without oxidizing Ge by calculating the diffusion behavior of Si during the Ge condensation process. As a result, we have found that the thermal diffusion of Si is sufficiently fast so that the selective oxidation of Si can continue during the GOI formation process until the averaged residual Si fraction in the SGOI layer becomes lower than 0.03%, which is essentially consistent with the experimental results. In addition, we have found that, even if the GOI layer is thick, the Ge purity of GOI layer can approach 100% infinitely in principle by enhancing the Si diffusion in SGOI compared to the oxidation rate of SGOI.

  8. Safety studies conducted on high-purity trans-resveratrol in experimental animals.

    PubMed

    Williams, Lonnie D; Burdock, George A; Edwards, James A; Beck, Mareike; Bausch, Jochen

    2009-09-01

    trans-Resveratrol is a naturally occurring polyphenolic compound found in a variety of foods, but predominantly in grapes. Safety studies were conducted on high-purity trans-resveratrol (Resvida), including skin and eye irritation, dermal sensitization, subchronic and reproductive toxicity, genotoxicity, and absorption, metabolism and excretion. Resvida was non-irritating to skin and eyes and non-sensitizing. It was non-mutagenic in a bacterial reverse mutation assay in Salmonella typhimurium and Escherichia coli, but exhibited clastogenic activity in a chromosomal aberration test in human lymphocytes. However, in an in vivo bone marrow micronucleus test in rats, Resvida was non-genotoxic. In a 28-day study, Resvida caused no adverse effects in rats at 50, 150 and 500 mg/kg bw/day. Similarly, in a 90-day study, Resvida did not cause any adverse effects in rats at up to 700 mg/kg bw/day; the highest dose tested. Resvida did not induce any adverse reproductive effects in an embryo-fetal toxicity study in rats at a dose of 750 mg/kg bw/day. Also, in vitro and in vivo absorption, metabolism, and excretion studies in Caco-2 cells, rat primary hepatocytes and male and female rats (in vivo) show that Resvida is readily absorbed, metabolized and excreted. These studies provide evidence that Resvida is well tolerated and non-toxic. PMID:19505523

  9. Industrial symbiosis: high purity recovery of metals from Waelz sintering waste by aqueous SO2 solution.

    PubMed

    Copur, Mehmet; Pekdemir, Turgay; Colak, Sabri; Künkül, Asim

    2007-10-22

    Sintering operation in the production of Zn, Cd, and Pb by Waelz process produces a powdery waste containing mainly (about 70%) ZnO, CdO, and PbO. The waste may be referred to as Waelz sintering waste (WSW). The aim of this study is to develop a process for the separation and recovery of the metals from WSW with high purities. The process is based on the dissolution of the WSW in aqueous SO2 solution. The research reported here concentrated on the effect of some important operational parameters on dissolution process. The parameters investigated and their ranges were as follows: SO(2) gas flow rate (V); 38-590 ml/min, stirring speed (W); 100-1000 rpm, reaction temperature (T); 13-60 degrees C, reaction time (t); 1-16 min, and solid-liquid ratio (S/L); 0.1-0.5 g/ml. The results showed that the dissolution rate increased with increasing W, V, and S/L and decreasing T. The best dissolution conditions were found to be V=325 ml/min, W=600 rpm, t=6 min, T=21 degrees C, and S/L=0.1g/ml. Separation of Zn from Cd involved precipitation of ZnSO3 from a mixture solution. The best pH level for the precipitation was observed to be 6. PMID:17482352

  10. High-energy proton radiation damage of high-purity germanium detectors

    NASA Technical Reports Server (NTRS)

    Pehl, R. H.; Varnell, L. S.; Metzger, A. E.

    1978-01-01

    Quantitative studies of radiation damage in high-purity germanium gamma-ray detectors due to high-energy charged particles have been carried out; two 1.0 cm thick planar detectors were irradiated by 6 GeV/c protons. Under proton bombardment, degradation in the energy resolution was found to begin below 7 x 10 to the 7th protons/sq cm and increased proportionately in both detectors until the experiment was terminated at a total flux of 5.7 x 10 to the 8th protons/sq cm, equivalent to about a six year exposure to cosmic-ray protons in space. At the end of the irradiation, the FWHM resolution measured at 1332 keV stood at 8.5 and 13.6 keV, with both detectors of only marginal utility as a spectrometer due to the severe tailing caused by charge trapping. Annealing these detectors after proton damage was found to be much easier than after neutron damage.

  11. Development, fabrication and test of a high purity silica heat shield

    NASA Technical Reports Server (NTRS)

    Rusert, E. L.; Drennan, D. N.; Biggs, M. S.

    1978-01-01

    A highly reflective hyperpure ( 25 ppm ion impurities) slip cast fused silica heat shield material developed for planetary entry probes was successfully scaled up. Process development activities for slip casting large parts included green strength improvements, casting slip preparation, aggregate casting, strength, reflectance, and subscale fabrication. Successful fabrication of a one-half scale Saturn probe (shape and size) heat shield was accomplished while maintaining the silica high purity and reflectance through the scale-up process. However, stress analysis of this original aggregate slip cast material indicated a small margin of safety (MS. = +4%) using a factor of safety of 1.25. An alternate hyperpure material formulation to increase the strength and toughness for a greater safety margin was evaluated. The alternate material incorporates short hyperpure silica fibers into the casting slip. The best formulation evaluated has a 50% by weight fiber addition resulting in an 80% increase in flexural strength and a 170% increase in toughness over the original aggregate slip cast materials with comparable reflectance.

  12. Native oxidation of ultra high purity Cu bulk and thin films

    NASA Astrophysics Data System (ADS)

    Iijima, J.; Lim, J.-W.; Hong, S.-H.; Suzuki, S.; Mimura, K.; Isshiki, M.

    2006-12-01

    The effect of microstructure and purity on the native oxidation of Cu was studied by using angle-resolved X-ray photoelectron spectroscopy (AR-XPS) and spectroscopic ellipsometry (SE). A high quality copper film prepared by ion beam deposition under a substrate bias voltage of -50 V (IBD Cu film at Vs = -50 V) showed an oxidation resistance as high as an ultra high purity copper (UHP Cu) bulk, whereas a Cu film deposited without substrate bias voltage (IBD Cu film at Vs = 0 V) showed lower oxidation resistance. The growth of Cu 2O layer on the UHP Cu bulk and both types of the films obeyed in principle a logarithmic rate law. However, the growth of oxide layer on the IBD Cu films at Vs = 0 and -50 V deviated upward from the logarithmic rate law after the exposure time of 320 and 800 h, respectively. The deviation from the logarithmic law is due to the formation of CuO on the Cu 2O layer after a critical time.

  13. Effect of chromium on low-temperature deformation of high-purity iron

    NASA Technical Reports Server (NTRS)

    Kelley, M. J.; Stoloff, N. S.

    1976-01-01

    A series of very low interstitial Fe-Cr alloys containing 0, 1, 3, 5, and 10 wt% Cr were prepared by vacuum melting and fabricated under argon to 1.83 mm diam wires exposed in an alumina system to wet hydrogen for 200 h at 1423 K followed by 1000 h in ZrH2-purified hydrogen at 1573 K. The wires were then transverse-rolled into thin sheet and cut into tensile specimens subjected to electropolishing and strained to fracture in a series of cryogenic baths ranging from 4.2 K to room temperature. It is shown that small Cr additions lower the twinning stress so that yielding occurs by twinning rather than by slip. Cr in amounts up to 10 wt% has little effect on the yield strength of high-purity Fe between 147 and 300 K, and ductility is not greatly affected at any test temperature. Higher solute contents provide appreciable strengthening only at temperatures of 112 K and below.

  14. Determination of halogens and sulfur in high-purity polyimide by IC after digestion by MIC.

    PubMed

    Krzyzaniak, Sindy R; Santos, Rafael F; Dalla Nora, Flavia M; Cruz, Sandra M; Flores, Erico M M; Mello, Paola A

    2016-09-01

    In this work, a method for sample preparation of high-purity polyimide was proposed for halogens and sulfur determination by ion chromatography (IC) with conductivity detection and, alternatively, by inductively coupled plasma mass spectrometry (ICP-MS). A relatively high polyimide mass (600mg) was completely digested by microwave-induced combustion (MIC) using 20bar of O2 and 50mmolL(-1) NH4OH as absorbing solution. These conditions allowed final solutions with low carbon content (<10mgL(-1)) and suitable pH for analysis by both IC and ICP-MS. The accuracy was evaluated using a certified reference material of polymer for Cl, Br and S and spike recovery experiments for all analytes. No statistical difference (t-test, 95% of confidence level) was observed between the results obtained for Cl, Br and S by IC after MIC and the certified values. In addition, spike recoveries obtained for F, Cl, Br, I and S ranged from 94% to 101%. The proposed method was suitable for polyimide decomposition for further determination of halogens and sulfur by IC and by ICP-MS (Br and I only). Taking into account the lack of methods and the difficulty of bringing this material into solution, MIC can be considered as a suitable alternative for the decomposition of polyimide for routine quality control of halogens and sulfur using IC or ICP-MS. PMID:27343595

  15. Simulation study comparing high-purity germanium and cadmium zinc telluride detectors for breast imaging

    PubMed Central

    Campbell, DL; Peterson, TE

    2014-01-01

    We conducted simulations to compare the potential imaging performance for breast cancer detection with High-Purity Germanium (HPGe) and Cadmium Zinc Telluride (CZT) systems with 1% and 3.8% energy resolution at 140 keV, respectively. Using the Monte Carlo N-Particle (MCNP5) simulation package, we modelled both 5 mm-thick CZT and 10 mm-thick HPGe detectors with the same parallel-hole collimator for the imaging of a breast/torso phantom. Simulated energy spectra were generated, and planar images were created for various energy windows around the 140-keV photopeak. Relative sensitivity and scatter and the torso fractions were calculated along with tumour contrast and signal-to-noise ratios (SNR). Simulations showed that utilizing a ±1.25% energy window with an HPGe system better suppressed torso background and small-angle scattered photons than a comparable CZT system using a −5%/+10% energy window. Both systems provided statistically similar contrast and SNR, with HPGe providing higher relative sensitivity. Lowering the counts of HPGe images to match CZT count density still yielded equivalent contrast between HPGe and CZT. Thus, an HPGe system may provide equivalent breast imaging capability at lower injected radioactivity levels when acquiring for equal imaging time. PMID:25360792

  16. High purity isolation and quantification of semiconducting carbon nanotubes via column chromatography.

    PubMed

    Tulevski, George S; Franklin, Aaron D; Afzali, Ali

    2013-04-23

    The isolation of semiconducting carbon nanotubes (CNTs) to ultrahigh (ppb) purity is a prerequisite for their integration into high-performance electronic devices. Here, a method employing column chromatography is used to isolate semiconducting nanotubes to 99.9% purity. The study finds that by modifying the solution preparation step, both the metallic and semiconducting fraction are resolved and elute using a single surfactant system, allowing for multiple iterations. Iterative processing enables a far more rapid path to achieving the level of purities needed for high performance computing. After a single iteration, the metallic peak in the absorption spectra is completely attenuated. Although absorption spectroscopy is typically used to characterize CNT purity, it is found to be insufficient in quantifying solutions of high purity (>98 to 99%) due to low signal-to-noise in the metallic region of ultrahigh purity solutions. Therefore, a high throughput electrical testing method was developed to quantify the degree of separation by characterizing ∼4000 field-effect transistors fabricated from the separated nanotubes after multiple iterations of the process. The separation and characterization methods described here provide a path to produce the ultrahigh purity semiconducting CNT solutions needed for high performance electronics. PMID:23484490

  17. Preparation of high purity glasses in the Ga-Ge-As-Se system

    NASA Astrophysics Data System (ADS)

    Shiryaev, V. S.; Velmuzhov, A. P.; Tang, Z. Q.; Churbanov, M. F.; Seddon, A. B.

    2014-11-01

    Small additions of Ga to Ge-As-Se glasses are known to enhance rare earth ion solubility in Ge-As-Se chalcogenide glasses designed for active optical applications. The effect of variants and conditions for producing samples of an exemplar Ge16As17Se64Ga3 (atomic%) glass on optical transmission, and the content of limiting impurities, is investigated. To prepare the high-purity glass samples, chemical distillation for purification of the Ge-As-Se base-glass is used. Next, a new vapor phase transport approach of metallic Ga transfer in a GaI3 flow is developed to purify and add the batch of metallic gallium into the silica-glass reactor for the Ge-As-Se-Ga glass synthesis. A thermodynamic equilibrium based vapor phase transport model is discussed. In the best examples of these glasses, the content of residual impurities is: hydrogen - 0.15 ppm, oxygen - <1 ppm, and transition metals - less than 0.1 ppm.

  18. Interaction between a high purity magnesium surface and PCL and PLA coatings during dynamic degradation.

    PubMed

    Chen, Ying; Song, Yang; Zhang, Shaoxiang; Li, Jianan; Zhao, Changli; Zhang, Xiaonong

    2011-04-01

    In this study, polycaprolactone (PCL) and polylactic acid (PLA) coatings were prepared on the surface of high purity magnesium (HPMs), respectively, and electrochemical and dynamic degradation tests were used to investigate the degradation behaviors of these polymer-coated HPMs. The experimental results indicated that two uniform and smooth polymer films with thicknesses between 15 and 20 µm were successfully prepared on the HPMs. Electrochemical tests showed that both PCL-coated and PLA-coated HPMs had higher free corrosion potentials (E(corr)) and smaller corrosion currents (I(corr)) in the modified simulated body fluid (m-SBF) at 37 °C, compared to those of the uncoated HPMs. Dynamic degradation tests simulating the flow conditions in coronary arteries were carried out on a specific test platform. The weight of the specimens and the pH over the tests were recorded to characterize the corrosion performance of those samples. The surfaces of the specimens after the dynamic degradation tests were also examined. The data implied that there was a special interaction between HPM and its polymer coatings during the dynamic degradation tests, which undermined the corrosion resistance of the coated HPMs. A model was proposed to illustrate the interaction between the polymer coatings and HPM. This study also suggested that this reciprocity may also exist on the implanted magnesium stents coated with biodegradable polymers, which is a potential obstacle for the further development of drug-eluting magnesium stents. PMID:21358027

  19. Leakage current in high-purity germanium detectors with amorphous semiconductor contacts

    NASA Astrophysics Data System (ADS)

    Looker, Q.; Amman, M.; Vetter, K.

    2015-03-01

    Amorphous semiconductor electrical contacts on high-purity Ge radiation detectors have become a valuable technology because they are simple to fabricate, result in thin dead layers, block both electron and hole injection, and can readily be finely segmented as needed for applications requiring imaging or particle tracking. Though significant numbers of detectors have been successfully produced for a variety of applications using the amorphous semiconductor contact technology, there remains a need to better understand the dependence of performance characteristics, particularly leakage current, on the fabrication process parameters so that the performance can be better optimized. To this end, we have performed a systematic study of leakage current on RF-sputter-deposited amorphous-Ge (a-Ge) and amorphous-Si (a-Si) contacts as a function of process and operational parameters including sputter gas pressure and composition, number of detector temperature cycles, and time spent at room temperature. The study focused primarily on the current resulting from electron injection at the contact. Significant findings from the study include that a-Si produces lower electron injection than a-Ge, the time the detector spends at room temperature rather than the number of temperature cycles experienced by the detector is the primary factor associated with leakage current change when the detector is warmed, and the time stability of the a-Ge contact depends on the sputter gas pressure with a higher pressure producing more stable characteristics.

  20. Simulation study comparing high-purity germanium and cadmium zinc telluride detectors for breast imaging

    NASA Astrophysics Data System (ADS)

    Campbell, D. L.; Peterson, T. E.

    2014-11-01

    We conducted simulations to compare the potential imaging performance for breast cancer detection with High-Purity Germanium (HPGe) and Cadmium Zinc Telluride (CZT) systems with 1% and 3.8% energy resolution at 140 keV, respectively. Using the Monte Carlo N-Particle (MCNP5) simulation package, we modelled both 5 mm-thick CZT and 10 mm-thick HPGe detectors with the same parallel-hole collimator for the imaging of a breast/torso phantom. Simulated energy spectra were generated, and planar images were created for various energy windows around the 140 keV photopeak. Relative sensitivity and scatter and the torso fractions were calculated along with tumour contrast and signal-to-noise ratios (SNR). Simulations showed that utilizing a ±1.25% energy window with an HPGe system better suppressed torso background and small-angle scattered photons than a comparable CZT system using a -5%/+10% energy window. Both systems provided statistically similar contrast and SNR, with HPGe providing higher relative sensitivity. Lowering the counts of HPGe images to match CZT count density still yielded equivalent contrast between HPGe and CZT. Thus, an HPGe system may provide equivalent breast imaging capability at lower injected radioactivity levels when acquiring for equal imaging time.

  1. High-purity propionate production from glycerol in mixed culture fermentation.

    PubMed

    Chen, Yun; Wang, Ting; Shen, Nan; Zhang, Fang; Zeng, Raymond J

    2016-11-01

    High-purity propionate production from glycerol in mixed culture fermentation (MCF) induced by high ammonium concentration was investigated. Fed-batch experiments revealed that higher ammonium concentration (>2.9g/L) had simultaneous negative effects on acetate and propionate degradation. Propionate production and yield was up to 22.6g/L and 0.45g COD/g COD glycerol, respectively, with a purity of 96%. Sequential batch experiments demonstrated that the yields of propionate were 0.3±0.05, 0.32±0.01, and 0.34±0.03g COD/g COD at a glycerol concentration of 2.78, 4.38, and 5.56g/L, respectively, and the purity of propionate was 91-100%. Microbial community analysis showed that the phylum Firmicutes dominated the bacterial community at different glycerol concentrations. However, the Methanosaeta population decreased from 46% to 6% when glycerol concentration increased from 2.78 to 5.56g/L, resulting in lower acetate degradation rate. Thus, the present study might provide an alternative option for the production of propionate from glycerol via MCF. PMID:27544916

  2. Safety studies conducted on a proprietary high-purity aloe vera inner leaf fillet preparation, Qmatrix.

    PubMed

    Williams, Lonnie D; Burdock, George A; Shin, Eunju; Kim, Seunghyun; Jo, T H; Jones, Kenneth N; Matulka, Ray A

    2010-06-01

    The aloe vera plant has a long history of safe use for oral and topical applications. This publication describes safety studies conducted on a proprietary high-purity aloe vera inner leaf fillet preparation, Qmatrix. In a 13-week study in rats, Qmatrix was administered via gavage at 0, 500, 1000 and 2000 mg/kg body weight (bw)/day. There were no significant changes in food or water consumption, body weight, serum biochemistry or hematology at any of the doses tested. Sporadic, significant increases were observed in some of the measured urinalysis parameters; however, these variations were not treatment-related, as most were observed only in one sex, not dose-dependent and within historical control values. Organ weights were unaffected, except for a statistically significant, though not dose-dependent, increase in absolute and relative weights of the right kidney in males at 500 and 2000 mg/kg bw/day, respectively. Histopathological analysis revealed no abnormal signs. Qmatrix was non-mutagenic in an Ames test and a chromosomal aberration test at concentrations up to 10,000 microg/plate, and in an in vivo bone marrow micronucleus test at doses up to 5000 mg/kg bw/day. Based on these results, Qmatrix is not genotoxic in vitro or in vivo and; has an oral NOAEL greater than 2000 mg/kg bw/day following 90 days of oral exposure. PMID:20096744

  3. Temperature sensitivity of surface channel effects on high-purity germanium detectors

    NASA Astrophysics Data System (ADS)

    Hull, E. L.; Pehl, R. H.; Madden, N. W.; Luke, P. N.; Cork, C. P.; Malone, D. L.; Xing, J. S.; Komisarcik, K.; Vanderwerp, J. D.; Friesel, D. L.

    1995-02-01

    The temperature sensitivity of surface channel effects on planar high-purity germanium detectors was measured using 60-keV gamma-ray scanning techniques, as part of a radiation damage study. When measured in this manner, the surface effects on most detectors showed extreme temperature sensitivity in the 72-95 K region. The effect of the surface channel increased with increasing temperature to such an extent that the efficiency, as measured by the count rate in the 1332-keV peak from a 60Co source, decreased by a factor of over two in some cases. Since the peak efficiency for the 1332-keV gamma ray decreased as the temperature increased throughout the operating range (72-120 K) the effect of the surface channel must continue to increase beyond the temperature (95 K) at which the 60-keV scan loses its sensitivity because of the strong attenuation of these much lower energy gamma rays. Radiation damage had no measurable effect on the surface characteristics. No correlation between the surface effects and the resolution changes of the 1332-keV peak was observed.

  4. Optimization of extraction of high purity all-trans-lycopene from tomato pulp waste.

    PubMed

    Poojary, Mahesha M; Passamonti, Paolo

    2015-12-01

    The aim of this work was to optimize the extraction of pure all-trans-lycopene from the pulp fractions of tomato processing waste. A full factorial design (FFD) consisting of four independent variables including extraction temperature (30-50 °C), time (1-60 min), percentage of acetone in n-hexane (25-75%, v/v) and solvent volume (10-30 ml) was used to investigate the effects of process variables on the extraction. The absolute amount of lycopene present in the pulp waste was found to be 0.038 mg/g. The optimal conditions for extraction were as follows: extraction temperature 20 °C, time 40 min, a solvent composition of 25% acetone in n-hexane (v/v) and solvent volume 40 ml. Under these conditions, the maximal recovery of lycopene was 94.7%. The HPLC-DAD analysis demonstrated that, lycopene was obtained in the all-trans-configuration at a very high purity grade of 98.3% while the amount of cis-isomers and other carotenoids were limited. PMID:26041168

  5. Multidimensional Study on Spall Behavior of High-Purity Copper Under Sliding Detonation

    NASA Astrophysics Data System (ADS)

    Yang, Yang; Peng, Zhiqiang; Guo, Zhaoliang; Luo, Shuhong; Tang, Tiegang; Hu, Haibo; Zhang, Qingming

    2015-09-01

    The spall behaviors of high-purity copper samples with different heat treatment histories were investigated using optical microscopy and X-ray computer tomography (XRCT). The spall samples were obtained by sliding detonation experiments at low pressures (2 to 4 GPa). It was found that the spall planes created by sliding detonation in this experiment are similar to the spall planes created by plate impact test, except for more secondary damage residual around the main spall plane. The results of damage degree, the shape, and the distributions of voids obtained by the means of metallography (2D) and XRCT (3D) statistics were consistent. For similar microstructure, the maximum damage degree and damage zone width increase with increasing shock stress. Whereas the ranges of voids distribution parallel to the shock stress direction decreases with the increasing of shock stress. For the shock stress is similar, the shape of voids in annealed samples are closed to spheres, their mean flatness is 0.51. The voids in samples with thermo-mechanical treatment histories are sheet like with mean flatness 0.16. The difference in grain size (40 and 9 μm) may be the main reason of such difference.

  6. High-Purity Germanium Spectroscopy at Rates in Excess of 10^{6} Events/s

    SciTech Connect

    VanDevender, Brent A.; Dion, Michael P.; Fast, James E.; Rodriguez, Douglas C.; Taubman, Matthew S.; Wilen, Christopher D.; Wood, Lynn S.; Wright, Michael E.

    2014-10-01

    Abstract—In gamma spectroscopy, a compromise must be made between energy resolution and event-rate capability. Some foreseen nuclear material safeguards applications require a spectrometer with energy resolution typical of high purity germanium (HPGe) detectors, operated at rates up to and exceeding 106 events per second. We report the performance of an HPGe spectrometer adapted to run at such rates. Our system consists of a commercial semi-coaxial HPGe detector, a modified high-voltagerail, resistive-feedback, charge-sensitive preamplifier and a continuous waveform digitizer. Digitized waveforms are analyzed offline with a novel time-variant trapezoidal filter algorithm. Several time-invariant trapezoidal filters are run in parallel and the slowest one not rejected by instantaneous pileup conditions is used to measure each pulse height. We have attained full-widthat- half-maximum energy resolution of less than 8 keV measured at 662 keV with 1:08*106 per second incoming event rate and 38% throughput. An additional constraint on the width of the fast trigger filter removes a significant amount of edge pileup that passes the first pileup cut, reducing throughput to 26%. While better resolution has been reported by other authors, our throughput is over an order of magnitude higher than any other reported HPGe system operated at such an event rate.

  7. Effectiveness of a high purity chlorine dioxide solution in eliminating intracanal Enterococcus faecalis biofilm.

    PubMed

    Herczegh, Anna; Ghidan, Agoston; Friedreich, Dóra; Gyurkovics, Milán; Bendő, Zsolt; Lohinai, Zsolt

    2013-03-01

    We investigated the effectiveness of chlorine dioxide (ClO2) solution in comparison to sodium hypochlorite (NaOCl) and chlorhexidine gluconate (CHX) in the elimination of intracanal Enterococcus faecalis biofilm. Extracted human teeth were inoculated with E. faecalis. After preparation the canals were irrigated with ClO2, NaOCl, CHX or physiologic saline for control. Two and five days later bacterial samples were collected and streaked onto Columbia agar. CFU/mL were counted. The canal walls were investigated by scanning electron microscopy (SEM). The gas phase was investigated in an upside down Petri dish where E. faecalis was inoculated onto blood agar. The irrigants were placed on absorbent paper into the cover. Bacteria were detectable in the control group, but not in any of the irrigants groups. There was a massive reinfection 2 or 5 days after irrigation in the control group. The lowest reinfection was found after the ClO2 treatment. These findings were confirmed by SEM images. We observed an antibacterial effect of ClO2 and NaOCl gas phases on E. faecalis growth, but not of CHX. ClO2 eliminates intracanal biofilm and keeps canal nearly free from bacteria. We suggest the use of high purity ClO2 as a root canal irrigant in clinical practice. PMID:23529300

  8. Isolation of Ubiquitinated Proteins to High Purity from In Vivo Samples.

    PubMed

    Ramirez, Juanma; Min, Mingwei; Barrio, Rosa; Lindon, Catherine; Mayor, Ugo

    2016-01-01

    Ubiquitination pathways are widely used within eukaryotic cells. The complexity of ubiquitin signaling gives rise to a number of problems in the study of specific pathways. One problem is that not all processes regulated by ubiquitin are shared among the different cells of an organism (e.g., neurotransmitter release is only carried out in neuronal cells). Moreover, these processes are often highly temporally dynamic. It is essential therefore to use the right system for each biological question, so that we can characterize pathways specifically in the tissue or cells of interest. However, low stoichiometry, and the unstable nature of many ubiquitin conjugates, presents a technical barrier to studying this modification in vivo. Here, we describe two approaches to isolate ubiquitinated proteins to high purity. The first one favors isolation of the whole mixture of ubiquitinated material from a given tissue or cell type, generating a survey of the ubiquitome landscape for a specific condition. The second one favors the isolation of just one specific protein, in order to facilitate the characterization of its ubiquitinated fraction. In both cases, highly stringent denaturing buffers are used to minimize the presence of contaminating material in the sample. PMID:27613036

  9. Electrical properties of as-grown and proton-irradiated high purity silicon

    NASA Astrophysics Data System (ADS)

    Krupka, Jerzy; Karcz, Waldemar; Kamiński, Paweł; Jensen, Leif

    2016-08-01

    The complex permittivity of as-grown and proton-irradiated samples of high purity silicon obtained by the floating zone method was measured as a function of temperature at a few frequencies in microwave spectrum by employing the quasi TE011 and whispering gallery modes excited in the samples under test. The resistivity of the samples was determined from the measured imaginary part of the permittivity. The resistivity was additionally measured at RF frequencies employing capacitive spectroscopy as well as in a standard direct current experiment. The sample of as-grown material had the resistivity of ∼85 kΩ cm at room temperature. The sample irradiated with 23-MeV protons had the resistivity of ∼500 kΩ cm at 295 K and its behavior was typical of the intrinsic material at room and at elevated temperatures. For the irradiated sample, the extrinsic conductivity region is missing and at temperatures below 250 K hopping conductivity occurs. Thermal cycle hysteresis of the resistivity for the sample of as-grown material is observed. After heating and subsequent cooling of the sample, its resistivity decreases and then slowly (∼50 h) returns to the initial value.

  10. Formation of formaldehyde and peroxides by air oxidation of high purity polyoxyethylene surfactants.

    PubMed

    Bergh, M; Magnusson, K; Nilsson, J L; Karlberg, A T

    1998-07-01

    Ethoxylated alcohols are non-ionic surfactants. The majority are used in household cleaners, laundry products, toiletries and in industrial and institutional cleaners. In previous studies, an ethoxylated non-ionic surfactant of technical quality showed allergenic activity in guinea pig experiments. Chemical analysis revealed a content of formaldehyde, a well-known contact allergen, and peroxides in the surfactant. Most cases of occupational contact dermatitis are considered to be of irritant origin, caused by contact with water and surfactants, but if allergenic autoxidation products can be formed, allergic contact dermatitis cannot be excluded. The sensitizing potential of a chemically defined high purity ethoxylated alcohol was investigated and oxidation under various storage and handling conditions was studied for this and a homologous product. The pure surfactant showed no significant allergenic activity on predictive testing in guinea pigs. When ethoxylated alcohols were stored in the refrigerator, their deterioration was limited. At room temperature, their content of peroxides and formaldehyde increased with time. Levels of formaldehyde above those capable of causing positive patch test reactions were found. Since such surfactants have wide applications, resulting exposure to formaldehyde could be more frequent than is generally realized, contributing to persistence of dermatitis in individuals allergic to formaldehyde. PMID:9686972

  11. a Study on the Role of Sintering Additives for Fabrication of sic Ceramic

    NASA Astrophysics Data System (ADS)

    Yoon, Han Ki; Lee, Young Ju; Cho, Ho Jun; Kim, Tae Gyu

    Silicon carbide (SiC) materials have been extensively studied for high temperature components in advanced energy system and advanced gas turbine. The SiC ceramics have been fabricated by a NITE (Nano Infiltration Transient Eutectic Phase) Process, using Nano-SiC powder. The sintering additives used for forming liquid phase under sintering process, used the sintering additives ratios were an Al2O3-Y2O3 system or add SiO2 contents. A major R&D focus for the SiC ceramics is the production to obtain high purity SiC ceramics. In this study, we investigated roles of the sintering additives(Al2O3:Y2O3) to fabrication of the SiC ceramics. The effects of SiO2 contents and density properties of the SiC ceramics were also investigated. To investigate the effects of SiO2, Al2O3/Y2O3 composition were fixed and then SiO2 ratios were changed as several kinds, and to confirm the effects of sintering additives ratios (Al2O3:Y2O3) they were changed between 4:6 and 6:4 in x wt.%.

  12. Application feasibility of Pb(Zr,Ti)O{sub 3} ceramics fabricated from sol-gel derived powders using titanium and zirconium alkoxides

    SciTech Connect

    Huang, C.L.; Chen, B.H.; Wu, L

    2004-04-02

    It is believed that what may be termed the 'Nanoscaled Century' will lead to a new industrial revolution, particularly in terms of sol-gel methods of assembly for nanostructure devices. A propyl alcohol (1-Pro) based sol-gel chemical has been developed to replace 2-methoxyethanol (MOE), 1,1,1-tris(hydroxymethyl)ethane (THOME) for the fabrication of PbZr{sub 0.53}Ti{sub 0.47}O{sub 3} (PZT) piezoelectric ceramics. This chemical is prepared from sol-gel derived powders that are near to the morphotropic phase boundary (MPB). The pyrochlore phase was still apparent when calcining at 900 deg. C with a shorter calcining time, such as 30 min. However, it disappeared for longer calcining times, for example 3 h or more. From the results of the analysis, PZT ceramics calcinations at 900 deg. C for 4 h, and sintering at 1100 deg. C for 2 h could reach a pyrochlore-free crystal phase with relative density of approximately 7.9 g/cm{sup 3}--close to 98% of the theoretical value. The P-E hysteresis loop, measured by the Sawyer-Tower circuit, revealed that the remanent polarization (P{sub r}) and coercive field (E{sub c}) were 8.54 {mu}C/cm{sup 2} and 15.6 kV/cm, respectively. The vibration modes of the PZT ceramics were between 150 and 1.5 MHz. Morevoer, under such processing conditions the PZT piezoceramics had uniform grain size distribution less than 1 {mu}m and zero temperature coefficient of resonant frequency (TCF). In summary, the PZT ceramics derived from the sol-gel method were confirmed to possess excellent piezoelectric properties. Furthermore, the processing temperatures were scaled down by 100-200 deg. C, compared to conventional oxide reaction. Finally, from an energy-saving viewpoint, this experiment can potentially make a very positive contribution.

  13. Thermoluminescence (TL) properties and x-ray diffraction (XRD) analysis of high purity CaSO{sub 4}:Dy TL material

    SciTech Connect

    Kamarudin, Nadira; Abdullah, Wan Saffiey Wan; Dollah, Mohd Taufik; Hamid, Muhammad Azmi Abdul

    2014-09-03

    This paper presents the characterization and TL properties of dysprosium (Dy) doped calcium sulfate (CaSO{sub 4}) TL material produced by co-precipitation technique with 0.5mol% concentration of dopant. The morphology of the produced TL material was studied using scanning electron microscope (SEM) and the micrograph shows that rectangular parallelepiped shaped crystal with the average of 150 μm in length were produced. The crystallinity of the produced powder was studied using x-ray powder diffraction (XRD). The XRD spectra show that the TL material produced is high purity anhydrite CaSO{sub 4} with average crystallite size of 74 nm with orthorhombic crystal system. The TL behavior of produced CaSO{sub 4}:Dy was studied using a TLD reader after exposure to gamma ray by Co{sup 60} source with the doses of 1,5 and 10 Gy. The glow curve shows linear response with glow peak around 230°C which is desired development in the field of radiation dosimetry.

  14. Formation mechanism and characteristics of lanthanum-doped BaTiO{sub 3} powders and ceramics prepared by the sol–gel process

    SciTech Connect

    Ianculescu, Adelina Carmen; Vasilescu, Catalina Andreea; Crisan, Maria; Raileanu, Malina; Vasile, Bogdan Stefan; Calugaru, Mihai; Crisan, Dorel; Dragan, Nicolae; Curecheriu, Lavinia; Mitoseriu, Liliana

    2015-08-15

    Pure and lanthanum-doped barium titanate nanopowders described by two different formulae, as Ba{sub 1−x}La{sub x}TiO{sub 3}, for lower La concentrations (0 ≤ x ≤ 0.005) and Ba{sub 1−x}La{sub x}Ti{sub 1−x/4}O{sub 3} for higher La concentration (x = 0.025) were prepared by an alkoxide sol–gel method. Single phase compositions were obtained after annealing at 900 °C for 2 h, in air. The increase of the lanthanum content causes structural and morphological changes in the oxide powders, including the evolution of the unit cell from tetragonal toward a cubic symmetry, the particle size decrease and a higher aggregation tendency. SEM investigations of the ceramics sintered at 1300 °C for 4 h indicate significant changes of the microstructural features (strong decrease of the average grain size and increase of the intergranular porosity) with the raise of La amount. Lanthanum addition to barium titanate prepared by sol–gel induces a more significant shift of the Curie temperature toward lower values, than that one reported in literature for ceramics of similar compositions, but processed by the conventional solid state method. The compositions with smaller La amount (x ≤ 0.005) show semiconducting properties at room temperature and high relative dielectric permittivity values, while the undoped ceramics and those doped with higher La content (x = 0.025) are good dielectrics. The ceramic with x = 0.025 exhibits acceptable low losses, a very diffuse ferroelectric–paraelectric transition and Curie temperature closed to the room temperature, being thus susceptible for high tunability applications. - Highlights: • Ba{sub 1−x}La{sub x}TiO{sub 3} (x ≤ 0.005) and Ba{sub 1−x}La{sub x}Ti{sub 1−x/4}O{sub 3} (x = 0.025) were prepared by sol–gel. • Ceramics with x < 0.5 exhibit semiconductor and high dielectric properties. • Ceramic with x = 0.025 exhibits acceptable low losses and diffuse phase transition.

  15. Powder treatment process

    DOEpatents

    Weyand, J.D.

    1988-02-09

    Disclosed are: (1) a process comprising spray drying a powder-containing slurry, the slurry containing a powder constituent susceptible of oxidizing under the temperature conditions of the spray drying, while reducing the tendency for oxidation of the constituent by including as a liquid constituent of the slurry an organic liquid; (2) a process comprising spray drying a powder-containing slurry, the powder having been pretreated to reduce content of a powder constituent susceptible of oxidizing under the temperature conditions of the spray drying, the pretreating comprising heating the powder to react the constituent; and (3) a process comprising reacting ceramic powder, grinding the reacted powder, slurrying the ground powder, spray drying the slurried powder, and blending the dried powder with metal powder. 2 figs.

  16. Powder treatment process

    DOEpatents

    Weyand, John D.

    1988-01-01

    (1) A process comprising spray drying a powder-containing slurry, the slurry containing a powder constituent susceptible of oxidizing under the temperature conditions of the spray drying, while reducing the tendency for oxidation of the constituent by including as a liquid constituent of the slurry an organic liquid; (2) a process comprising spray drying a powder-containing slurry, the powder having been pretreated to reduce content of a powder constituent susceptible of oxidizing under the temperature conditions of the spray drying, the pretreating comprising heating the powder to react the constituent; and (3) a process comprising reacting ceramic powder, grinding the reacted powder, slurrying the ground powder, spray drying the slurried powder, and blending the dried powder with metal powder.

  17. Laser synthesis of palladium alumina composite membranes for production of high purity hydrogen from gasification

    NASA Astrophysics Data System (ADS)

    Singh, Binay; Sheth, Atul C.; Dahotre, Narendra B.

    2006-11-01

    This paper describes a special method of laser-based deposition to synthesize palladium-ceramic composite membranes. Thin film Pd was deposited on a ceramic substrate by Nd-YAG laser irradiation of coating precursor PdCl 2 on γ-alumina substrate. The parameters of the laser processing technique were optimized to synthesize metal-ceramic composite membranes. The physical and chemical characteristics of Pd coated γ-alumina membranes were studied and compared with various other alumina membranes referenced in the literature. Hydrogen permeation experiments were performed in a CO + CO 2 + CH 4 + H 2 environment under typical catalytic steam gasifier exit conditions. The Pd-ceramic composite showed good mechanical and thermal stability and resulted in a hydrogen permeability flux of about 0.061 mol/m 2 s. The activation energy of the Pd membrane was found to be 5.39 kJ/mol in a temperature range of 900-1300 °F.

  18. N-Type delta Doping of High-Purity Silicon Imaging Arrays

    NASA Technical Reports Server (NTRS)

    Blacksberg, Jordana; Hoenk, Michael; Nikzad, Shouleh

    2005-01-01

    A process for n-type (electron-donor) delta doping has shown promise as a means of modifying back-illuminated image detectors made from n-doped high-purity silicon to enable them to detect high-energy photons (ultraviolet and x-rays) and low-energy charged particles (electrons and ions). This process is applicable to imaging detectors of several types, including charge-coupled devices, hybrid devices, and complementary metal oxide/semiconductor detector arrays. Delta doping is so named because its density-vs.-depth characteristic is reminiscent of the Dirac delta function (impulse function): the dopant is highly concentrated in a very thin layer. Preferably, the dopant is concentrated in one or at most two atomic layers in a crystal plane and, therefore, delta doping is also known as atomic-plane doping. The use of doping to enable detection of high-energy photons and low-energy particles was reported in several prior NASA Tech Briefs articles. As described in more detail in those articles, the main benefit afforded by delta doping of a back-illuminated silicon detector is to eliminate a "dead" layer at the back surface of the silicon wherein high-energy photons and low-energy particles are absorbed without detection. An additional benefit is that the delta-doped layer can serve as a back-side electrical contact. Delta doping of p-type silicon detectors is well established. The development of the present process addresses concerns specific to the delta doping of high-purity silicon detectors, which are typically n-type. The present process involves relatively low temperatures, is fully compatible with other processes used to fabricate the detectors, and does not entail interruption of those processes. Indeed, this process can be the last stage in the fabrication of an imaging detector that has, in all other respects, already been fully processed, including metallized. This process includes molecular-beam epitaxy (MBE) for deposition of three layers, including

  19. Electrochemical Characterization of a Solid Oxide Membrane Electrolyzer for Production of High-Purity Hydrogen

    NASA Astrophysics Data System (ADS)

    Pati, Soobhankar; Yoon, Kyung Joong; Gopalan, Srikanth; Pal, Uday B.

    2009-12-01

    A laboratory-scale solid oxide membrane (SOM) steam electrolyzer that can potentially use energy value in waste or any source of carbon or hydrocarbon to produce high-purity hydrogen has been fabricated and evaluated. The SOM electrolyzer comprises an oxygen-ion-conducting yttria-stabilized zirconia (YSZ) electrolyte with a Ni-YSZ cermet cathode coated on one side and liquid-metal anode on the other side. The SOM electrolyzer is operated at 1000 °C by providing a steam-rich gas feed to the Ni-YSZ cermet cathode and feeding a reductant source into the liquid-metal anode. The steam is reduced over the cathode, and oxygen ions are transported through the YSZ electrolyte and are oxidized at the molten metal electrode by the reductant feed. The advantage of SOM electrolyzer over the state-of-the-art solid oxide electrolyzer is its ability to use solid, liquid, and gaseous reductant feed in the liquid-metal anode to reduce the oxygen chemical potential and drive the reaction for hydrogen production. In this study, an electrochemical process model for a SOM electrolyzer was developed. The condition of the liquid-metal anode with reductant was simulated by bubbling humidified hydrogen (3 pct H2O) in the liquid metal, and the electrochemical performance of the SOM electrolyzer was modeled. The experimental data were curve-fitted into the model to identify the various polarization losses. It showed that the performance of the SOM electrolyzer was dominated by the ohmic resistance of the YSZ membrane. Based on the results of this study, future work is needed toward increasing the performance efficiency of the SOM electrolyzer.

  20. High-purity 3D nano-objects grown by focused-electron-beam induced deposition

    NASA Astrophysics Data System (ADS)

    Córdoba, Rosa; Sharma, Nidhi; Kölling, Sebastian; Koenraad, Paul M.; Koopmans, Bert

    2016-09-01

    To increase the efficiency of current electronics, a specific challenge for the next generation of memory, sensing and logic devices is to find suitable strategies to move from two- to three-dimensional (3D) architectures. However, the creation of real 3D nano-objects is not trivial. Emerging non-conventional nanofabrication tools are required for this purpose. One attractive method is focused-electron-beam induced deposition (FEBID), a direct-write process of 3D nano-objects. Here, we grow 3D iron and cobalt nanopillars by FEBID using diiron nonacarbonyl Fe2(CO)9, and dicobalt octacarbonyl Co2(CO)8, respectively, as starting materials. In addition, we systematically study the composition of these nanopillars at the sub-nanometer scale by atom probe tomography, explicitly mapping the homogeneity of the radial and longitudinal composition distributions. We show a way of fabricating high-purity 3D vertical nanostructures of ∼50 nm in diameter and a few micrometers in length. Our results suggest that the purity of such 3D nanoelements (above 90 at% Fe and above 95 at% Co) is directly linked to their growth regime, in which the selected deposition conditions are crucial for the final quality of the nanostructure. Moreover, we demonstrate that FEBID and the proposed characterization technique not only allow for growth and chemical analysis of single-element structures, but also offers a new way to directly study 3D core–shell architectures. This straightforward concept could establish a promising route to the design of 3D elements for future nano-electronic devices.

  1. Gamma background studies for the XENON experiment using a High Purity Germanium Detector

    NASA Astrophysics Data System (ADS)

    Angle, Jesse Isaac

    The XENON Dark Matter Experiment, deployed at the Gran Sasso National Laboratory in Italy on March 2006, is a liquid noble gas detector designed to directly detect dark matter. The detector uses a dual-phase (gas/liquid) Xenon target to search for nuclear recoils associated with nucleus-WIMP interactions. Due to the high sensitivity needed in such an experiment, it is vital to not only reduce the background but to also understand the remaining background so as to aid in the understanding of the data as well as to facilitate upgrades beyond the early Research and Development phases. Many of the components of the XENON10 detector have been screened using a High Purity Germanium Detector known as the GATOR detector. Full analysis of the screening data requires Monte Carlo simulations of the GATOR detector and the sample. Results from this screening will be presented. Using the information obtained from the screening operation, Monte Carlo simulations of the XENON10 electron recoil background will be examined and compared to the actual detector data. The success of this simulation to data comparison indicates that we have a good understanding of the XENON10 gamma background and will be able to make more informed decisions regarding the next stage of detector development. This type of analysis has aided in the selection and design of many of the materials and components being incorporated into the new XENON100 detector, the next generation detector which will be capable of improving the limit set by XENON10 by at least an order of magnitude. (Full text of this dissertation may be available via the University of Florida Libraries web site. Please check http:/ /www.uflib.ufl.edu/etd.html)

  2. High-Purity Nickel Prepared by Electron Beam Melting: Purification Mechanism

    NASA Astrophysics Data System (ADS)

    Zhang, Tao; Shang, Zaiyan; Chen, Ming; He, Jinjiang; Lv, Baoguo; Wang, Xingquan; Xiong, Xiaodong

    2013-12-01

    A bulk cylindrical high-purity nickel ingot, with purity of more than 99.999 pct (5N) in mass, was obtained from the raw nickel with 99.95 pct (3N5) initial purity by virtue of double electron beam melting (EBM). A chemical analysis was performed by using glow discharge mass spectrometry (GDMS) analysis for all elements in the periodic table except carbon, nitrogen, and oxygen, which were tested by the high-performance combustion and fusion method. The major impurities B, Na, Al, Si, P, S, Ca, Ti, Cr, Fe, Cu, Co, Zn, As, Ag, Sb, and Pb showed an excellent removal effect with removal efficiency of more than 85 pct following the double EBMs. Li, Mg, Cl, K, V, Mn, Ga, Ge, Cd, Se, In, Sn, Tl, Au, and Pt were below the detection limit. No significant change in concentration was found for the refractory elements W, Mo, Ta, Nb, and Ir. Be, F, Sc, Se, Br, Rb, Sr, Zr, Y, Ru, Rh, Pd, Te, I, Cs, Ba, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Hf, Re, Os, Hg, Bi, Th, and U were not detectable following the purification as compared to the raw nickel. Gaseous impurities, C, N, O, especially for N, was removed sufficiently. Theoretical calculations for removal efficiency of impurity Fe based on the calculated vapor pressure, activity coefficient, and melt temperature were in good agreement with measured results, and the purification mechanism was ascribed to the evaporation of major impurities and subsequently evacuation by repetitive EBM.

  3. High-purity 3D nano-objects grown by focused-electron-beam induced deposition.

    PubMed

    Córdoba, Rosa; Sharma, Nidhi; Kölling, Sebastian; Koenraad, Paul M; Koopmans, Bert

    2016-09-01

    To increase the efficiency of current electronics, a specific challenge for the next generation of memory, sensing and logic devices is to find suitable strategies to move from two- to three-dimensional (3D) architectures. However, the creation of real 3D nano-objects is not trivial. Emerging non-conventional nanofabrication tools are required for this purpose. One attractive method is focused-electron-beam induced deposition (FEBID), a direct-write process of 3D nano-objects. Here, we grow 3D iron and cobalt nanopillars by FEBID using diiron nonacarbonyl Fe2(CO)9, and dicobalt octacarbonyl Co2(CO)8, respectively, as starting materials. In addition, we systematically study the composition of these nanopillars at the sub-nanometer scale by atom probe tomography, explicitly mapping the homogeneity of the radial and longitudinal composition distributions. We show a way of fabricating high-purity 3D vertical nanostructures of ∼50 nm in diameter and a few micrometers in length. Our results suggest that the purity of such 3D nanoelements (above 90 at% Fe and above 95 at% Co) is directly linked to their growth regime, in which the selected deposition conditions are crucial for the final quality of the nanostructure. Moreover, we demonstrate that FEBID and the proposed characterization technique not only allow for growth and chemical analysis of single-element structures, but also offers a new way to directly study 3D core-shell architectures. This straightforward concept could establish a promising route to the design of 3D elements for future nano-electronic devices. PMID:27454835

  4. Supercapacitor Electrodes Based on High-Purity Electrospun Polyaniline and Polyaniline-Carbon Nanotube Nanofibers.

    PubMed

    Simotwo, Silas K; DelRe, Christopher; Kalra, Vibha

    2016-08-24

    Freestanding, binder-free supercapacitor electrodes based on high-purity polyaniline (PANI) nanofibers were fabricated via a single step electrospinning process. The successful electrospinning of nanofibers with an unprecedentedly high composition of PANI (93 wt %) was made possible due to blending ultrahigh molecular weight poly(ethylene oxide) (PEO) with PANI in solution to impart adequate chain entanglements, a critical requirement for electrospinning. To further enhance the conductivity and stability of the electrodes, a small concentration of carbon nanotubes (CNTs) was added to the PANI/PEO solution prior to electrospinning to generate PANI/CNT/PEO nanofibers (12 wt % CNTs). Scanning electron microscopy (SEM) and Brunauer-Emmett-Teller (BET) porosimetry were conducted to characterize the external morphology of the nanofibers. The electrospun nanofibers were further probed by transmission electron microscopy (TEM), X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FT-IR). The electroactivity of the freestanding PANI and PANI/CNT nanofiber electrodes was examined using cyclic voltammetry, galvanostatic charge-discharge, and electrochemical impedance spectroscopy. Competitive specific capacitances of 308 and 385 F g(-1) were achieved for PANI and PANI-CNT based electrodes, respectively, at a current density of 0.5 A g(-1). Moreover, specific capacitance retentions of 70 and 81.4% were observed for PANI and PANI-CNT based electrodes, respectively, after 1000 cycles. The promising electrochemical performance of the fabricated electrodes, we believe, stems from the porous 3-D electrode structure characteristic of the nonwoven interconnected nanostructures. The interconnected nanofiber network facilitates efficient electron conduction while the inter- and intrafiber porosity enable excellent electrolyte penetration within the polymer matrix, allowing fast ion transport to the active sites. PMID:27467445

  5. In vitro studies of composite bone filler based on poly(propylene fumarate) and biphasic α-tricalcium phosphate/hydroxyapatite ceramic powder.

    PubMed

    Wu, Chang-Chin; Yang, Kai-Chiang; Yang, Shu-Hua; Lin, Min-Huei; Kuo, Tzong-Fu; Lin, Feng-Huei

    2012-04-01

    While many different filler materials have been applied in vertebral augmentation procedures, none is perfect in all biomechanical and biological characteristics. To minimize possible shortages, we synthesized a new biodegradable, injectable, and premixed composite made from poly(propylene fumarate) (PPF) and biphasic α-tricalcium phosphate (α-TCP)/hydroxyapatite (HAP) ceramics powder and evaluated the material properties of the compound in vitro. We mixed the PPF cross-linked by N-vinyl pyrrolidinone and biphasic α-TCP/HAP powder in different ratios with benzoyl peroxide as an initiator. The setting time and temperature were recorded, although they could be manipulated by modulating the concentrations of hydroquinone and N,N-dimethyl-p-toluidine. Degradation, cytocompatibility, mechanical properties, and radiopacity were analyzed after the composites were cured by a cylindrical shape. We also compared the study materials with poly(methyl methacrylate) (PMMA) and PPF with pure HAP particles. Results showed that lower temperature during curing process (38-44°C), sufficient initial mechanical compressive fracture strength (61.1±3.7MPa), and gradual degradation were observed in the newly developed bone filler. Radiopacity in Hounsfield units was similar to PMMA as determined by computed tomography scan. Both pH value variation and cytotoxicity were within biological tolerable limits based on the biocompatibility tests. Mixtures with 70% α-TCP/HAP powder were superior to other groups. This study indicated that a composite of PPF and biphasic α-TCP/HAP powder is a promising, premixed, injectable biodegradable filler and that a mixture containing 70% α-TCP/HAP exhibits the best properties. PMID:22145803

  6. Fabrication Of Ceramic Mats

    NASA Technical Reports Server (NTRS)

    Collins, Earl R., Jr.

    1991-01-01

    Process to make mats of fine zirconia filaments proposed. Ceramic mats formed by sintering mats of partially dried filaments extruded from slurry of ceramic powder, binder, and solvent. Mats of fine zirconia fibers easier to ball-mill than commercially available zirconia powder.

  7. The synthesis, characterization and formation chemistry of Si-C-N-O-M ceramic and composite powders. Final technical report

    SciTech Connect

    Mariam, Y.H.

    1998-08-01

    Brief summaries are given for the work in each of the following areas: (1) general pattern of behavior in the conversion processes of SiNC precursors; (2) thermal and oxidative stability of SiNC ceramics; and (3) modification of PMVSEDA(poly(methylvinyl)silylethylenediamine) with borane-dimethyl sulfide.

  8. Dry pressing technical ceramics

    SciTech Connect

    Lewis, W.A. Jr.

    1996-04-01

    Dry pressing of technical ceramics is a fundamental method of producing high-quality ceramic components. The goals of dry pressing technical ceramics are uniform compact size and green density, consistent part-to-part green density and defect-free compact. Dry pressing is the axial compaction of loosely granulated dry ceramic powders (< 3% free moisture) within a die/punch arrangement. The powder, under pressure, conforms to the specific shape of the punch faces and die. Powder compaction occurs within a rigid-walled die and usually between a top and bottom punch. Press configurations include anvil, rotary, multiple-punch and multiple-action.

  9. A Pilot Study of Ceramic Powder Far-Infrared Ray Irradiation (cFIR) on Physiology: Observation of Cell Cultures and Amphibian Skeletal Muscle.

    PubMed

    Leung, Ting-Kai; Lee, Chi-Ming; Tsai, Shih-Yin; Chen, Yi-Chien; Chao, Jo-Shui

    2011-08-31

    The purpose of this research was to assess the potential for far-infrared ray irradiation from ceramic powder to improve exercise performance at room temperature. We designed experiments with murine myoblast cells (C2C12) to study the effect of cFIR irradiation on cell viability and lactate dehydrogenase release under H2O2-mediated oxidative stress and evaluated intracellular levels of nitric oxide and calmodulin. We also used electro-stimulation of amphibian skeletal muscle. Our results show that cFIR strengthened C2C12 under oxidative stress and delayed onset of fatigue induced by muscle contractions. We discuss possible mechanisms including anti-oxidation and prevention of acid build-up in muscle tissue based, and expect to see more applications of cFIR in the future. PMID:22129823

  10. Alumina-based ceramic composite

    DOEpatents

    Alexander, Kathleen B.; Tiegs, Terry N.; Becher, Paul F.; Waters, Shirley B.

    1996-01-01

    An improved ceramic composite comprising oxide ceramic particulates, nonoxide ceramic particulates selected from the group consisting of carbides, borides, nitrides of silicon and transition metals and mixtures thereof, and a ductile binder selected from the group consisting of metallic, intermetallic alloys and mixtures thereof is described. The ceramic composite is made by blending powders of the ceramic particulates and the ductile to form a mixture and consolidating the mixture of under conditions of temperature and pressure sufficient to produce a densified ceramic composite.

  11. Preparation of Nanocrystalline Powders of ZrO2, Stabilized by Y2O3 Dobs for Ceramics

    NASA Astrophysics Data System (ADS)

    Petrunin, V. F.; Korovin, S. A.

    The purpose of this study was to develop a synthesis conditions and produce samples of nanocrystalline zirconia powder in a high-temperature phase state. To increase the stability of this state at room temperature, Y2O3 was used as a dop in the two-stages chemical method including coprecipitation mixture of the corresponding hydroxides and air drying. To reduce agglomeration of nanoparticles during heat treatment of precursors the microwave oven instead of a muffle was used. Different characterisation methods have been used to determine that the obtained powders are nano-scale corresponds to a high-temperature tetragonal phase of ZrO2. It is shown that such nanocrystalline powders may be used to produce highly-dense nanoceramics.

  12. Inactivation and clearance of viruses during the manufacture of high purity factor IX.

    PubMed

    Johnston, A; Macgregor, A; Borovec, S; Hattarki, M; Stuckly, K; Anderson, D; Goss, N H; Oates, A; Uren, E

    2000-09-01

    Haemophilia is a bleeding disorder characterised by a deficiency in Factor IX. Replacement therapy in the form of a Factor IX concentrate is a widely accepted practice. In this paper we describe a double virus inactivated chromatographic process for producing a high purity Factor IX product, MonoFIX((R))-VF. The process involves separation of the prothrombin complex by cryoprecipitation, fraction I precipitation and DEAE-cellulose adsorption, further ion-exchange chromatography of crude Factor IX, followed by solvent/detergent treatment. Heparin affinity chromatography is then used to further purify Factor IX. Final nanofiltration is sequential through 35 nm then 15 nm membrane filters. The principal virus inactivation/removal steps are solvent/detergent treatment and nanofiltration and the partitioning of relevant and model viruses provides further reduction in virus load through the production process.Solvent/detergent treatment was shown to achieve log reduction factors of 4.5 for HIV-1, 5.1 for Sindbis virus, 6.1 for vesicular stomatitis virus (VSV), 5.1 for bovine viral diarrhoea virus (BVDV) and 5.3 for pseudorabies virus (PRV). BVDV is a model for hepatitis C virus (HCV), and pseudorabies virus (PRV), like hepatitis B virus (HBV) is an enveloped DNA virus. Using scaled down models of the production process, we have also demonstrated the neutralization/partitioning of at least 6 logs of hepatitis A virus (HAV) during cryoprecipitation, Fraction I precipitation, and the DEAE adsorption and elution step, and a further 1.6 log reduction in HAV load as a result of heparin affinity chromatography. The log reduction factors for HAV as a result of the second ion-exchange chromatography step and as a result of enhanced neutralisation associated with solvent/detergent treatment were not significant. Nanofiltration was shown to contribute a further log reduction factor of 6.7 for HAV and 5.8 for BVDV indicating that log reduction factors of this order would be obtained

  13. High-Purity Aluminum Magnet Technology for Advanced Space Transportation Systems

    NASA Technical Reports Server (NTRS)

    Goodrich, R. G.; Pullam, B.; Rickle, D.; Litchford, R. J.; Robertson, G. A.; Schmidt, D. D.; Cole, John (Technical Monitor)

    2001-01-01

    Basic research on advanced plasma-based propulsion systems is routinely focused on plasmadynamics, performance, and efficiency aspects while relegating the development of critical enabling technologies, such as flight-weight magnets, to follow-on development work. Unfortunately, the low technology readiness levels (TRLs) associated with critical enabling technologies tend to be perceived as an indicator of high technical risk, and this, in turn, hampers the acceptance of advanced system architectures for flight development. Consequently, there is growing recognition that applied research on the critical enabling technologies needs to be conducted hand in hand with basic research activities. The development of flight-weight magnet technology, for example, is one area of applied research having broad crosscutting applications to a number of advanced propulsion system architectures. Therefore, NASA Marshall Space Flight Center, Louisiana State University (LSU), and the National High Magnetic Field Laboratory (NHMFL) have initiated an applied research project aimed at advancing the TRL of flight-weight magnets. This Technical Publication reports on the group's initial effort to demonstrate the feasibility of cryogenic high-purity aluminum magnet technology and describes the design, construction, and testing of a 6-in-diameter by 12-in-long aluminum solenoid magnet. The coil was constructed in the machine shop of the Department of Physics and Astronomy at LSU and testing was conducted in NHMFL facilities at Florida State University and at Los Alamos National Laboratory. The solenoid magnet was first wound, reinforced, potted in high thermal conductivity epoxy, and bench tested in the LSU laboratories. A cryogenic container for operation at 77 K was also constructed and mated to the solenoid. The coil was then taken to NHMFL facilities in Tallahassee, FL. where its magnetoresistance was measured in a 77 K environment under steady magnetic fields as high as 10 T. In

  14. Diffusion bonding and brazing of high purity copper for linear collider accelerator structures

    NASA Astrophysics Data System (ADS)

    Elmer, J. W.; Klingmann, J.; van Bibber, K.

    2001-05-01

    Diffusion bonding and brazing of high purity copper were investigated to develop procedures for joining precision machined copper components for the Next Linear Collider (NLC). Diffusion bonds were made over a range of temperatures from 400 °C to 1000 °C, under two different loading conditions [3.45 kPa (0.5 psi) and 3.45 MPa (500 psi)], and on two different diamond machined surface finishes. Brazes were made using pure silver, pure gold, and gold-nickel alloys, and different heating rates produced by both radiation and induction heating. Braze materials were applied by both physical vapor deposition (PVD) and conventional braze alloy shims. Results of the diffusion bonding experiments showed that bond strengths very near that of the copper base metal could be made at bonding temperatures of 700 °C or higher at 3.45 MPa bonding pressure. At lower temperatures, only partial strength diffusion bonds could be made. At low bonding pressures (3.45 kPa), full strength bonds were made at temperatures of 800 °C and higher, while no bonding (zero strength) was observed at temperatures of 700 °C and lower. Observations of the fracture surfaces of the diffusion bonded samples showed the effects of surface finish on the bonding mechanism. These observations clearly indicate that bonding began by point asperity contact, and flatter surfaces resulted in a higher percentage of bonded area under similar bonding conditions. Results of the brazing experiments indicated that pure silver worked very well for brazing under both conventional and high heating rate scenarios. Similarly, pure silver brazed well for both the PVD layers and the braze alloy shims. The gold and gold-containing brazes had problems, mainly due to the high diffusivity of gold in copper. These problems led to the necessity of overdriving the temperature to ensure melting, the presence of porosity in the joint, and very wide braze joints. Based on the overall findings of this study, a two-step joining method

  15. Analysis of high-purity germanium dioxide by ETV-ICP-AES with preliminary concentration of trace elements.

    PubMed

    Medvedev, Nickolay S; Shaverina, Anastasiya V; Tsygankova, Alphiya R; Saprykin, Anatoly I

    2016-08-01

    The paper presents a combined technique of germanium dioxide analysis by inductively coupled plasma atomic emission spectrometry (ICP-AES) with preconcentration of trace elements by distilling off matrix and electrothermal (ETV) introduction of the trace elements concentrate into the ICP. Evaluation of metrological characteristics of the developed technique of high-purity germanium dioxide analysis was performed. The limits of detection (LODs) for 25 trace elements ranged from 0.05 to 20ng/g. The accuracy of proposed technique is confirmed by "added-found" («or spiking») experiment and comparing the results of ETV-ICP-AES and ICP-AES analysis of high purity germanium dioxide samples. PMID:27216693

  16. Equilibrium between titanium ions and high-purity titanium electrorefining in a NaCl-KCl melt

    NASA Astrophysics Data System (ADS)

    Song, Jian-xun; Wang, Qiu-yu; Hu, Guo-jing; Zhu, Xiao-bo; Jiao, Shu-qiang; Zhu, Hong-min

    2014-07-01

    TiCl x ( x = 2.17) was prepared by using titanium sponge to reduce the concentration of TiCl4 in a NaCl-KCl melt under negative pressure. The as-prepared NaCl-KCl-TiCl x melt was employed as the electrolyte, and two parallel crude titanium plates and one high-purity titanium plate were used as the anode and cathode, respectively. A series of electrochemical tests were performed to investigate the influence of electrolytic parameters on the current efficiency and quality of cathodic products. The results indicated that the quality of cathodic products was related to the current efficiency, which is significantly dependent on the current density and the initial concentration of titanium ions. The significance of this study is the attainment of high-purity titanium with a low oxygen content of 30 × 10-6.

  17. Production of high-purity isomalto-oligosaccharides syrup by the enzymatic conversion of transglucosidase and fermentation of yeast cells.

    PubMed

    Pan, Yen-Chung; Lee, Wen-Chien

    2005-03-30

    A method for the production of high-purity isomalto-oligosaccharides (IMO) involving the transglucosylation by transglucosidase and yeast fermentation was proposed. The starch of rice crumbs was enzymatically liquefied and saccharified, and then converted to low-purity IMO syrup by transglucosylation. The low-purity IMO produced either from rice crumbs or tapioca flour as the starch source could be effectively converted to high-purity IMO by yeast fermentation to remove the digestible sugars including glucose, maltose, and maltotriose. Both Saccharomyces carlsbergensis and Saccharomyces cerevisiae were able to ferment glucose in the IMO syrup. Cells of S. carlsbergensis harvested from the medium of malt juice were also able to ferment maltose and maltotriose. A combination of these two yeasts or S. carlsbergensis alone could be used to totally remove the digestible sugars in the IMO, coupled with the production of ethanol. The resultant high-purity IMO, including mainly isomaltose, panose, and isomaltotriose made up more than 98% w/w of the total sugars after a 3-day fermentation. When the low-purity IMO was produced from the starch of tapioca flour, 3-day fermentation under the same conditions resulted in IMO with purity lower than that from rice crumbs. For low-purity IMO from rice crumbs, fermentation with washed S. carlsbergensis cells harvested at log phase was the most effective. However, for the low-purity IMO from tapioca flour, incubation with S. cerevisiae for the first 24 h and then supplementing with an equal amount of S. carlsbergensis cells for further fermentation was the most effective approach for producing high-purity IMO. PMID:15672377

  18. Application of multisection packing concept to sorption-enhanced steam methane reforming reaction for high-purity hydrogen production

    NASA Astrophysics Data System (ADS)

    Lee, Chan Hyun; Mun, Sungyong; Lee, Ki Bong

    2015-05-01

    Hydrogen has been gaining popularity as a new clean energy carrier, and bulk hydrogen production is achieved through the steam methane reforming (SMR) reaction. Since hydrogen produced via the SMR reaction contains large amounts of impurities such as unreacted reactants and byproducts, additional purification steps are needed to produce high-purity hydrogen. By applying the sorption-enhanced reaction (SER), in which catalytic reaction and CO2 byproduct removal are carried out simultaneously in a single reactor, high-purity hydrogen can be directly produced. Additionally, the thermodynamic limitation of conventional SMR reaction is circumvented, and the SMR reaction process becomes simplified. To improve the performance of the SER, a multisection packing concept was recently proposed. In this study, the multisection packing concept is experimentally demonstrated by applying it to a sorption-enhanced SMR (SE-SMR) reaction. The experimental results show that the SE-SMR reaction is significantly influenced by the reaction temperature, owing to the conflicting dependence of the reaction rate and the CO2 sorption uptake on the reaction temperature. Additionally, it is confirmed that more high-purity hydrogen (<10 ppm of CO) can be produced by applying the multisection packing concept to the SE-SMR reactions operated at sufficiently high temperatures where the SMR reaction is not limited by rate.

  19. Intra- and inter-tube exciton relaxation dynamics in high purity semiconducting and metallic single-walled carbon nanotubes

    NASA Astrophysics Data System (ADS)

    Ichida, Masao; Saito, Shingo; Miyata, Yasumitsu; Yanagi, Kazuhiro; Kataura, Hiromichi; Ando, Hiroaki

    2013-02-01

    We have measured the exciton and carrier dynamics in the high purity semiconducting (S-) and metallic (M-) single-walled carbon nanotubes (SWNTs) in the isolated and aggregated (bundled) forms. The exciton relaxation decay times are measured by using the pump-probe spectroscopy. For bundled samples, the relaxation time becomes shorter than that for isolated SWNTs sample, because of the existence of inter-tube relaxation. We estimate the relaxation rates from S-SWNT to S-SWNT and S-SWNT to M-SWNT using the decay times for isolated SWNTs, high purity S-SWNTs bundle, and doped S-SWNTs in high purity M-SWNTs bundle. For S-SWNTs, inter-tube relaxation plays an important role in the relaxation dynamics. However, for M-SWNTs, the inter-tube relaxation is not so important, and the transition energy and intensity of exciton in M-SWNTs is strongly affected by the photoexcited carriers which plays like as photo doping.

  20. Gelcasting superalloy powders

    SciTech Connect

    Janney, M.A.

    1995-12-31

    Gelcasting is a process for forming inorganic powders into complex shapes. It was originally developed for ceramic powders. A slurry of powder and a monomer solution is poured in to mold and polymerized in-situ to form gelled parts. Typically, only 2-4 wt % Polymer is used. The process has both aqueous and nonaqueous versions. Gelcasting is a generic process and has been used to produce ceramic parts from over a dozen different ceramic compositions ranging from alumina-based refractories to high-performance silicon nitride. Recently, gelcasting has been applied to forming superalloy powders into complex shapes. This application has posed several challenges not previously encountered in ceramics. In particular, problems were caused by the larger particle size and the higher density of the particles. Additional problems were encountered with binder removal. How these problems were overcome will be described.

  1. Synthesis and processing of monosized oxide powders

    DOEpatents

    Barringer, E.A.; Fegley, M.B. Jr.; Bowen, H.K.

    1985-09-24

    Uniform-size, high-purity, spherical oxide powders are formed by hydrolysis of alkoxide precursors in dilute alcoholic solutions. Under controlled conditions (concentrations of 0.03 to 0.2 M alkoxide and 0.2 to 1.5 M water, for example) oxide particles on the order of about 0.05 to 0.7 microns can be produced. Methods of doping such powders and forming sinterable compacts are also disclosed. 6 figs.

  2. Synthesis and processing of monosized oxide powders

    DOEpatents

    Barringer, Eric A.; Fegley, Jr., M. Bruce; Bowen, H. Kent

    1985-01-01

    Uniform-size, high-purity, spherical oxide powders are formed by hydrolysis of alkoxide precursors in dilute alcoholic solutions. Under controlled conditions (concentrations of 0.03 to 0.2 M alkoxide and 0.2 to 1.5 M water, for example) oxide particles on the order of about 0.05 to 0.7 micron can be produced. Methods of doping such powders and forming sinterable compacts are also disclosed.

  3. Fabrication process development for high-purity germanium radiation detectors with amorphous semiconductor contacts

    NASA Astrophysics Data System (ADS)

    Looker, Quinn

    High-purity germanium (HPGe) radiation detectors are well established as a valuable tool in nuclear science, astrophysics, and nuclear security applications. HPGe detectors excel in gamma-ray spectroscopy, offering excellent energy resolution with large detector sizes for high radiation detection efficiency. Although a robust fabrication process has been developed, improvement is needed, especially in developing electrical contact and surface passivation technology for position-sensitive detectors. A systematic study is needed to understand how the detector fabrication process impacts detector performance and reliability. In order to provide position sensitivity, the electrical contacts are segmented to form multiple electrodes. This segmentation creates new challenges in the fabrication process and warrants consideration of additional detector effects related to the segmentation. A key area of development is the creation of the electrical contacts in a way that enables reliable operation, provides low electronic noise, and allows fine segmentation of electrodes, giving position sensitivity for radiation interactions in the detector. Amorphous semiconductor contacts have great potential to facilitate new HPGe detector designs by providing a thin, high-resistivity surface coating that is the basis for electrical contacts that block both electrons and holes and can easily be finely segmented. Additionally, amorphous semiconductor coatings form a suitable passivation layer to protect the HPGe crystal surface from contamination. This versatility allows a simple fabrication process for fully passivated, finely segmented detectors. However, the fabrication process for detectors with amorphous semiconductors is not as highly developed as for conventional technologies. The amorphous semiconductor layer properties can vary widely based on how they are created and these can translate into varying performance of HPGe detectors with these contacts. Some key challenges include

  4. Lightweight ceramic insulation and method

    NASA Technical Reports Server (NTRS)

    Green, David J. (Inventor)

    1990-01-01

    A process is disclosed for manufacturing a low density ceramic powder which can be formed to make a lightweight material for insulation or other construction. The ceramic product made from the process has a final density of less than 25 to about 1 percent of the theoretical weight of the ceramic powder. The ceramic product is lightweight and can be made to withstand high temperatures greater than 1400 C.

  5. High Purity Hydrogen Production with In-Situ Carbon Dioxide and Sulfur Capture in a Single Stage Reactor

    SciTech Connect

    Nihar Phalak; Shwetha Ramkumar; Daniel Connell; Zhenchao Sun; Fu-Chen Yu; Niranjani Deshpande; Robert Statnick; Liang-Shih Fan

    2011-07-31

    Enhancement in the production of high purity hydrogen (H{sub 2}) from fuel gas, obtained from coal gasification, is limited by thermodynamics of the water gas shift (WGS) reaction. However, this constraint can be overcome by conducting the WGS in the presence of a CO{sub 2}-acceptor. The continuous removal of CO{sub 2} from the reaction mixture helps to drive the equilibrium-limited WGS reaction forward. Since calcium oxide (CaO) exhibits high CO{sub 2} capture capacity as compared to other sorbents, it is an ideal candidate for such a technique. The Calcium Looping Process (CLP) developed at The Ohio State University (OSU) utilizes the above concept to enable high purity H{sub 2} production from synthesis gas (syngas) derived from coal gasification. The CLP integrates the WGS reaction with insitu CO{sub 2}, sulfur and halide removal at high temperatures while eliminating the need for a WGS catalyst, thus reducing the overall footprint of the hydrogen production process. The CLP comprises three reactors - the carbonator, where the thermodynamic constraint of the WGS reaction is overcome by the constant removal of CO{sub 2} product and high purity H{sub 2} is produced with contaminant removal; the calciner, where the calcium sorbent is regenerated and a sequestration-ready CO{sub 2} stream is produced; and the hydrator, where the calcined sorbent is reactivated to improve its recyclability. As a part of this project, the CLP was extensively investigated by performing experiments at lab-, bench- and subpilot-scale setups. A comprehensive techno-economic analysis was also conducted to determine the feasibility of the CLP at commercial scale. This report provides a detailed account of all the results obtained during the project period.

  6. Determination of rare earth impurities in high purity samarium oxide using inductively coupled plasma mass spectrometry after extraction chromatographic separation

    NASA Astrophysics Data System (ADS)

    Zhang, Xinquan; Liu, Jinglei; Yi, Yong; Liu, Yonglin; Li, Xiang; Su, Yaqin; Lin, Ping

    2007-01-01

    A method for the determination of trace of 14 rare earth elements (REEs) as impurities in high purity samarium oxide (Sm2O3) using inductively coupled plasma mass spectrometry (ICP-MS) was described. Analytes, such as La, Ce, Pr, Nd, Eu, Gd, Tb, Lu and Y were measured without Sm matrix separation because of no interference problems occurring that could affect the analysis of these elements. On the other hand, analytes, such as Dy, Ho, Er, Tm and Yb were carried out after Sm matrix being eliminated completely by means of 2-ethylhexyl hydrogen-ethylhexy phosphonate (EHEHP) extraction chromatographic separation. The inherent problem associated with matrix-induced suppression was effectively compensated with spiking In as internal standard element and the mass spectra isobaric interferences of atomic and molecular ions arose from Sm matrix had been overcome after the removal of Sm matrix. The limits of quantitations (LOQ) for 14 REEs impurities were from 0.01 to 0.07 [mu]g g-1 together with the recoveries of spiking sample of 14 REEs were found to be in the range of 85-110% and the proposed method precision was less than 5%. A synthetic standard Sm2O3 sample with well-known 14 REEs concentrations was prepared and analysed in order to prove the accuracy and precision of the proposed method together with another high purity Sm2O3 was also measured using ICP-MS. The methodology had been found to be suitable for the determination of trace of 14 REEs in 99.999-99.9999% high purity Sm2O3.

  7. Magnetic and magnetothermal properties and the magnetic phase diagram of high purity single crystalline terbium along the easy magnetization direction

    SciTech Connect

    Zverev, V. I.; Tishin, A. M.; Chernyshov, A. S.; Mudryk, Ya; Gschneidner Jr., Karl A.; Pecharsky, Vitalij K.

    2014-01-21

    The magnetic and magnetothermal properties of a high purity terbium single crystal have been re-investigated from 1.5 to 350 K in magnetic fields ranging from 0 to 75 kOe using magnetization, ac magnetic susceptibility and heat capacity measurements. The magnetic phase diagram has been refined by establishing a region of the fan-like phase broader than reported in the past, by locating a tricritical point at 226 K, and by a more accurate definition of the critical fields and temperatures associated with the magnetic phases observed in Tb.

  8. Gas chromatographic separation of nitrogen, oxygen, argon, and carbon monoxide using custom-made porous polymers from high purity divinylbenzene

    NASA Technical Reports Server (NTRS)

    Pollock, G. E.; Ohara, D.; Hollis, O. L.

    1984-01-01

    Existing porous polymers were surveyed for their ability to separate the subject gases. Certain products that showed more promise than others were synthesized and the existing synthetic procedures studied and modified to produce new polymers with enhanced ability to separate the subject gases. Evaluation of the porous polymers was carried out practically by gas chromatography at ambient temperature. The modified synthetic procedures were somewhat simpler than the originals. The new porous polymers made with high purity divinylbenzene enabled use of shorter columns to obtain the separations desired.

  9. Using standard calibrated geometries to characterize a coaxial high purity germanium gamma detector for Monte Carlo simulations

    SciTech Connect

    Graaf, E. R. van der Dendooven, P.; Brandenburg, S.

    2014-06-15

    A detector model optimization procedure based on matching Monte Carlo simulations with measurements for two experimentally calibrated sample geometries which are frequently used in radioactivity measurement laboratories results in relative agreement within 5% between simulated and measured efficiencies for a high purity germanium detector. The optimization procedure indicated that the increase in dead layer thickness is largely responsible for a detector efficiency decrease in time. The optimized detector model allows Monte Carlo efficiency calibration for all other samples of which the geometry and bulk composition is known. The presented method is a competitive and economic alternative to more elaborate detector scanning methods and results in a comparable accuracy.

  10. Preparation of uniform nanoparticles of ultra-high purity metal oxides, mixed metal oxides, metals, and metal alloys

    DOEpatents

    Woodfield, Brian F.; Liu, Shengfeng; Boerio-Goates, Juliana; Liu, Qingyuan; Smith, Stacey Janel

    2012-07-03

    In preferred embodiments, metal nanoparticles, mixed-metal (alloy) nanoparticles, metal oxide nanoparticles and mixed-metal oxide nanoparticles are provided. According to embodiments, the nanoparticles may possess narrow size distributions and high purities. In certain preferred embodiments, methods of preparing metal nanoparticles, mixed-metal nanoparticles, metal oxide nanoparticles and mixed-metal nanoparticles are provided. These methods may provide tight control of particle size, size distribution, and oxidation state. Other preferred embodiments relate to a precursor material that may be used to form nanoparticles. In addition, products prepared from such nanoparticles are disclosed.

  11. Bioactivity and cell proliferation in radiopaque gel-derived CaO-P2O5-SiO2-ZrO2 glass and glass-ceramic powders.

    PubMed

    Montazerian, Maziar; Yekta, Bijan Eftekhari; Marghussian, Vahak Kaspari; Bellani, Caroline Faria; Siqueira, Renato Luiz; Zanotto, Edgar Dutra

    2015-10-01

    In this study, 10 mol% ZrO2 was added to a 27CaO-5P2O5-68SiO2 (mol%) base composition synthesized via a simple sol-gel method. This composition is similar to that of a frequently investigated bioactive gel-glass. The effects of ZrO2 on the in vitro bioactivity and MG-63 cell proliferation of the glass and its derivative polycrystalline (glass-ceramic) powder were investigated. The samples were characterized using thermo-gravimetric and differential thermal analysis (TG/DTA), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM) coupled to energy dispersive X-ray spectroscopy (EDS). Release of Si, Ca, P and Zr into simulated body fluid (SBF) was determined by inductively coupled plasma (ICP). Upon heat treatment at 1000 °C, the glass powder crystallized into an apatite-wollastonite-zirconia glass-ceramic powder. Hydroxycarbonate apatite (HCA) formation on the surface of the glass and glass-ceramic particles containing ZrO2 was confirmed by FTIR and SEM. Addition of ZrO2 to the base glass composition decreased the rate of HCA formation in vitro from one day to three days, and hence, ZrO2 could be employed to control the rate of apatite formation. However, the rate of HCA formation on the glass-ceramic powder containing ZrO2 crystal was equal to that in the base glassy powder. Tests with a cultured human osteoblast-like MG-63 cells revealed that the glass and glass-ceramic materials stimulated cell proliferation, indicating that they are biocompatible and are not cytotoxic in vitro. Moreover, zirconia clearly increased osteoblast proliferation over that of the Zr-free samples. This increase is likely associated with the lower solubility of these samples and, consequently, a smaller variation in the media pH. Despite the low solubility of these materials, bioactivity was maintained, indicating that these glassy and polycrystalline powders are potential candidates for bone graft substitutes and bone cements with

  12. Functional properties of BaTiO3-Ni0.5Zn0.5Fe2O4 magnetoelectric ceramics prepared from powders with core-shell structure

    NASA Astrophysics Data System (ADS)

    Curecheriu, L. P.; Buscaglia, M. T.; Buscaglia, V.; Mitoseriu, L.; Postolache, P.; Ianculescu, A.; Nanni, P.

    2010-05-01

    In the present work, diphasic ceramic composites with core-shell nanostructures formed by Ni0.50Zn0.50Fe2O4 core and BaTiO3 shell were investigated. Their properties were compared with those of composites prepared by coprecipitation. The core-shell structure was confirmed by microstructural powder analysis. Homogeneous microstructures with a good phase mixing and percolated dielectric phase by the magnetic one were obtained from coprecipitated powders. Less homogeneous microstructures resulted in ceramics produced from the powder prepared by core-shell method, with isolated small ferrite grains besides large ferrite aggregates embedded into the BaTiO3 matrix. Both the ferroelectric and magnetic phases preserve their basic properties in bulk composite form. However, important differences in the dielectric relaxation and conduction mechanisms were found as result of the microstructural difference. Extrinsic contributions play important roles in modifying the electric properties in both ceramics, causing space charge effect, Maxwell-Wagner relaxations and hopping conductivity, mainly due to the ferrite low resistivity phase. The conductivity and dielectric modulus spectra analysis allowed to identify different polaron contributions associated with the microstructural differences. It results that by using the core-shell method, improved dielectric properties and limited hopping contributions can be realized.

  13. Functional properties of BaTiO{sub 3}-Ni{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} magnetoelectric ceramics prepared from powders with core-shell structure

    SciTech Connect

    Curecheriu, L. P.; Mitoseriu, L.; Postolache, P.; Buscaglia, M. T.; Buscaglia, V.; Ianculescu, A.; Nanni, P.

    2010-05-15

    In the present work, diphasic ceramic composites with core-shell nanostructures formed by Ni{sub 0.50}Zn{sub 0.50}Fe{sub 2}O{sub 4} core and BaTiO{sub 3} shell were investigated. Their properties were compared with those of composites prepared by coprecipitation. The core-shell structure was confirmed by microstructural powder analysis. Homogeneous microstructures with a good phase mixing and percolated dielectric phase by the magnetic one were obtained from coprecipitated powders. Less homogeneous microstructures resulted in ceramics produced from the powder prepared by core-shell method, with isolated small ferrite grains besides large ferrite aggregates embedded into the BaTiO{sub 3} matrix. Both the ferroelectric and magnetic phases preserve their basic properties in bulk composite form. However, important differences in the dielectric relaxation and conduction mechanisms were found as result of the microstructural difference. Extrinsic contributions play important roles in modifying the electric properties in both ceramics, causing space charge effect, Maxwell-Wagner relaxations and hopping conductivity, mainly due to the ferrite low resistivity phase. The conductivity and dielectric modulus spectra analysis allowed to identify different polaron contributions associated with the microstructural differences. It results that by using the core-shell method, improved dielectric properties and limited hopping contributions can be realized.

  14. Characterization of the alkoxide-based sol-gel derived La9.33Si6O26 powder and ceramic.

    PubMed

    Vojisavljević, Katarina; Chevreux, Pierrick; Jouin, Jenny; Malič, Barbara

    2014-01-01

    In this study, we report on the acid-catalysed synthesis of La(9.33)Si(6)O(26) from lanthanum nitrate or acetate and silicon ethoxide (TEOS) in the ethanol solvent, upon the transition from liquid to amorphous and crystalline phases. The similarity of the Fourier transform infrared spectra of the lanthanum-salt solutions and lanthanum-silicon sols indicates that the lanthanum environment is not changed in the reaction of the La-salt with TEOS. In the nitric-acid catalysed synthesis, the hydrolysis reaction was almost instantaneous, as a consequence of a higher amount of water in this system, which contributed to a high level of chemical heterogeneity in the product. The acetic acid-based synthesis ensured a good mixing of the reagents at the nanometre level, which gave rise to the formation of the pure La(9.33)Si(6)O(26) powder upon heating at 900 °C, and single phase ceramics with 94 % relative density after sintering at 1400 °C for 3 h in air, which is 200 °C lower temperature then usually reported for the apatite material. PMID:25286208

  15. Qualification and initial characterization of a high-purity 233U spike for use in uranium analyses

    DOE PAGESBeta

    Mathew, K. J.; Canaan, R. D.; Hexel, C.; Giaquinto, J.; Krichinsky, A. M.

    2015-08-20

    Several high-purity 233U items potentially useful as isotope dilution mass spectrometry standards for safeguards, non-proliferation, and nuclear forensics measurements are identified and rescued from downblending. By preserving the supply of 233U materials of different pedigree for use as source materials for certified reference materials (CRMs), it is ensured that the safeguards community has high quality uranium isotopic standards required for calibration of the analytical instruments. One of the items identified as a source material for a high-purity CRM is characterized for the uranium isotope-amount ratios using thermal ionization mass spectrometry (TIMS). Additional verification measurements on this material using quadrupole inductivelymore » coupled plasma mass spectrometry (ICPMS) are also performed. As a result, the comparison of the ICPMS uranium isotope-amount ratios with the TIMS data, with much smaller uncertainties, validated the ICPMS measurement practices. ICPMS is proposed for the initial screening of the purity of items in the rescue campaign.« less

  16. Qualification and initial characterization of a high-purity 233U spike for use in uranium analyses

    SciTech Connect

    Mathew, K. J.; Canaan, R. D.; Hexel, C.; Giaquinto, J.; Krichinsky, A. M.

    2015-08-20

    Several high-purity 233U items potentially useful as isotope dilution mass spectrometry standards for safeguards, non-proliferation, and nuclear forensics measurements are identified and rescued from downblending. By preserving the supply of 233U materials of different pedigree for use as source materials for certified reference materials (CRMs), it is ensured that the safeguards community has high quality uranium isotopic standards required for calibration of the analytical instruments. One of the items identified as a source material for a high-purity CRM is characterized for the uranium isotope-amount ratios using thermal ionization mass spectrometry (TIMS). Additional verification measurements on this material using quadrupole inductively coupled plasma mass spectrometry (ICPMS) are also performed. As a result, the comparison of the ICPMS uranium isotope-amount ratios with the TIMS data, with much smaller uncertainties, validated the ICPMS measurement practices. ICPMS is proposed for the initial screening of the purity of items in the rescue campaign.

  17. All electrochemical fabrication of a bilayer membrane composed of nanotubular photocatalyst and palladium toward high-purity hydrogen production

    NASA Astrophysics Data System (ADS)

    Hattori, Masashi; Noda, Kei

    2015-12-01

    We developed an all-electrochemical technique for fabricating a bilayer structure of a titanium dioxide (TiO2) nanotube array (TNA) and a palladium film (TNA/Pd membrane), which works for photocatalytic high-purity hydrogen production. Electroless plating was used for depositing the Pd film on the TNA surface prepared by anodizing a titanium foil. A 3-μm-thick TNA/Pd membrane without any pinholes in a 1.5-cm-diameter area was fabricated by transferring a 1-μm-thick TNA onto an electroless-plated 2-μm-thick Pd film with a mechanical peel-off process. This ultrathin membrane with sufficient mechanical robustness showed photocatalytic H2 production via methanol reforming under ultraviolet illumination on the TNA side, immediately followed by the purification of the generated H2 gas through the Pd layer. The hydrogen production rate and the apparent quantum yield for high-purity H2 production from methanol/water mixture with the TNA/Pd membrane were also examined. This work suggests that palladium electroless plating is more suitable and practical for preparing a well-organized TNA/Pd heterointerface than palladium sputter deposition.

  18. Impurity analyses of high-purity carbon monoxide gas using micro gas chromatography for development as a certified reference material.

    PubMed

    Matsumoto, Nobuhiro; Watanabe, Takuro; Kato, Kenji

    2013-03-22

    High-purity carbon monoxide (CO) gas as a certified reference material (CRM) was analyzed using a micro gas chromatograph (micro-GC) with a micro thermal conductivity detector. The main reason to select the micro-GC was its compact size to provide a safe experimental environment. Thus, both the CO gas cylinder and the micro-GC were placed inside a draft shield with a limited small space. Peaks of several impurities were found in chromatograms of the micro-GC. The main impurities in the CO gas were helium, hydrogen, oxygen, nitrogen and carbon dioxide. It was found that helium was the impurity of the highest concentration. High-accuracy calibration gas mixtures were used to construct calibration lines for the micro-GC. The mixtures were precisely prepared by the gravimetric blending method. Calibration lines had enough linearity and accuracy for quantitative analyses of the impurities. The values of detection limit of the impurities were 0.7-4μmol/mol. The purity of the high-purity CO gas was around 99.996%, which was the value estimated from the sum of the concentrations of the impurities. PMID:23415447

  19. Mechanical Properties of High Purity SiC Fiber-Reinforced CVI-SiC Matrix Composites

    SciTech Connect

    Hinoki, Tatsuya; Lara-Curzio, Edgar; Snead, Lance L.

    2003-07-15

    Mechanical properties of silicon carbide composites reinforced with highly crystalline fibers and fabricated by the chemical vapor infiltration method were evaluated. Materials used were SiC/SiC composites reinforced with unidirectional Hi-Nicalon Type-S fibers and unidirectional Tyranno SA fibers with various fiber/matrix interphase. Also, SiC/SiC composites reinforced with plain weave Tyranno SA fibers with carbon or multilayers of silicon carbide and carbon interphase were evaluated. In-plane tensile, transthickness tensile and interlaminar shear properties were evaluated by the in-plane tensile test, the transthickness tensile test, the diametral compression test and the compression test of double-notched specimens.The elastic modulus and proportional limit stress were improved by using high purity silicon carbide fibers. The in-plane tensile properties were insensitive to carbon interphase thickness for a range of thicknesses between 30 and 230 nm. It was found that the in-plane tensile strength of composites containing multilayers of silicon carbide and carbon coating of fibers and fiber bundles was superior to that of composites with carbon alone. Transthickness tensile strength and shear strength of high purity silicon carbide composites were successfully evaluated.

  20. Tensile properties and interfacial bonding of multi-layered, high-purity titanium strips fabricated by ARB process.

    PubMed

    Ghafari-Gousheh, Soroush; Nedjad, Syamak Hossein; Khalil-Allafi, Jafar

    2015-11-01

    Severe plastic deformation (SPD) processing has shown very effective in promotion of mechanical properties of metals and alloys. In this study, the results of investigating mechanical properties and also inter-layer bond performance of accumulative roll bonded high purity titanium (HP-Ti) strips are presented. High purity titanium plates were severely deformed by use of a combination of cold rolling (CR) to a thickness reduction of approximately 87% and then accumulative roll bonding (ARB) for three cycles (N=3) at ambient temperature. Optical and scanning electron microscopy, tensile testing, and hardness measurements were conducted. The ARB strips exhibited lower tensile strength and ductility in comparison to cold rolled one which can basically be attributed to the poor function of the latest bonds established in the centerlines of the strips. Fractographic examinations revealed the interfacial de-bonding along the centerline between the layers having undergone roll bonding for just one cycle. It was while the interfaces having experienced roll bonding for more cycles showed much higher resistance against delaminating. PMID:26253205

  1. Heat treatment's effects on hydroxyapatite powders in water vapor and air atmosphere

    NASA Astrophysics Data System (ADS)

    Karabulut, A.; Baştan, F. E.; Erdoǧan, G.; Üstel, F.

    2015-03-01

    Hydroxyapatite (HA; Ca10(PO4)6(OH)2) is the main chemical constituent of bone tissue (~70%) as well as HA which is a calcium phosphate based ceramic material forms inorganic tissue of bone and tooth as hard tissues is used in production of prosthesis for synthetic bone, fractured and broken bone restoration, coating of metallic biomaterials and dental applications because of its bio compatibility. It is known that Hydroxyapatite decomposes with high heat energy after heat treatment. Therefore hydroxyapatite powders that heated in water vapor will less decomposed phases and lower amorphous phase content than in air atmosphere. In this study high purity hydroxyapatite powders were heat treated with open atmosphere furnace and water vapor atmosphere with 900, 1000, 1200 °C. Morphology of same powder size used in this process by SEM analyzed. Chemical structures of synthesized coatings have been examined by XRD. The determination of particle size and morphological structure of has been characterized by Particle Sizer, and SEM analysis, respectively. Weight change of sample was recorded by thermogravimetric analysis (TGA) during heating and cooling.

  2. Microstructures and superconducting properties of high performance MgB2 thin films deposited from a high-purity, dense Mg-B target

    NASA Astrophysics Data System (ADS)

    Li, G. Z.; Susner, M. A.; Bohnenstiehl, S. D.; Sumption, M. D.; Collings, E. W.

    2015-12-01

    High quality, c-axis oriented, MgB2 thin films were successfully grown on 6H-SiC substrates using pulsed laser deposition (PLD) with subsequent in situ annealing. To obtain high purity films free from oxygen contamination, a dense Mg-B target was specially made from a high temperature, high pressure reaction of Mg and B to form large-grained (10-50 μm) MgB2. Microstructural analysis via electron microscopy found that the resulting grains of the film were composed of ultrafine columnar grains of 19-30 nm. XRD analysis showed the MgB2 films to be c-axis oriented; the a-axis and c-axis lattice parameters were determined to be 3.073 ± 0.005 Å and 3.528 ± 0.010 Å, respectively. The superconducting critical temperature, Tc,onset, increased monotonically as the annealing temperature was increased, varying from 25.2 K to 33.7 K. The superconducting critical current density as determined from magnetic measurements, Jcm, at 5 K, was 105 A/cm2 at 7.8 T; at 20 K, 105 A/cm2 was reached at 3.1 T. The transport and pinning properties of these films were compared to "powder-in-tube" (PIT) and "internal-infiltration" (AIMI) processed wires. Additionally, examination of the pinning mechanism showed that when scaled to the peak in the pinning curve, the films follow the grain boundary, or surface, pinning mechanism quite well, and are similar to the response seen for C doped PIT and AIMI strands, in contrast to the behavior seen in undoped PIT wires, in which deviations are seen at high b (b = B/Bc2). On the other hand, the magnitude of the pinning force was similar for the thin films and AIMI conductors, unlike the values from connectivity-suppressed PIT strands.

  3. Preparation of High Purity, High Molecular-Weight Chitin from Ionic Liquids for Use as an Adsorbate for the Extraction of Uranium from Seawater

    SciTech Connect

    Rogers, Robin

    2013-12-21

    Ensuring a domestic supply of uranium is a key issue facing the wider implementation of nuclear power. Uranium is mostly mined in Kazakhstan, Australia, and Canada, and there are few high-grade uranium reserves left worldwide. Therefore, one of the most appealing potential sources of uranium is the vast quantity dissolved in the oceans (estimated to be 4.4 billion tons worldwide). There have been research efforts centered on finding a means to extract uranium from seawater for decades, but so far none have resulted in an economically viable product, due in part to the fact that the materials that have been successfully demonstrated to date are too costly (in terms of money and energy) to produce on the necessary scale. Ionic Liquids (salts which melt below 100{degrees}C) can completely dissolve raw crustacean shells, leading to recovery of a high purity, high molecular weight chitin powder and to fibers and films which can be spun directly from the extract solution suggesting that continuous processing might be feasible. The work proposed here will utilize the unprecedented control this makes possible over the chitin fiber a) to prepare electrospun nanofibers of very high surface area and in specific architectures, b) to modify the fiber surfaces chemically with selective extractant capacity, and c) to demonstrate their utility in the direct extraction and recovery of uranium from seawater. This approach will 1) provide direct extraction of chitin from shellfish waste thus saving energy over the current industrial process for obtaining chitin; 2) allow continuous processing of nanofibers for very high surface area fibers in an economical operation; 3) provide a unique high molecular weight chitin not available from the current industrial process, leading to stronger, more durable fibers; and 4) allow easy chemical modification of the large surface areas of the fibers for appending uranyl selective functionality providing selectivity and ease of stripping. The

  4. Silicon nitride/silicon carbide composite densified materials prepared using composite powders

    DOEpatents

    Dunmead, S.D.; Weimer, A.W.; Carroll, D.F.; Eisman, G.A.; Cochran, G.A.; Susnitzky, D.W.; Beaman, D.R.; Nilsen, K.J.

    1997-07-01

    Prepare silicon nitride-silicon carbide composite powders by carbothermal reduction of crystalline silica powder, carbon powder and, optionally, crystalline silicon nitride powder. The crystalline silicon carbide portion of the composite powders has a mean number diameter less than about 700 nanometers and contains nitrogen. The composite powders may be used to prepare sintered ceramic bodies and self-reinforced silicon nitride ceramic bodies.

  5. Piezoelectric Properties of Li-Doped (K0.48Na0.52)NbO3 Ceramics Synthesized Using Hydrothermally-Derived KNbO3 and NaNbO3 Fine Powders

    NASA Astrophysics Data System (ADS)

    Maeda, Takafumi; Hemsel, Tobias; Morita, Takeshi

    2012-09-01

    [Lix(Na0.52K0.48)1-x]NbO3 (0 ≤x ≤0.091) ceramics were synthesized using hydrothermal powders and the lithium doping content was controlled to optimize their piezoelectric properties. The raw KNbO3 and NaNbO3 powders were obtained separately by a hydrothermal method and LiNbO3 powders were prepared by milling a commercial LiNbO3 single crystal. These powders were mixed with ethanol at a molar ratio LiNbO3: (Na0.52K0.48)NbO3= x : 1-x. The synthesized powders were sintered at 1060-1120 °C for 2 h. We succeeded in obtaining highly dense [Lix(Na0.52K0.48)1-x]NbO3 ceramics using hydrothermal powder. The X-ray diffraction patterns revealed that the crystal phase changed from orthorhombic to tetragonal at around x = 0.06. At this morphotropic phase boundary (MPB), the c/a ratio changed from 1.016 to 1.024 and the highest piezoelectric constant was obtained with the chemical component of [Li0.065(K0.48Na0.52)0.935]NbO3. The obtained piezoelectric properties were as follows: k33 = 0.51, ɛ33T/ɛ0 = 836, c33E = 46 GPa, d33 = 203 pC/N, and Tc = 482 °C.

  6. Effect of Si3N4 powder reactivity on the preparation of the Si2N2O-Al2O3 silicon aluminum oxynitride solid solution

    NASA Technical Reports Server (NTRS)

    Sekercioglu, I.; Wills, R. R.

    1979-01-01

    Dense high-purity silicon aluminum oxynitride was prepared by reactive hot-pressing of an Si3N4-Al2O3-SiO2 mixture. The formation of a single-phase material was found to be critically dependent on the Si3N4 powder in the starting mixture. It is suggested that evolution of a chlorine- and nitrogen-containing species may enhance the reactivity of Si3N4 in this reaction. Densities of O prime sialons are very similar to that of Si2N2O, the widely quoted value in the ceramics literature of 3.1 g/cu cm for the density of Si2N2O being incorrect.

  7. The use of a high-purity germanium detector for routine measurements of {sup 125}I in radiation workers

    SciTech Connect

    Kopp, P.; Bergmann, H.; Havlik, E.; Aiginger, H.; Unfried, E.; Riedlmayer, L.

    1994-12-01

    A high-purity germanium detector was calibrated for the assessment of {sup 125}I uptake in the thyroid gland of radiation workers. A cylindrical water phantom (perspex walls) with high flexibility for position and size of the thyroid was constructed. Within a massive shielding chamber built for a whole-body counter, an activity of 2.2 Bq was detectable (MDA). This is well below the very restrictive limiting value of 20 Bq for inhalation specified by Austrian law. An activity of 128 Bq was measured with a statistical uncertainty of 5% in a counting period of 10 min. Various parameters influencing the result are investigated as well as the performance of two other measurement geometries outside the shielding chamber. 13 refs., 4 figs., 2 tabs.

  8. Room-temperature annealing of vacancy-type defect in high-purity n-type Si

    SciTech Connect

    Bleka, J. H.; Monakhov, E. V.; Svensson, B. G.; Avset, B. S.

    2007-12-15

    Electron-irradiated p{sup +}-n{sup -}-n{sup +} diodes produced from low-doped high-purity Si wafers were found, by deep-level transient spectroscopy (DLTS), to have a prominent defect, labeled E4, with an energy level 0.37 eV below the conduction-band edge and a concentration of {approx}(1/4) relative to the divacancy. The samples were kept at room temperature, and the E4 concentration was seen to reduce to half during five weeks. Annealing data revealed a similar peak E5 overlapping that of the single-negatively charged divacancy and showing a one-to-one proportionality with E4. E4 and E5 arise most likely from a vacancy-type defect and a tentative assignment to a planar tetravacancy is put forward.

  9. Delta-Doped High Purity Silicon UV-NIR CCDs with High QE and Low Dark Current

    NASA Technical Reports Server (NTRS)

    Hoenk, Michael; Blacksberg, Jordana; Nikzad, Shouleh; Elliott, S. Tom; Holland, Steve; Bebek, Chris; Scowen, Paul; Veach, Todd

    2006-01-01

    Delta doping process was developed on p-channel CCDs for MIDEX-Orion and JDEM/SNAP and was applied to large format (2k x4k) CCDs. Delta doping is applied to fully-fabricated CCDs (complete with Al metallization). High QE and low dark current is demonstrated with delta doped p-channel CCDs. In-house AR coating is demonstrated. Advantages include: Delta doping enables high QE and stability across the entire spectral range attainable with silicon. Delta doping is a low temperature process and is compatible with fully-fabricated detector arrays. Same base device for Orion two channels. High radiation tolerance and no thinning requirements of high purity p-channel. CCDs are additional advantages.

  10. Pitting Corrosion in CVD SiC at 300°C in Deoxygenated High-Purity Water

    SciTech Connect

    Henager, Charles H.; Schemer-Kohrn, Alan L.; Pitman, Stan G.; Senor, David J.; Geelhood, Ken J.; Painter, Chad L.

    2008-08-15

    SiC is a candidate for nuclear applications at elevated temperatures but has not been fully studied under typical light-water reactor operating conditions, such as moderate temperatures and high pressures. Coupons of high-purity chemical vapor deposited SiC were exposed to deoxygenated, pressurized water at 573K and 100 Bar for up to 4000 hours. Ceramographic examination of the exposed SiC surfaces revealed both embryonic and large, d > 300 µm, pits on the surface. The pits were characterized using scanning electron microscopy for structure and chemistry analysis. Pit densities were also determined by standard counting methods. The chemical analysis revealed that the pits are associated with the formation of silica and subsequent loss of Si, which is expected due to several suggested reactions between SiC and water.

  11. Enhanced quantum efficiency of high-purity silicon imaging detectors by ultralow temperature surface modification using Sb doping

    SciTech Connect

    Blacksberg, Jordana; Hoenk, Michael E.; Elliott, S. Tom; Holland, Stephen E.; Nikzad, Shouleh

    2005-12-19

    A low temperature process for Sb doping of silicon has been developed as a backsurface treatment for high-purity n-type imaging detectors. Molecular beam epitaxy (MBE) is used to achieve very high dopant incorporation in a thin, surface-confined layer. The growth temperature is kept below 450 deg. C for compatibility with Al-metallized devices. Imaging with MBE-modified 1kx1k charge coupled devices (CCDs) operated in full depletion has been demonstrated. Dark current is comparable to the state-of-the-art process, which requires a high temperature step. Quantum efficiency is improved, especially in the UV, for thin doped layers placed closer to the backsurface. Near 100% internal quantum efficiency has been demonstrated in the ultraviolet for a CCD with a 1.5 nm silicon cap layer.

  12. Phase transformations of high-purity PbI2 nanoparticles synthesized from lead-acid accumulator anodes

    NASA Astrophysics Data System (ADS)

    Malevu, T. D.; Ocaya, R. O.; Tshabalala, K. G.

    2016-09-01

    High-purity hexagonal lead iodide nanoparticles have been synthesized from a depleted sealed lead acid battery anode. The synthesized product was found to consist of the rare 6R polytype form of PbI2 that is thought to have good potential in photovoltaic applications. We investigate the effects of annealing time and post-melting temperature on the structure and optical properties using 1.5418 Å CuKα radiation. Photoluminescence measurements were done under 150 W/221 nm wavelength xenon excitation. Phase transformation was observed through XRD peaks when annealing time increased from 0.5-5 h. The nanoparticle grain size and inter-planar distance appeared to be independent of annealing time. PL measurements show three broad peaks in a range of 400 nm to 700 nm that are attributed to excitonic, donor-acceptor pair and luminescence bands from the deep levels.

  13. Synthesis and optical properties of high-purity CoO nanowires prepared by an environmentally friendly molten salt route

    NASA Astrophysics Data System (ADS)

    Wang, Wenzhong; Zhang, Guling

    2009-08-01

    CoO nanowires with diameters of 50 _80 nm, and lengths of up to more than 5 μm have been successfully synthesized by a simple environmentally friendly molten salt route, in which the precursor CoCO 3 nanoparticles are decomposed to form high-purity CoO nanowires in NaCl flux. The structure features and morphology of the as-prepared CoO nanowires were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution TEM (HRTEM), and selected area electron diffraction (SAED). The chemical composition and oxidation state of the prepared nanowires were systemically studied by X-ray photoelectron spectra (XPS) and laser Raman spectroscopy. The results indicated that the as-prepared CoO nanowires were composed of pure cubic CoO phase. The growth mechanism of the synthesized nanowires was also discussed in detail based on the experimental results.

  14. Performance of A Compact Multi-crystal High-purity Germanium Detector Array for Measuring Coincident Gamma-ray Emissions

    SciTech Connect

    Howard, Chris; Daigle, Stephen; Buckner, Matt; Erikson, Luke E.; Runkle, Robert C.; Stave, Sean C.; Champagne, Art; Cooper, Andrew; Downen, Lori; Glasgow, Brian D.; Kelly, Keegan; Sallaska, Anne

    2015-02-18

    The Multi-sensor Airborne Radiation Survey (MARS) detector is a 14-crystal array of high-purity germanium (HPGe) detectors housed in a single cryostat. The array was used to measure the astrophysical S-factor for the 14N(p,γ)15O* reaction for several transition energies at an effective center of mass energy of 163 keV. Owing to the segmented nature of the MARS detector, the effect of gamma-ray summing was greatly reduced in comparison to past experiments which utilized large, single-crystal detectors. The new S-factor values agree within the uncertainties with the past measurements. Details of the analysis and detector performance will be presented.

  15. Enhanced quantum efficiency of high-purity silicon imaging detectors by ultralow temperature surface modification using Sb doping

    NASA Technical Reports Server (NTRS)

    Blacksberg, Jordana; Hoenk, Michael E.; Elliott, S. Tom; Holland, Stephen E.; Nikzad, Shouleh

    2005-01-01

    A low temperature process for Sb doping of silicon has been developed as a backsurface treatment for high-purity n-type imaging detectors. Molecular beam epitaxy (MBE) is used to achieve very high dopant incorporation in a thin, surface-confined layer. The growth temperature is kept below 450 (deg)C for compatibility with Al-metallized devices. Imaging with MBE-modified 1kx1k charge coupled devices (CCDs) operated in full depletion has been demonstrated. Dark current is comparable to the state-of-the-art process, which requires a high temperature step. Quantum efficiency is improved, especially in the UV, for thin doped layers placed closer to the backsurface. Near 100% internal quantum efficiency has been demonstrated in the ultraviolet for a CCD with a 1.5 nm silicon cap layer.

  16. Formation and annihilation of intrinsic defects induced by electronic excitation in high-purity crystalline SiO{sub 2}

    SciTech Connect

    Kajihara, Koichi; Skuja, Linards; Hosono, Hideo

    2013-04-14

    Formation and thermal annihilation of intrinsic defects in {alpha}-quartz were examined using high-purity samples, while minimizing the contributions of reactions involving metallic impurities. Electronic excitation with {sup 60}Co {gamma}-rays was employed to avoid radiation-induced amorphization. The results clearly show that formation of oxygen vacancies (Si-Si bonds) as a result of decomposition of regular Si-O-Si bonds (Frenkel process) is the dominant intrinsic defect process. Compared with amorphous SiO{sub 2}, in {alpha}-quartz, the formation yield of Si-Si bonds is an order of magnitude smaller, the 7.6 eV optical absorption band is less broadened, and their thermal annihilation is complete at a lower temperature, around the {alpha}-{beta} quartz transition. In contrast, radiation-induced interstitial oxygen atoms practically do not form interstitial oxygen molecules.

  17. The effectiveness of circulating aeration in air and high purity oxygen systems for control of VOC emissions from aeration basins

    SciTech Connect

    Zhu, H.; Keener, T.C.; Bishop, P.L.; Orton, T.L.; Wang, M.; Siddiqui, K.F.

    1997-12-31

    A simple steady state circulating aeration system (CAS) model has been used to study the effects of volatility and degradability on the fate of VOCs in both air and high purity oxygen (HPO) systems. With increase of circulation ratio in an air CAS, air emissions by stripping can be significantly reduced for compounds of low degradabilities and high volatilities. Enhancement of biodegradation is more significant for compounds of high degradabilities and volatilities. A large portion of VOCs will remain in the wastewater when circulation ratio is high, especially for VOCs that are difficult to degrade. In HPO systems, emissions by stripping are much less than air systems. However, VOCs will remain in the wastewater if they have poor degradabilities. Volatilities of VOCs are not important in HPO systems. Due to their wide range and large uncertainties, degradation rate constants are a major factor determining the effectiveness of a CAS for VOC emission control

  18. Purification of Al(OH)3 synthesized by Bayer process for preparation of high purity alumina as sapphire raw material

    NASA Astrophysics Data System (ADS)

    Park, No-Kuk; Choi, Hee-Young; Kim, Do-Hyeong; Lee, Tae Jin; Kang, Misook; Lee, Won Gun; Kim, Heun Duk; Park, Joon Woo

    2013-06-01

    To produce high purity alumina as the raw material for sapphire growth, gibbsite, which is the precursor for the synthesis of alumina, was synthesized by the Bayer process, and treated with an acid solution to remove the sodium component. In this study, the digestion process was carried out under the following conditions: an Al/Na ratio of 0.9 with a 5 N NaOH solution and a temperature of 140 °C. Bauxite containing 75 wt% alumina was converted to a sodium aluminate solution, and 60 wt% of the dissolved aluminate was crystallized to gibbsite. The sodium content in the gibbsite, which was measured by inductively coupled plasma/optical emission spectroscopy, was reduced by approximately 5700 ppm and below 2900 ppm after the water washing and acid treatments, respectively. The sodium content decreased with increasing acid concentration in the solution, temperature and acid treatment time.

  19. Nature of heterophase inclusions in high-purity optical fiber materials as studied with 3D laser ultramicroscopy

    NASA Astrophysics Data System (ADS)

    Ketkova, L. A.

    2015-09-01

    3D laser ultramicroscopy (3D LUM) is intended specially for determining the concentration and size distribution of submicron inclusions in the bulk samples of high-purity materials for visible and IR fiber optics. In this work the 3D LUM technique is shown to be able to identify the nature of individual inclusions detected. The measurement of the light scattered by an inclusion at a varied probe beam wavelength and polarization and at a varied scattered light collection angle makes it possible to determine the inclusion refractive index. The 3D LUM possibilities are illustrated by the example of studying the inclusion nature in the As2S3 glass samples prepared by the direct synthesis from elements in a quartz container at elevated temperatures.

  20. High purity H2 by sorption-enhanced chemical looping reforming of waste cooking oil in a packed bed reactor.

    PubMed

    Pimenidou, P; Rickett, G; Dupont, V; Twigg, M V

    2010-12-01

    High purity hydrogen (>95%) was produced at 600 degrees C and 1 atm by steam reforming of waste cooking oil at a molar steam to carbon ratio of 4 using chemical looping, a process that features redox cycles of a Ni catalyst with the in-situ carbonation/calcination of a CO(2) sorbent (dolomite) in a packed bed reactor under alternated feedstreams of fuel-steam and air. The fuel and steam conversion were higher with the sorbent present than without it. Initially, the dolomite carbonation was very efficient (100%), and 98% purity hydrogen was produced, but the carbonation decreased to around 56% with a purity of 95% respectively in the following cycles. Reduction of the nickel catalyst occurred alongside steam reforming, water gas shift and carbonation, with H(2) produced continuously under fuel-steam feeds. Catalyst and CO(2)-sorbent regeneration was observed, and long periods of autothermal operation within each cycle were demonstrated. PMID:20655199

  1. Industrial-scale separation of high-purity single-chirality single-wall carbon nanotubes for biological imaging

    NASA Astrophysics Data System (ADS)

    Yomogida, Yohei; Tanaka, Takeshi; Zhang, Minfang; Yudasaka, Masako; Wei, Xiaojun; Kataura, Hiromichi

    2016-06-01

    Single-chirality, single-wall carbon nanotubes are desired due to their inherent physical properties and performance characteristics. Here, we demonstrate a chromatographic separation method based on a newly discovered chirality-selective affinity between carbon nanotubes and a gel containing a mixture of the surfactants. In this system, two different selectivities are found: chiral-angle selectivity and diameter selectivity. Since the chirality of nanotubes is determined by the chiral angle and diameter, combining these independent selectivities leads to high-resolution single-chirality separation with milligram-scale throughput and high purity. Furthermore, we present efficient vascular imaging of mice using separated single-chirality (9,4) nanotubes. Due to efficient absorption and emission, blood vessels can be recognized even with the use of ~100-fold lower injected dose than the reported value for pristine nanotubes. Thus, 1 day of separation provides material for up to 15,000 imaging experiments, which is acceptable for industrial use.

  2. Performance of a compact multi-crystal high-purity germanium detector array for measuring coincident gamma-ray emissions

    NASA Astrophysics Data System (ADS)

    Howard, Chris; Daigle, Stephen; Buckner, Matt; Erikson, Luke E.; Runkle, Robert C.; Stave, Sean C.; Champagne, Arthur E.; Cooper, Andrew; Downen, Lori; Glasgow, Brian D.; Kelly, Keegan; Sallaska, Anne

    2015-05-01

    The Multi-sensor Airborne Radiation Survey (MARS) detector is a 14-crystal array of high-purity germanium (HPGe) detectors housed in a single cryostat. The array was used to measure the astrophysical S-factor for the 14N(p,γ)15O* reaction for several transition energies at an effective center-of-mass energy of 163 keV. Owing to the granular nature of the MARS detector, the effect of gamma-ray summing was greatly reduced in comparison to past experiments which utilized large, single-crystal detectors. The new S-factor values agree within their uncertainties with the past measurements. Details of the analysis and detector performance are presented.

  3. Role of Chemical Driving Force in Martensitic Transformations of High-Purity Fe-Cr-Ni Alloys

    NASA Astrophysics Data System (ADS)

    Behjati, P.; Najafizadeh, A.

    2011-12-01

    The main objective of the present work is to point out the respective roles of chemical driving force and stacking fault energy (SFE) in the occurrence of martensitic transformations in high-purity Fe-Cr-Ni alloys. For this purpose, the transmission electron microscope (TEM), X-ray diffractometer, thermal differential microanalyzer (TDA), and tension test were employed to report M s temperatures, austenite stacking fault energies, and driving forces for the concerned alloys. It was observed that the martensitic transformations in the studied alloys occur through the γ → ɛ → α' steps. As a remarkable result, it was shown that a low SFE, if necessary to ɛ-phase nucleation, is not a sufficient condition for nucleation of α' phase. In fact, the formation of stable α' nuclei from α' embryos occur if the required chemical driving force is provided. Also, an equation was proposed for the kinetics of spontaneous martensitic transformation as a function of driving force.

  4. Thickness dependence of the poling and current-voltage characteristics of paint films made up of lead zirconate titanate ceramic powder and epoxy resin

    NASA Astrophysics Data System (ADS)

    Egusa, Shigenori; Iwasawa, Naozumi

    1995-11-01

    A specially prepared paint made up of lead zirconate titanate (PZT) ceramic powder and epoxy resin was coated on an aluminum plate and was cured at room temperature, thus forming the paint film of 25-300 μm thickness with a PZT volume fraction of 53%. The paint film was then poled at room temperature, and the poling behavior was determined by measuring the piezoelectric activity as a function of poling field. The poling behavior shows that the piezoelectric activity obtained at a given poling field increases with an increase in the film thickness from 25 to 300 μm. The current-voltage characteristic of the paint film, on the other hand, shows that the increase in the film thickness leads not only to an increase in the magnitude of the current density at a given electric field but also to an increase in the critical electric field at which the transition from the ohmic to space-charge-limited conduction takes place. This fact indicates that the amount of the space charge of electrons injected into the paint film decreases as the film thickness increases. Furthermore, comparison of the current-voltage characteristic of the paint film with that of a pure epoxy film reveals that the space charge is accumulated largely at the interface between the PZT and epoxy phases in the paint film. On the basis of this finding, a model is developed for the poling behavior of the paint film by taking into account a possible effect of the space-charge accumulation and a broad distribution of the electric field in the PZT phase. This model is shown to give an excellent fit to the experimental data of the piezoelectric activity obtained here as a function of poling field and film thickness.

  5. High-purity 60GHz band millimeter-wave generation based on optically injected semiconductor laser under subharmonic microwave modulation.

    PubMed

    Fan, Li; Xia, Guangqiong; Chen, Jianjun; Tang, Xi; Liang, Qing; Wu, Zhengmao

    2016-08-01

    Based on an optically injected semiconductor laser (OISL) operating at period-one (P1) nonlinear dynamical state, high-purity millimeter-wave generation at 60 GHz band is experimentally demonstrated via 1/4 and 1/9 subharmonic microwave modulation (the order of subharmonic is with respect to the frequency fc of the acquired 60 GHz band millimeter-wave but not the fundamental frequency f0 of P1 oscillation). Optical injection is firstly used to drive a semiconductor laser into P1 state. For the OISL operates at P1 state with a fundamental frequency f0 = 49.43 GHz, by introducing 1/4 subharmonic modulation with a modulation frequency of fm = 15.32 GHz, a 60 GHz band millimeter-wave with central frequency fc = 61.28 GHz ( = 4fm) is experimentally generated, whose linewidth is below 1.6 kHz and SSB phase noise at offset frequency 10 kHz is about -96 dBc/Hz. For fm is varied between 13.58 GHz and 16.49 GHz, fc can be tuned from 54.32 GHz to 65.96 GHz under matched modulation power Pm. Moreover, for the OISL operates at P1 state with f0 = 45.02 GHz, a higher order subharmonic modulation (1/9) is introduced into the OISL for obtaining high-purity 60 GHz band microwave signal. With (fm, Pm) = (7.23 GHz, 13.00 dBm), a microwave signal at 65.07 GHz ( = 9fm) with a linewidth below 1.6 kHz and a SSB phase noise less than -98 dBc/Hz is experimentally generated. Also, the central frequency fc can be tuned in a certain range through adjusting fm and selecting matched Pm. PMID:27505789

  6. Recovery of high purity zinc from filter ash produced during the thermal treatment of waste and inerting of residual materials.

    PubMed

    Schlumberger, Stefan; Schuster, Michael; Ringmann, Stefan; Koralewska, Ralf

    2007-12-01

    The method described below recovers zinc, a valuable metal that is present in high concentrations in filter ash from the thermal treatment of waste, and returns the filter ash stripped of heavy metals to the combustion process in order to destroy organic substances. On an industrial scale, the heavy metals in the filter ash were mobilized by means of hydrochloric acid in the acidic fluids produced in the flue-gas scrubbing process without the addition of further chemicals. A pilot plant for implementing the selective reactive extraction (SRE) method on the ash extracts, using a highly selective complexant, was operated over a period of several months in order to obtain a concentrated, high-purity zinc salt solution (mono metal solution). A zinc depletion rate of 99.8% in the aqueous extract was achieved using mixer-settler units. The residual zinc concentration in the waste water was then < 2 mg L(-1). By stripping the loaded organic phase, a concentrated, high-purity mono metal solution with 190 g L(-1) zinc was obtained. Zinc metal with a purity > 99.99% is then separated by means of electrolysis. To destroy organic substances present in the filter ash, particularly dioxins and furans, the extracted filter ash cake was returned to the combustion process together with household waste. Plant operation, raw and pure gas parameters, and quality of the bottom ash produced were not impacted by such recirculation. The profitability of the overall process is attributable both to the recovery of valuable zinc metal and to the cost savings made in waste water treatment and in the disposal of the waste combustion residues because the remaining mixture of filter ash and bottom ash can be reused in a combined form. This method therefore supports the sustainable and economically viable reuse of filter ash. PMID:18229749

  7. Determination of trace impurities in high purity gold by inductively coupled plasma mass spectrometry with prior matrix removal by electrodeposition

    NASA Astrophysics Data System (ADS)

    Sun, Y. C.; Hsieh, C. H.; Lin, T. S.; Wen, J. C.

    2000-09-01

    A novel method for the determination of 11 trace impurities (Be, Mg, Cr, Mn, Ni, Cu, Zn, Ag, Pd, Sn and Pb) in high purity gold with a combination of electrochemical deposition separation and inductively coupled plasma mass spectrometric measurement was investigated. In the present study, an efficient separation procedure was developed to remove the gold matrix by the electrodepositon method on the basis of the difference in reduction potential of gold and the other trace impurities. The effects of deposition potential, deposition time and composition of the electrolyte on the separation efficiency were studied. According to our experimental results, most impurities, except for silver, can remain in the electrolyte and the interference from gold can be completely removed through the application of electrodeposition at suitable potential. To achieve simultaneous separation of silver from the gold matrix, a unique complexation reaction between silver ions and ammonia ions was successfully employed to alter the reduction potential of silver ion. By way of a suitable adjustment of the deposition potential and the composition of electrolytes, the spike recoveries of 11 interesting impurities were found to be in the range of 85-105%. The limit of detection (based on the 3-σ criterion) of these elements was 10 -1-10 -2 μg g -1. The applicability of the proposed method has also been validated by the analysis of high purity gold reference materials (FAU9 and FAU11, Royal Canadian Mint). Comparing with the certified values, the recoveries of interesting elements were found to be in the range of 82-118% through the use of proposed method.

  8. A facile approach for synthesizing Fe-based layered double hydroxides with high purity and its exfoliation.

    PubMed

    Wang, Yinling; Li, Fajun; Dong, Shengye; Liu, Xiaowang; Li, Maoguo

    2016-04-01

    Transition metal (e.g., Fe, Co, Ni)-based layered double hydroxides (LDHs) and their exfoliated nanosheets have great potential applications due to their redox and magnetic properties. Here we report a facile approach for the preparation of Co-Fe LDHs with good crystallinity and high purity. The proposed approach includes two steps: (1) The mixed divalent metal (e.g., Co(2+), Fe(2+)) hydroxides were first synthesized using a homogeneous precipitation without piping N2 into the system; hexamethylenetetramine (HMT) was the hydrolysis agent providing OH(-), and hydroxylamine hydrochloride (HAH) was used as both a reducing and a complexing reagent. (2) Then the as-prepared hydroxides were slowly oxidated by air and simultaneously intercalated by CO3(2-) to form CO3-intercalated LDHs. The Co-Fe LDHs were roundly characterized by XRD, SEM, EDX and FT-IR. The effect of HAH on the morphology and structure of the Co-Fe LDHs was also studied. The magnetism of Co-Fe LDHs at room temperature was investigated and the results showed that the LDHs displayed a low saturation magnetization value of 6.3emug(-1), suggesting that the purity of the products was very high. In addition, the intercalated CO3(2-) in the Co-Fe LDHs could be successfully exchanged with other anions such as Cl(-) and ClO4(-). Furthermore, the exchanged-LDHs could be exfoliated in formamide. This work establishes a new method for the synthesis of Fe-based LDHs with good crystallinity and high purity under mild conditions, and can accelerate the development of applications using these layered materials. PMID:26773611

  9. Method for synthesizing powder materials

    DOEpatents

    Buss, R.J.; Ho, P.

    1988-01-21

    A method for synthesizing ultrafine powder materials, for example, ceramic and metal powders, comprises admitting gaseous reactants from which the powder material is to be formed into a vacuum reaction chamber maintained at a pressure less than atmospheric and at a temperature less than about 400/degree/K (127/degree/C). The gaseous reactants are directed through a glow discharge provided in the vacuum reaction chamber to form the ultrafine powder material. 1 fig.

  10. Synthesis, Structural and Electrical properties of Bi4Ti3O12 & Bi3.5La0.5Ti3O12 Ferroelectric ceramics

    NASA Astrophysics Data System (ADS)

    Roy, M.; Bala, Indu; Barbar, S. K.; Jangid, S.; Dave, P.

    2011-07-01

    Polycrystalline ceramic samples of Bi4Ti3O12 and the La-doped Bi3.5La0.5Ti3O12 have been synthesized by standard high temperature solid state reaction method using high purity oxides and carbonates. The effect of lanthanum doping on the structure of Bi4Ti3O12 powders was investigated by X-ray diffraction. A better agreement between the observed and calculated X-Ray diffraction pattern was obtained by performing the Rietveld refinement with a structural model using the non centrosymmetric space group Fmmm. Rietveld analysis revealed that with the partial substitution of La on the Bi site increases the a and b lattice parameters and decreases the c parameter. The activation energies calculated from dc conductivities are 1.033 eV and 2.244 eV which shows that La doping increases the resistivity of the material useful for dielectric devices.

  11. Microwave dielectric properties and sintering behavior of nano-scaled ({alpha} + {theta})-Al{sub 2}O{sub 3} ceramics

    SciTech Connect

    Huang, C.-L. Wang, J.-J.; Yen, F.-S.; Huang, C.-Y.

    2008-06-03

    The dielectric properties at microwave frequencies and the microstructures of nano ({alpha} + {theta})-Al{sub 2}O{sub 3} ceramics were investigated. Using the high-purity nano ({alpha} + {theta})-Al{sub 2}O{sub 3} powders can effectively increase the value of the quality factor and lower the sintering temperature of the ceramic samples. Grain growth can be limited with {theta}-phase Al{sub 2}O{sub 3} addition and high-density alumina ceramics can be obtained with smaller grain size comparing to pure {alpha}-Al{sub 2}O{sub 3}. Relative density of sintered samples can be as high as 99.49% at 1400 deg. C for 8 h. The unloaded quality factors Q x f are strongly dependent on the sintering time. Further improvement of the Q x f value can be achieved by extending the sintering time to 8 h. A dielectric constant ({epsilon}{sub r}) of 10, a high Q x f value of 634,000 GHz (measured at 14 GHz) and a temperature coefficient of resonant frequency ({tau}{sub f}) of -39.88 ppm/deg. C were obtained for specimen sintered at 1400 deg. C for 8 h. Sintered ceramic samples were also characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM)

  12. Submicron silicon powder production in an aerosol reactor

    NASA Technical Reports Server (NTRS)

    Wu, J. J.; Flagan, R. C.; Gregory, O. J.

    1986-01-01

    Powder synthesis by thermally induced vapor phase reactions is described. The powder generated by this technique consists of spherical, nonagglomerated particles of high purity. The particles are uniform in size, in the 0.1-0.2-micron size range. Most of the particles are crystalline spheres. A small fraction of the spheres are amorphous. Chain agglomerates account for less than 1 percent of the spherules.

  13. History of ``NANO''-Scale VERY EARLY Solid-State (and Liquid-State) Physics/Chemistry/Metallurgy/ Ceramics; Interstitial-Alloys Carbides/Nitrides/Borides/...Powders and Cermets, Rock Shocks, ...

    NASA Astrophysics Data System (ADS)

    Maiden, Colin; Siegel, Edward

    History of ``NANO'': Siegel-Matsubara-Vest-Gregson[Mtls. Sci. and Eng. 8, 6, 323(`71); Physica Status Solidi (a)11,45(`72)] VERY EARLY carbides/nitrides/borides powders/cermets solid-state physics/chemistry/metallurgy/ ceramics FIRST-EVER EXPERIMENTAL NANO-physics/chemistry[1968 ->Physica Status Solidi (a)11,45(`72); and EARLY NANO-``physics''/NANO-``chemistry'' THEORY(after: Kubo(`62)-Matsubara(`60s-`70s)-Fulde (`65) [ref.: Sugano[Microcluster-Physics, Springer('82 `98)

  14. Alumina-based ceramic composite

    DOEpatents

    Alexander, K.B.; Tiegs, T.N.; Becher, P.F.; Waters, S.B.

    1996-07-23

    An improved ceramic composite comprising oxide ceramic particulates, nonoxide ceramic particulates selected from the group consisting of carbides, borides, nitrides of silicon and transition metals and mixtures thereof, and a ductile binder selected from the group consisting of metallic, intermetallic alloys and mixtures thereof is described. The ceramic composite is made by blending powders of the ceramic particulates and the ductile to form a mixture and consolidating the mixture of under conditions of temperature and pressure sufficient to produce a densified ceramic composite. 5 figs.

  15. Micro-scale simulation of dynamic compaction of oxide and metal powder mixture

    NASA Astrophysics Data System (ADS)

    Kamegai, M.; Walton, Otis R.; Taylor, A. G.

    1989-10-01

    Many features of the dynamic compaction of powders are potentially favorable for use in processing high T(sub c) oxide superconductors. Conventional sintering methods tend to produce unwanted impurities, voids, and oxygen-deficient grain boundaries and have, thus, failed to form bulk oxide superconductors with high critical current. One proposed approach for a dynamic process is to compress a mixture of high purity single crystallite particles and fine silver particles. Computer modeling of dynamic compaction has thus far been limited to bulk simulation of the process by continuum mechanics codes. Results of compaction experiments are not reliably predicted with such techniques because the micro-scale dynamics of powder compaction are only modeled by phenomenological approximation. A micro-scale simulation technique was developed and applied to computer models similar to those of molecular dynamics, which were originally designed to simulate the flow behavior of inelastic, frictional particles. In this method, the oxide grain is represented by a nearly elastic sphere while an individual silver grain is modeled by an aggregate of effective inelastic-frictional particles bound by a prescribed interparticle force. The first 2-D simulation results for a simple configuration (a single aggregate silver grain crushed between two nearly elastic ceramic spheres) are compared with the continuum calculations for the same configuration. This micro-scale simulation technique can be extended to study an assembly of dissimilar grains in 3-D space.

  16. Custom fabrication of reinforced lithium disilicate ceramic ingot.

    PubMed

    Chander, Gopi Naveen; Sasikala, C; Mutukumar, B; Dhanasekar, N

    2016-01-01

    A method of formulating a reinforcement lithium disilicate ceramic ingot was proposed. The ceramic ingot was broken manually with a mallet to finer particles. The sectioned ingot is ball milled along with 10% of nano zirconia by weight to obtain the desired powder. The reinforced powder is condensed in a 5 ml disposable syringe by powder slurry technique. The compacted ceramic were sintered at 900°C to obtain ceramic ingots. The reinforced ceramic ingots were used in pressable ceramic machines to obtain the desired advantages of zirconia reinforcement and pressable ceramic system. PMID:27134457

  17. Custom fabrication of reinforced lithium disilicate ceramic ingot

    PubMed Central

    Chander, Gopi Naveen; Sasikala, C.; Mutukumar, B.; Dhanasekar, N.

    2016-01-01

    A method of formulating a reinforcement lithium disilicate ceramic ingot was proposed. The ceramic ingot was broken manually with a mallet to finer particles. The sectioned ingot is ball milled along with 10% of nano zirconia by weight to obtain the desired powder. The reinforced powder is condensed in a 5 ml disposable syringe by powder slurry technique. The compacted ceramic were sintered at 900°C to obtain ceramic ingots. The reinforced ceramic ingots were used in pressable ceramic machines to obtain the desired advantages of zirconia reinforcement and pressable ceramic system. PMID:27134457

  18. Method for preparing thin-walled ceramic articles of configuration

    DOEpatents

    Holcombe, C.E.; Powell, G.L.

    1975-11-01

    A method for preparing a hollow thin-walled ceramic product is described. Ceramic powder is plasma-sprayed onto a concave surface of a substrate having a coefficient of thermal expansion less than that of the ceramic. The coated substrate is heated to sinter the ceramic and then cooled to effect a separation of the ceramic product from the substrate. (auth)

  19. Wafer and bulk high-purity silicon trace element analysis at the Texas A and M University Nuclear Science Center

    SciTech Connect

    Van Dalsem, Daniel James

    1998-11-24

    A trace element analysis program for wafer and bulk high-purity silicon (Si) samples has been operating at the Texas A and M University Nuclear Science Center (TAMU NSC) since 1996. Samples are irradiated in the NSC's 1-MW TRIGA research reactor at a thermal neutron fluence rate of 10{sup 13} n/cm{sup 2}/s for 14 hours. After an appropriate decay length, bulk samples are chemically etched to remove surface contamination while wafer surfaces are first rinsed with acid to determine surface contamination and then etched to obtain epitaxial layer contamination information. All samples, along with the appropriate etching solutions are analyzed using gamma-ray spectroscopy to quantitatively determine the various radioisotopes created during irradiation. Elements typically determined are antimony (Sb), arsenic (As), bromine (Br), cadmium (Cd), chromium (Cr), cobalt (Co), copper (Cu), gallium (Ga), gold (Au), iron (Fe), molybdenum (Mo), potassium (K), silver (Ag), sodium (Na) tungsten (W) and zinc (Zn). The potential exists to also determine cesium (Cs), iridium (Ir), lanthanum (La), mercury (Hg), rubidium (Rb), scandium (Sc), and zirconium (Zr). Detection limits range from 10{sup 14} down to 10{sup 7} atoms/cm{sup 2} in surface analysis and 10{sup 13} down to 10{sup 8} atoms/cm{sup 3} in bulk Si.

  20. Industrial-scale separation of high-purity single-chirality single-wall carbon nanotubes for biological imaging

    PubMed Central

    Yomogida, Yohei; Tanaka, Takeshi; Zhang, Minfang; Yudasaka, Masako; Wei, Xiaojun; Kataura, Hiromichi

    2016-01-01

    Single-chirality, single-wall carbon nanotubes are desired due to their inherent physical properties and performance characteristics. Here, we demonstrate a chromatographic separation method based on a newly discovered chirality-selective affinity between carbon nanotubes and a gel containing a mixture of the surfactants. In this system, two different selectivities are found: chiral-angle selectivity and diameter selectivity. Since the chirality of nanotubes is determined by the chiral angle and diameter, combining these independent selectivities leads to high-resolution single-chirality separation with milligram-scale throughput and high purity. Furthermore, we present efficient vascular imaging of mice using separated single-chirality (9,4) nanotubes. Due to efficient absorption and emission, blood vessels can be recognized even with the use of ∼100-fold lower injected dose than the reported value for pristine nanotubes. Thus, 1 day of separation provides material for up to 15,000 imaging experiments, which is acceptable for industrial use. PMID:27350127

  1. High-Purity Isolation and Recovery of Circulating Tumor Cells using Conducting Polymer-deposited Microfluidic Device

    PubMed Central

    Jeon, SeungHyun; Hong, WooYoung; Lee, Eun Sook; Cho, Youngnam

    2014-01-01

    We have developed a conductive nano-roughened microfluidic device and demonstrated its use as an electrically modulated capture and release system for studying rare circulating tumor cells (CTCs). The microchannel surfaces were covalently decorated with epithelial cancer-specific anti-EpCAM antibody by electrochemical deposition of biotin-doped polypyrrole (Ppy), followed by the assembly of streptavidin and biotinylated antibody. Our method utilizes the unique topographical features and excellent electrical activity of Ppy for i) surface-induced preferential recognition and release of CTCs, and ii) selective elimination of non-specifically immobilized white blood cells (WBCs), which are capable of high-purity isolation of CTCs. In addition, the direct incorporation of biotin molecules offers good flexibility, because it allows the modification of channel surfaces with diverse antibodies, in addition to anti-EpCAM, for enhanced detection of multiple types of CTCs. By engineering a series of electrical, chemical, and topographical cues, this simple yet efficient device provides a significant advantage to CTC detection technology as compared with other conventional methods. PMID:25250093

  2. Towards a single step process to create high purity gold structures by electron beam induced deposition at room temperature.

    PubMed

    Mansilla, C; Mehendale, S; Mulders, J J L; Trompenaars, P H F

    2016-10-14

    Highly pure metallic structures can be deposited by electron beam induced deposition and they have many important applications in different fields. The organo-metallic precursor is decomposed and deposited under the electron beam, and typically it is purified with post-irradiation in presence of O2. However, this approach limits the purification to the surface of the deposit. Therefore, 'in situ' purification during deposition using simultaneous flows of both O2 and precursor in parallel with two gas injector needles has been tested and verified. To simplify the practical arrangements, a special concentric nozzle has been designed allowing deposition and purification performed together in a single step. With this new device metallic structures with high purity can be obtained more easily, while there is no limit on the height of the structures within a practical time frame. In this work, we summarize the first results obtained for 'in situ' Au purification using this concentric nozzle, which is described in more detail, including flow simulations. The operational parameter space is explored in order to optimize the shape as well as the purity of the deposits, which are evaluated through scanning electron microscope and energy dispersive x-ray spectroscopy measurements, respectively. The observed variations are interpreted in relation to other variables, such as the deposition yield. The resistivity of purified lines is also measured, and the influence of additional post treatments as a last purification step is studied. PMID:27587078

  3. A prototype high-purity germanium detector system with fast photon-counting circuitry for medical imaging.

    PubMed

    Hasegawa, B H; Stebler, B; Rutt, B K; Martinez, A; Gingold, E L; Barker, C S; Faulkner, K G; Cann, C E; Boyd, D P

    1991-01-01

    A data-acquisition system designed for x-ray medical imaging utilizes a segmented high-purity germanium (HPGe) detector array with 2-mm wide and 6-mm thick elements. The detectors are contained within a liquid-nitrogen cryostat designed to minimize heat losses. The 50-ns pulse-shaping time of the preamplifier electronics is selected as the shortest time constant compatible with the 50-ns charge collection time of the detector. This provides the detection system with the fastest count-rate capabilities and immunity from microphonics, with moderate energy resolution performance. A theoretical analysis of the preamplifier electronics shows that its noise performance is limited primarily by its input capacitance, and is independent of detector leakage current up to approximately 100 nA. The system experimentally demonstrates count rates exceeding 1 million counts per second per element with an energy resolution of 7 keV for the 60-keV gamma ray photon from 241Am. The results demonstrate the performance of a data acquisition system utilizing HPGe detector systems which would be suitable for dual-energy imaging as well as systems offering simultaneous x-ray transmission and radionuclide emission imaging. PMID:1961152

  4. Search of neutrino magnetic moments with a high-purity germanium detector at the Kuo-Sheng nuclear power station

    SciTech Connect

    Wong, H. T.; Li, H. B.; Lee, F. S.; Wu, S. C.; Chen, C. P.; Chou, M. H.; Jon, G. C.; Lai, W. P.; Lee, S. C.; Lin, F. K.; Lin, S. K.; Lin, S. T.; Chang, H. M.; Liao, H. Y.; Singh, V.; Chang, C. Y.; Deniz, M.; Fang, J. M.; Su, R. F.; Hu, C. H.

    2007-01-01

    A search of neutrino magnetic moments was carried out at the Kuo-Sheng nuclear power station at a distance of 28 m from the 2.9 GW reactor core. With a high purity germanium detector of mass 1.06 kg surrounded by scintillating NaI(Tl) and CsI(Tl) crystals as anti-Compton detectors, a detection threshold of 5 keV and a background level of 1 kg{sup -1} keV{sup -1} day{sup -1} near threshold were achieved. Details of the reactor neutrino source, experimental hardware, background understanding, and analysis methods are presented. Based on 570.7 and 127.8 days of Reactor ON and OFF data, respectively, at an average Reactor ON electron antineutrino flux of 6.4x10{sup 12} cm{sup -2} s{sup -1}, the limit on the neutrino magnetic moments of {mu}{sub {nu}{sub e}}<7.4x10{sup -11}{mu}{sub B} at 90% confidence level was derived. Indirect bounds on the {nu}{sub e} radiative decay lifetimes were inferred.

  5. Preparation and coagulation efficiency of polyaluminium ferric silicate chloride composite coagulant from wastewater of high-purity graphite production.

    PubMed

    Niu, Xiaoxia; Li, Xili; Zhao, Jihong; Ren, Yigang; Yang, Yanqin

    2011-01-01

    The aim of the present work was to produce a polyaluminium ferric silicate chloride (PAFSiC) coagulant from acidic and alkaline wastewater of purifying graphite by roasting, and subsequently to evaluate coagulation efficiency of the reagent by treating surface water from the Yellow River as well as municipal wastewater in comparison with the conventional coagulant polyaluminium chloride (PAC). The PAFSiC coagulant was prepared by co-polymerization. The effects of (Al+Fe)/Si molar ratio, OH/(Al+Fe) molar ratio (i.e., y value), coagulant dosage and pH value of test suspension on the coagulation behavior of FAFSiC and the stability of the PAFSiC were also examined. Results showed that PAFSiC performed more efficiently than PAC in removing turbidity, chemical oxygen demand (COD), and total phosphate (TP). The PAFSiC with a y value of 2.0 and (Al+Fe)/Si ratio of 5 (PAFSiC 2.0/5) showed excellent coagulation effect for both turbidity and COD, while PAFSiC 1.0/5 was the best for TP. The optimum coagulation pH range of PAFSiC 2.0/5 was 5.0-9.0, slightly wider than that of PAC (6.0-8.0). The process can be easily incorporated into high-purity graphite production plants, thereby reducing wastewater pollution and producing a valuable coagulant. PMID:22125904

  6. Wafer and bulk high-purity silicon trace element analysis at the Texas A&M University Nuclear Science Center

    NASA Astrophysics Data System (ADS)

    Van Dalsem, Daniel James

    1998-11-01

    A trace element analysis program for wafer and bulk high-purity silicon (Si) samples has been operating at the Texas A&M University Nuclear Science Center (TAMU NSC) since 1996. Samples are irradiated in the NSC's 1-MW TRIGA research reactor at a thermal neutron fluence rate of 1013n/cm2/s for 14 hours. After an appropriate decay length, bulk samples are chemically etched to remove surface contamination while wafer surfaces are first rinsed with acid to determine surface contamination and then etched to obtain epitaxial layer contamination information. All samples, along with the appropriate etching solutions are analyzed using gamma-ray spectroscopy to quantitatively determine the various radioisotopes created during irradiation. Elements typically determined are antimony (Sb), arsenic (As), bromine (Br), cadmium (Cd), chromium (Cr), cobalt (Co), copper (Cu), gallium (Ga), gold (Au), iron (Fe), molybdenum (Mo), potassium (K), silver (Ag), sodium (Na) tungsten (W) and zinc (Zn). The potential exists to also determine cesium (Cs), iridium (Ir), lanthanum (La), mercury (Hg), rubidium (Rb), scandium (Sc), and zirconium (Zr). Detection limits range from 1014 down to 107atoms/cm2 in surface analysis and 1013 down to 108atoms/cm3 in bulk Si.

  7. Gas-induced formation of Cu nanoparticle as catalyst for high-purity straight and helical carbon nanofibers.

    PubMed

    Jian, Xian; Jiang, Man; Zhou, Zuowan; Zeng, Qun; Lu, Jun; Wang, Dingchuan; Zhu, Junting; Gou, Jihua; Wang, Yong; Hui, David; Yang, Mingli

    2012-10-23

    The facile preparation of high-purity carbon nanofibers (CNFs) remains challenging due to the high complexity and low controllability in reaction. A novel approach using gas-induced formation of Cu crystals to control the growth of CNFs is developed in this study. By adjusting the atmospheric composition, controllable preparation of Cu nanoparticles (NPs) with specific size and shape is achieved, and they are further used as a catalyst for the growth of straight or helical CNFs with good selectivity and high yield. The preparation of Cu NPs and the formation of CNFs are completed by a one-step process. The inducing effect of N(2), Ar, H(2), and C(2)H(2) on the formation of Cu NPs is systematically investigated through a combined experimental and computational approach. The morphology of CNFs obtained under different conditions is rationalized in terms of Cu NP and CNF growth models. The results suggest that the shapes of CNFs, namely, straight or helical, depend closely on the size, shape, and facet activity of Cu NPs, while such a gas-inducing method offers a simple way to control the formation of Cu NPs. PMID:22963353

  8. Effect of annealing on contact performance and electrical properties of p-type high purity germanium single crystal

    NASA Astrophysics Data System (ADS)

    Yang, Gang; Mei, Dongming; Govani, Jayesh; Wang, Guojian; Khizar, Muhammad

    2013-10-01

    Van de Pauw Hall measurement is an effective method to characterize the properties of semiconductors, such as bulk concentration, mobility, and resistivity, all of which are used to describe the purity level in the semiconductors. However, the performance of the ohmic contacts has a direct impact on the reliability and accuracy of the results obtained from the Van de Pauw Hall measurement. In the present work, the influences of different annealing techniques on the performance of the InSn ohmic contacts have been investigated using a High Purity Germanium (HPGe) crystal sample. The results show that the preferred annealing condition is at 400 °C for 1 hour, which has provided a significant improvement of the InSn contact quality and microscopic homogenization of the impurities in the HPGe crystal. The carrier concentration, charge mobility, and resistivity of the sample annealed at 400 °C for 1 hour are 5.772×1010/cm3, 1.883×104× cm2/Vs, and 5.795×103×Ω cm at 77 K, respectively.

  9. Increased yield of high purity recombinant human brain natriuretic peptide by acid hydrolysis of short fusion partner in Escherichia coli.

    PubMed

    Kanumuri, Radha Madhavi; Bajji, Chitra; Tummuru, Rajesh R; Tatireddigari, Venkat R R Arva; Mangamoori, Lakshmi Narasu; Panati, Kalpana; Narala, Venkata Ramireddy

    2015-07-01

    Recombinant human B-type natriuretic peptide (rhBNP) is a 32-amino acid peptide used to treat congestive heart failure. In this paper, we report a method for the increased production of rhBNP in Escherichia coli with high purity. hBNP was cloned with a short growth hormone fusion partner coupled with a unique acid-labile dipeptide linker to cleave the fusion protein to release the rhBNP. The recombinant fusion protein was expressed as an inclusion body (IB) and the fermentation process was optimized to produce on large scale. The IBs were recovered by cell lysis, and the pure IBs were directly treated with diluted acid to get the target peptide from the fusion protein and the resultant peptide was purified by reversed phase chromatography. The final purity of the rhBNP was more than 99% with yield of 50mg per liter of culture, which is ten times higher than the previous reports. The purified rhBNP exhibited specific biological activity similar to the standard peptide in producing cyclic-guanosine monophosphate. PMID:25823948

  10. High purity GaAs and Al xGa 1-xAs grown by metalorganic molecular beam epitaxy

    NASA Astrophysics Data System (ADS)

    Furuhata, Naoki; Okamoto, Akihiko; Hoshino, Hitoshi

    1990-06-01

    High purity GaAs and Al xGa 1- xAs were grown by metalorganic molecular beam epitaxy (MOMBE) using metalorganic sources and arsenic (As 4). In GaAs growth using triethylgallium (TEG) and As 4, carrier concentrations depended on As 4 pressure and substrate temperatures. Below 1.5 x 10 -4 Torr As 4 pressure, the p-type carrier concentrations decreased with an increase in As 4 pressure. Above 1.5 x 10 -4 Torr As 4 pressure, the epilayer converted from p-type to n-type conductivity. Carrier concentrations decreased with a decrease in substrate temperatures. At 500°C and 1.5 x 10 -4 Torr As 4 pressure, the carrier concentration in the p-type GaAs epilayer exhibited 1.5 x 10 14 cm -3 with a room temperature mobility of 400 cm 2/V.s. Al xGa 1-xAs ( x=0.1-0. .2) was also grown using TEG, three different Al sources (triethylaluminum (TEA), trimethylaluminum (TMA) and dimethylaluminum hydride (DMAH) and As 4. Using TEG, TEA and As 4, the Al 0.15Ga 0.85As epilayer showed p-type conduction with carrier concentration of 1.2x10 15 cm -3 and mobility of 117 cm 2/V.s. This carrier concentration is the lowest value ever reported for Al xGa 1- xAs grown by MOMBE.

  11. Migration of grain boundaries and triple junctions in high-purity aluminum during annealing after slight cold rolling

    SciTech Connect

    Yin, Wenhong; Wang, Weiguo; Fang, Xiaoying; Qin, Congxiang; Xing, Xiaoguang

    2015-09-15

    Grain orientations and grain boundary migrations near triple junctions in a high purity aluminum were analyzed by electron back scattered diffraction. The results indicate that there are good correlations between the Schmid factors or Taylor factors and the misorientation values of point to original point in grains near the triple junctions in a slightly deformed sample. Grains with higher Schmid factors or lower Taylor factors typically correspond to higher misorientation values near the triple junctions. In a subsequent annealing at 400 °C, both grain boundaries and triple junctions migrate, but the former leave ghost lines. During such migration, a grain boundary grows from the grain with lower Schmid factor (higher Taylor factor) into the grain with higher Schmid factor (lower Taylor factor). Usually, the amount of migration of a grain boundary is considerably greater than that of a triple junction, and the grain boundary becomes more curved after migration. These observations indicate that the triple junctions have drag effects on grain boundary migration. - Highlights: • Polycrystalline aluminum with fine grains about 30 μm were used. • Off-line in situ EBSD was used to identify TJs before and after annealing. • Grains with higher SFs have higher misorientation values near TJs after deformation. • Grain boundaries grow from hard grains into soft grains during annealing. • Triple junctions have drag effects on grain boundaries migration.

  12. The Stress Corrosion Crack Growth Rate of Alloy 600 Heat Affected Zones Exposed to High Purity Water

    SciTech Connect

    George A. Young; Nathan Lewis

    2003-04-05

    Grain boundary chromium carbides improve the resistance of nickel based alloys to primary water stress corrosion cracking (PWSCC). However, in weld heat affected zones (HAZ's), thermal cycles from fusion welding can solutionize beneficial grain boundary carbides, produce locally high residual stresses and strains, and promote PWSCC. The present research investigates the crack growth rate of an A600 HAZ as a function of test temperature. The A600 HAZ was fabricated by building up a gas-tungsten-arc-weld deposit of EN82H filler metal onto a mill-annealed A600 plate. Fracture mechanics based, stress corrosion crack growth rate testing was performed in high purity water between 600 F and 680 F at an initial stress intensity factor of 40 ksi {radical}in and at a constant electrochemical potential. The HAZ samples exhibited significant SCC, entirely within the HAZ at all temperatures tested. While the HAZ samples showed the same temperature dependence for SCC as the base material (HAZ: 29.8 {+-} 11.2{sub 95%} kcal/mol vs A600 Base: 35.3 {+-} 2.58{sub 95%} kcal/mol), the crack growth rates were {approx} 30X faster than the A600 base material tested at the same conditions. The increased crack growth rates of the HAZ is attributed to fewer intergranular chromium rich carbides and to increased plastic strain in the HAZ as compared to the unaffected base material.

  13. Search of neutrino magnetic moments with a high-purity germanium detector at the Kuo-Sheng nuclear power station

    NASA Astrophysics Data System (ADS)

    Wong, H. T.; Li, H. B.; Lin, S. T.; Lee, F. S.; Singh, V.; Wu, S. C.; Chang, C. Y.; Chang, H. M.; Chen, C. P.; Chou, M. H.; Deniz, M.; Fang, J. M.; Hu, C. H.; Huang, H. X.; Jon, G. C.; Kuo, W. S.; Lai, W. P.; Lee, S. C.; Li, J.; Liao, H. Y.; Lin, F. K.; Lin, S. K.; Lu, J. Q.; Sheng, H. Y.; Su, R. F.; Tong, W. S.; Xin, B.; Yeh, T. R.; Yue, Q.; Zhou, Z. Y.; Zhuang, B. A.

    2007-01-01

    A search of neutrino magnetic moments was carried out at the Kuo-Sheng nuclear power station at a distance of 28 m from the 2.9 GW reactor core. With a high purity germanium detector of mass 1.06 kg surrounded by scintillating NaI(Tl) and CsI(Tl) crystals as anti-Compton detectors, a detection threshold of 5 keV and a background level of 1kg-1keV-1day-1 near threshold were achieved. Details of the reactor neutrino source, experimental hardware, background understanding, and analysis methods are presented. Based on 570.7 and 127.8 days of Reactor ON and OFF data, respectively, at an average Reactor ON electron antineutrino flux of 6.4×1012cm-2s-1, the limit on the neutrino magnetic moments of μν¯e<7.4×10-11μB at 90% confidence level was derived. Indirect bounds on the ν¯e radiative decay lifetimes were inferred.

  14. Nb-3{sub Sn} layers on high-purity Nb cavities with very high quality factors and accelerating gradients

    SciTech Connect

    G. Muller; Peter Kneisel; D. Mansen; H. Piel; J. Pouryamout; R.W. Roth

    1996-06-01

    We have optimized the vapor diffusion technique to coat high-purity Nb cavities up to RRR=1000 with a micronthick Nb3Sn layer without loss of the thermal stabilization of defects. Systematic measurements on samples have shown no change of RRR of the bulk Nb and homogeneously nucleated growth of the Nb3Sn layers. Rinsing of such layers just with high pressure water resulted in low field emission activity and residual surface resistance values in the nW range, i.e. comparable to the best Nb surfaces. Single-cell 1.5 GHz cavities provided Q0 values up to 1011 at 2 K and above 1010 at 4.2 K, which stayed nearly constant up to peak electric surface fields of 10 MV/m but decreased to about 109 at 20 MV/m. No field emission and no quench could be observed in these cavities up to the maximum achievable accelerating gradients of about 15 MV/m at 2 K as limited by the available rf power. The performance of the Nb3Sn cavities at 4.2 K exceeds the design value of the CEBAF Nb cavities at 2 K. First results on a five-cell cavity are promising.

  15. Process for fabrication of large titanium diboride ceramic bodies

    DOEpatents

    Moorhead, Arthur J.; Bomar, E. S.; Becher, Paul F.

    1989-01-01

    A process for manufacturing large, fully dense, high purity TiB.sub.2 articles by pressing powders with a sintering aid at relatively low temperatures to reduce grain growth. The process requires stringent temperature and pressure applications in the hot-pressing step to ensure maximum removal of sintering aid and to avoid damage to the fabricated article or the die.

  16. NHEXAS PHASE I MARYLAND STUDY--STANDARD OPERATING PROCEDURE FOR OPERATION OF AN ULTRA-HIGH PURITY WATER SYSTEM (L03)

    EPA Science Inventory

    The purpose of this SOP is to ensure that all procedures, field and lab, utilize the highest quality water needed or available when sampling or analyzing NHEXAS samples. Using ultra-high-purity water (Milli-Q, Nanopure, or its equivalent with a resistivity more than 18 megaohm) ...

  17. Low temperature joining of ceramic composites

    DOEpatents

    Barton, Thomas J.; Anderson, Iver E.; Ijadi-Maghsoodi, Sina; Nosrati, Mohammad; Unal, Ozer

    1999-07-13

    A method of joining similar or dissimilar ceramic and ceramic composite materials, such as SiC continuous fiber ceramic composites, at relatively low joining temperatures uses a solventless, three component bonding agent effective to promote mechanical bond toughness and elevated temperature strength to operating temperatures of approximately 1200 degrees C. The bonding agent comprises a preceramic precursor, an aluminum bearing powder, such as aluminum alloy powder, and mixtures of aluminum metal or alloy powders with another powder, and and boron powder in selected proportions. The bonding agent is disposed as an interlayer between similar or dissimilar ceramic or ceramic composite materials to be joined and is heated in ambient air or inert atmosphere to a temperature not exceeding about 1200 degrees C. to form a strong and tough bond joint between the materials. The bond joint produced is characterized by a composite joint microstructure having relatively soft, compliant aluminum bearing particulate regions dispersed in a ceramic matrix.

  18. Low temperature joining of ceramic composites

    DOEpatents

    Barton, T.J.; Anderson, I.E.; Ijadi-Maghsoodi, S.; Nosrati, M.; Unal, O.

    1999-01-12

    A method of joining similar or dissimilar ceramic and ceramic composite materials, such as SiC continuous fiber ceramic composites, at relatively low joining temperatures uses a solventless, three component bonding agent effective to promote mechanical bond toughness and elevated temperature strength to operating temperatures of approximately 1200 degrees C. The bonding agent comprises a preceramic precursor, an aluminum bearing powder, such as aluminum alloy powder, and mixtures of aluminum metal or alloy powders with another powder, and boron powder in selected proportions. The bonding agent is disposed as an interlayer between similar or dissimilar ceramic or ceramic composite materials to be joined and is heated in ambient air or inert atmosphere to a temperature not exceeding about 1200 degrees C. to form a strong and tough bond joint between the materials. The bond joint produced is characterized by a composite joint microstructure having relatively soft, compliant aluminum bearing particulate regions dispersed in a ceramic matrix. 3 figs.

  19. Low temperature joining of ceramic composites

    DOEpatents

    Barton, T.J.; Anderson, I.E.; Ijadi-Maghsoodi, S.; Nosrati, M.; Unal, O.

    1999-07-13

    A method of joining similar or dissimilar ceramic and ceramic composite materials, such as SiC continuous fiber ceramic composites, at relatively low joining temperatures uses a solventless, three component bonding agent effective to promote mechanical bond toughness and elevated temperature strength to operating temperatures of approximately 1200 C. The bonding agent comprises a preceramic precursor, an aluminum bearing powder, such as aluminum alloy powder, and mixtures of aluminum metal or alloy powders with another powder, and boron powder in selected proportions. The bonding agent is disposed as an interlayer between similar or dissimilar ceramic or ceramic composite materials to be joined and is heated in ambient air or inert atmosphere to a temperature not exceeding about 1200 C to form a strong and tough bond joint between the materials. The bond joint produced is characterized by a composite joint microstructure having relatively soft, compliant aluminum bearing particulate regions dispersed in a ceramic matrix. 3 figs.

  20. Stress corrosion cracking of A471 turbine disk steels: Effects of dissolved oxygen and carbon dioxide in high-purity water: Final report

    SciTech Connect

    Eiselstein, L.E.; Caligiuri, R.D.

    1987-06-01

    Experiments were performed to determine the effect of dilute impurities in high purity water on the rate of initiation and growth of stress corrosion cracks in NiCrMoV steels. 3.5 NiCrMoV steels of commercial quality, high purity, and high purity with intentionally added tramp elements were investigated. Dissolved oxygen and carbon dioxide were the primary water impurities investigated. The tests were conducted on constant load, smooth bar tensile specimens of the NiCrMoV steels in flowing 160C high purity water containing various dilute levels of impurities. It was determined that the initiation rate is very sensitive to changes in dissolved oxygen content; the peak initiation rate are achieved between 20 and 80 ppB dissolved oxygen. The initiation rate is less sensitive to dissolved CO2 content. The crack growth rate in high purity water is only weakly dependent on dissolved O2 and CO2. This work shows that the crack growth rate is strongly dependent on the yield strength (and therefore the microstructure that develops as a result of tempering) of the turbine disc alloy, whereas the initiation rate is only weakly dependent on material yield strength. In addition, crack growth rates decrease as grain sizes are decreased. In general, crack growth rates are very slow (less than 10 m/s) in these dilute environments in materials with yield strengths below 690 Mpa (100 ksi). The results of these experiments indicate that a hydrogen-assisted process may be an important cracking mechanism in these alloys in these dilute environments. Implication of a hydrogen-assisted mechanism could have important consequences in the design and selection of turbine disc alloys.

  1. Refinement of Eutectic Si in High Purity Al-5Si Alloys with Combined Ca and P Additions

    NASA Astrophysics Data System (ADS)

    Ludwig, Thomas Hartmut; Li, Jiehua; Schaffer, Paul Louis; Schumacher, Peter; Arnberg, Lars

    2015-01-01

    The effects of combined additions of Ca and P on the eutectic Si in a series of high purity Al-5 wt pct Si alloys have been investigated with the entrained droplet technique and complementary sets of conventional castings. Differential scanning calorimetry (DSC) and thermal analysis were used to investigate the eutectic droplet undercooling and the recalescence undercooling, respectively. Optical microscopy, SEM, EPMA, and TEM were employed to characterize the resultant microstructures. It was found that 250 ppm Ca addition to Al-5Si wt pct alloys with higher P contents leads to a significant increase of the eutectic droplet undercooling. For low or moderate cooling rates, the TEM results underline that Ca additions do not promote Si twinning. Thus, a higher twin density cannot be expected in Ca containing Al-Si alloys after, e.g., sand casting. Consequently, a refinement of the eutectic Si from coarse flake-like to fine plate-like structure, rather than a modification of the eutectic Si to a fibrous morphology, was achieved. This strongly indicates that the main purpose of Ca additions is to counteract the coarsening effect of the eutectic Si imposed by higher P concentrations. Significant multiple Si twinning was observed in melt-spun condition; however, this can be attributed to the higher cooling rate. After DSC heating (slow cooling), most of Si twins disappeared. Thus, the well-accepted impurity-induced twinning mechanism may be not valid in the case of Ca addition. The possible refinement mechanisms were discussed in terms of nucleation and growth of eutectic Si. We propose that the pre-eutectic Al2Si2Ca phase and preferential formation of Ca3P2 deactivate impurity particles, most likely AlP, poisoning the nucleation sites for eutectic Si.

  2. Synthesis, thermal and spectral characterization of nanosized Ni xMg 1- xAl 2O 4 powders as new ceramic pigments via combustion route using 3-methylpyrozole-5-one as fuel

    NASA Astrophysics Data System (ADS)

    Ahmed, Ibrahim S.; Shama, Sayed A.; Dessouki, Hassan A.; Ali, Ayman A.

    2011-10-01

    New Ni xMg 1- xAl 2O 4 nanosized in different composition (0.1 ≤ x ≤ 0.8) powders have been synthesized successively for first time by using low temperature combustion reaction (LTCR) of corresponding metal chlorides, carbonates and nitrates as salts with 3-methylpyrozole-5-one (3MP5O) as fuel at 300 °C in open air furnace. Magnesium aluminate spinel (MgAl 2O 4) was used as crystalline host network for the synthesis of nickel-based nano ceramic pigments. The structure of prepared samples was characterized by using different techniques such as thermal analysis (TG-DTG/DTA), X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and transmission electron microscopy (TEM). UV/Visible and Diffuse reflectance spectroscopy (DRS) using CIE- L* a* b* parameters methods have been used for color measurements. The obtained results reveal that Ni xMg 1- xAl 2O 4 powder of samples is formed in the single crystalline and pure phase with average particle size of 6.35-33.11 nm in the temperature range 500-1200 °C. The density, particle size, shape and color are determined for all prepared samples with different calcination time and temperature.

  3. Synthesis, thermal and spectral characterization of nanosized Ni(x)Mg(1-x)Al2O4 powders as new ceramic pigments via combustion route using 3-methylpyrozole-5-one as fuel.

    PubMed

    Ahmed, Ibrahim S; Shama, Sayed A; Dessouki, Hassan A; Ali, Ayman A

    2011-10-15

    New Ni(x)Mg(1-x)Al(2)O(4) nanosized in different composition (0.1≤x≤0.8) powders have been synthesized successively for first time by using low temperature combustion reaction (LTCR) of corresponding metal chlorides, carbonates and nitrates as salts with 3-methylpyrozole-5-one (3MP5O) as fuel at 300°C in open air furnace. Magnesium aluminate spinel (MgAl(2)O(4)) was used as crystalline host network for the synthesis of nickel-based nano ceramic pigments. The structure of prepared samples was characterized by using different techniques such as thermal analysis (TG-DTG/DTA), X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and transmission electron microscopy (TEM). UV/Visible and Diffuse reflectance spectroscopy (DRS) using CIE-L*a*b* parameters methods have been used for color measurements. The obtained results reveal that Ni(x)Mg(1-x)Al(2)O(4) powder of samples is formed in the single crystalline and pure phase with average particle size of 6.35-33.11 nm in the temperature range 500-1200°C. The density, particle size, shape and color are determined for all prepared samples with different calcination time and temperature. PMID:21783407

  4. Lanthanide (Nd, Gd) compounds with garnet and monazite structures. Powders synthesis by "wet" chemistry to sintering ceramics by Spark Plasma Sintering

    NASA Astrophysics Data System (ADS)

    Potanina, Ekaterina; Golovkina, Ludmila; Orlova, Albina; Nokhrin, Aleksey; Boldin, Maksim; Sakharov, Nikita

    2016-05-01

    Complex oxide Y2.5Nd0.5Al5O12 with garnet structure and phosphates NdPO4 and GdPO4 with monazite structure were obtained by using precipitation methods. Ceramics Y2.5Nd0.5Al5O12 and NdPO4 were processed by Spark Plasma Sintering (SPS). Relative density more 98%, sintering time did not exceed 8 min, sintering temperature 1330-1390 °C. Leaching rates of elements from ceramics were 10-6-10-7 g/(cm2 d). The process of ceramics sintering has two-stage character: the first step of sintering-compaction process is related to the plastic flow of the material, the second step-to the process of grain boundary diffusion and grain growth.

  5. Effect of Rare Earth Oxide Content on Nanograined Base Metal Electrode Multilayer Ceramic Capacitor Powder Prepared by Aqueous Chemical Coating Method

    NASA Astrophysics Data System (ADS)

    Zhang, Yichi; Wang, Xiaohui; Kim, Jinyong; Li, Longtu

    2013-02-01

    The aqueous chemical coating route is highly effective in preparing BaTiO3 nanoparticles uniformly coated with additives. Such nanoparticles can be used to produce nano-grained temperature stable BaTiO3 ceramics with core-shell structure, fulfilling the need of next-generation ultrathin layer base metal electrode (BME) multilayer ceramic capacitors (MLCCs). Rare earth oxides are an important class of additives owing to their ability to fulfill both donor and acceptor roles. In this paper, the effects of Y2O3 and Ho2O3 co-dopant content on dielectric and microstructural properties were investigated. By applying chemical coating, BaTiO3-based high performance temperature stabilized ceramics with the average grain size of about 130 nm, which met the requirement of next generation BME MLCCs, were obtained.

  6. Ceramic/ceramic total hip arthroplasty.

    PubMed

    Bizot, P; Nizard, R; Lerouge, S; Prudhommeaux, F; Sedel, L

    2000-01-01

    Alumina-on-alumina total hip arthroplasty has been used for 30 years, mainly in Europe. The theoretical advantages of this combination are represented by its remarkable sliding characteristics, its very low wear debris generation, and its sufficient fracture toughness. These advantages are achieved if the material is properly controlled with high density, high purity, and small grains. The authors summarize the results obtained with ceramic/ceramic total hip arthroplasty. Information is provided about in vivo behavior regarding wear debris characterization and quantification, and histological tissue examinations for inflammatory reactions, which were not encountered except when alumina debris was mixed with metal or cement. Modification of socket fixation resulted in improved clinical outcomes. With a press-fit metal shell and an alumina liner utilized for 10 years, the results are excellent especially in a young and active population. Alumina-on-alumina seems at the moment to be one of the best choices when a total hip arthroplasty has to be performed in young and active patients. PMID:11180930

  7. Couples Magnetic and Structural Transitions in High-Purity Dy and Gd5SbxGe4-x

    SciTech Connect

    Alexander S. Chernyshov

    2006-08-09

    Magnetic materials exhibiting magnetic phase transitions simultaneously with structural rearrangements of their crystal lattices hold a promise for numerous applications including magnetic refrigeration, magnetomechanical devices and sensors. We undertook a detailed study of a single crystal of dysprosium metal, which is a classical example of a system where magnetic and crystallographic sublattices can be either coupled or decoupled from one another. Magnetocaloric effect, magnetization, ac magnetic susceptibility, and heat capacity of high purity single crystals of dysprosium have been investigated over broad temperature and magnetic field intervals with the magnetic field vector parallel to either the a- or c-axes of the crystal. Notable differences in the behavior of the physical properties when compared to Dy samples studied in the past have been observed between 110 K and 125 K, and between 178 K and {approx}210 K. A plausible mechanism based on the formation of antiferromagnetic clusters in the impure Dy has been suggested in order to explain the reduction of the magnetocaloric effect in the vicinity of the Neel point. Experimental and theoretical investigations of the influence of commensurability effects on the magnetic phase diagram and the value of the magnetocaloric effect have been conducted. The presence of newly found anomalies in the physical properties has been considered as evidence of previously unreported states of Dy. The refined magnetic phase diagram of dysprosium with the magnetic field vector parallel to the a-axis of a crystal has been constructed and discussed. The magnetic and crystallographic properties of Gd{sub 5}Sb{sub x}Ge{sub 4-x} pseudo-binary system were studied by x-ray diffraction (at room temperature), heat capacity, ac-magnetic susceptibility, and magnetization in the temperature interval 5-320 K in magnetic fields up to 100 kOe. The magnetic properties of three composition (x = 0.5, 1,2) were examined in detail. The Gd{sub 5

  8. Ceramic Stereolithography: Additive Manufacturing for Ceramics by Photopolymerization

    NASA Astrophysics Data System (ADS)

    Halloran, John W.

    2016-07-01

    Ceramic stereolithography and related additive manufacturing methods involving photopolymerization of ceramic powder suspensions are reviewed in terms of the capabilities of current devices. The practical fundamentals of the cure depth, cure width, and cure profile are related to the optical properties of the monomer, ceramic, and photo-active components. Postpolymerization steps, including harvesting and cleaning the objects, binder burnout, and sintering, are discussed and compared with conventional methods. The prospects for practical manufacturing are discussed.

  9. Improved compaction of ZnO nano-powder triggered by the presence of acetate and its effect on sintering

    NASA Astrophysics Data System (ADS)

    Dargatz, Benjamin; Gonzalez-Julian, Jesus; Guillon, Olivier

    2015-04-01

    The retention of nanocrystallinity in dense ceramic materials is still a challenge, even with the application of external pressure during sintering. The compaction behavior of high purity and acetate enriched zinc oxide (ZnO) nano-powders was investigated. It was found that acetate in combination with water plays a key role during the compaction into green bodies at moderate temperatures. Application of constant pressure resulted in a homogeneous green body with superior packing density (86% of theoretical value) at moderate temperature (85 °C) in the presence of water. In contrast, no improvement in density could be achieved if pure ZnO powder was used. This compaction behavior offers superior packing of the particles, resulting in a high relative density of the consolidated compact with negligible coarsening. Dissolution accompanying creep diffusion based matter transport is suggested to strongly support reorientation of ZnO particles towards densities beyond the theoretical limit for packing of ideal monosized spheres. Finally, the sintering trajectory reveals that grain growth is retarded compared to conventional processing up to 90% of theoretical density. Moreover, nearly no radial shrinkage was observed after sinter-forging for bodies performed with this advanced processing method.

  10. Synthesis of Nano-Polycrystalline Synroc-B Powders as a High Level Radioactive Wastes Ceramic Forms by a Solution Combustion Synthesis.

    PubMed

    Han, Young-Min; Lee, Sang-Jin; Kim, Yeon-Ku; Jung, Choong-Hwan

    2016-02-01

    Synroc (Synthetic Rock) consists of four main titanate phases: peroveskite (CaTiO3), zirconolite (CaZrTi2O7), hollandite (BaAl2Ti6O16) and rutile (TiO2). Nano-polycrystalline synroc powders were made by a synthesis combustion process. The combustion process, an externally initiated reaction is self-sustained owing to the exothermic reaction. A significant volume of gas is evolved during the combustion reaction and leads to loosely agglomerated powders. This exothermic reaction provides necessary heat to further carry the reaction in forward direction to produce nanocrystalline powders as the final product. Glycine is used as a fuel, being oxidized by nitrate ions. It is inexpensive, has high energy efficiency, fast heating rates, short reaction times and high compositional homogeneity. In this study, combustion synthesis of nano-sized synroc-B powder is introduced. The fabrication of synroc-B powder result of observation XRD were prepared for polycrystalline (perovskite, zirconolite, hollandite, rutile) structures. The characterization of the synthesized powders is conducted by using XRD, SEM/EDS and TEM. PMID:27433644

  11. Sol-gel synthesis and characterizations of crystalline NaGd(WO4)2 powder for anisotropic transparent ceramic laser application

    NASA Astrophysics Data System (ADS)

    Durairajan, A.; Thangaraju, D.; Balaji, D.; Moorthy Babu, S.

    2013-02-01

    NaGd(WO4)2 powders were synthesized at different pH (3.5, 4.5, 5.5, 6.5 and 7.5) values by conventional Pechini method. Sodium and gadolinium nitrate salts and ammonium paratungstate are used as starting precursors. Metal cations were chelated by citric acid and individual citrates were bound together with ethylene glycol. Synthesized gel was analyzed using differential thermal analysis (DTA), thermo gravimetric (TG) and FT-IR spectroscopy to understand the degradation of gel and formation of metal citrates. Calcined powders (250, 600, 700 and 800 °C) were characterized by powder XRD, FT-IR, Raman and FE-SEM analysis. The temperature dependent phase formation was examined by powder XRD. The morphological changes at different pH derived powders were observed with FE-SEM micrographs. Stepwise organic liberation with respect to temperature and presence of carbon content in the pre-fired powder were analyzed using FT-IR analysis. Raman spectrum reveals disordered tungstate vibrations in the NGW matrix.

  12. Efficient synthesis of high purity homo-arm and mikto-arm poly(ethylene glycol) stars using epoxide and azide-alkyne coupling chemistry.

    PubMed

    Zhang, Boyu; Zhang, Hong; Elupula, Ravinder; Alb, Alina M; Grayson, Scott M

    2014-01-01

    High purity homo-arm and mikto-arm poly(ethylene glycol) (PEG) stars are successfully prepared by the combination of epoxide ring-openings and azide-alkyne click reactions. First, monohydroxy-PEG was modified via epoxide chemistry to bear one hydroxyl and one azide functionality at the same end. An alkyne-functionalized PEG chain was then coupled to the azide. Subsequently, the remaining hydroxyl could be reactivated to an azide again and again to enable stepwise addition of alkyne-functionalized polymer arms. The use of efficient reactions for this iterative route provides star polymers with an exact number of arms, and a tailorable degree of polymerization for each arm. Detailed characterization confirms the high purity of multi-arm polyethylene glycol products. PMID:24272944

  13. Method of forming ceramic bricks

    DOEpatents

    Poeppel, Roger B.; Claar, Terry D.; Silkowski, Peter

    1988-01-01

    A method for forming free standing ceramic bricks for use as tritium breeder material is disclosed. Aqueous solutions of sodium carbonate and potassium carbonate are mixed with an organic hydrocolloid dispersion and powdered lithium carbonate, spray dried, and ceramic bricks formed by molding in a die and firing.

  14. Method of forming ceramic bricks

    DOEpatents

    Poeppel, Roger B.; Claar, Terry D.; Silkowski, Peter

    1988-09-06

    A method for forming free standing ceramic bricks for use as tritium breeder material is disclosed. Aqueous solutions of sodium carbonate and potassium carbonate are mixed with an organic hydrocolloid dispersion and powdered lithium carbonate, spray dried, and ceramic bricks formed by molding in a die and firing.

  15. Method of forming ceramic bricks

    DOEpatents

    Poeppel, R.B.; Claar, T.D.; Silkowski, P.

    1987-04-22

    A method for forming free standing ceramic bricks for use as tritium breeder material is disclosed. Aqueous solutions of sodium carbonate and potassium carbonate are mixed with an organic hydrocolloid dispersion and powdered lithium carbonate, spray dried, and ceramic bricks formed by molding in a die and firing.

  16. Low temperature joining of ceramic composites

    DOEpatents

    Barton, Thomas J.; Anderson, Iver E.; Ijadi-Maghsoodi, Sina; Nosrati, Mohammad; Unal, Ozer

    2001-04-10

    A method of joining similar or dissimilar ceramic and ceramic composite materials, such as SiC continuous fiber ceramic composites, at relatively low joining temperatures uses a solventless, three component bonding agent effective to promote mechanical bond toughness and elevated temperature strength to operating temperatures of approximately 1200 degrees C. The bonding agent comprises a preceramic precursor, an aluminum bearing powder, such as aluminum alloy powder, and mixtures of aluminum metal or alloy powders with another powder, and and boron powder in selected proportions. The bonding agent is disposed as an interlayer between similar or dissimilar ceramic or cermaic composite materials to be joined and is heated in ambient air or inert atmosphere to a temperature not exceeding about 1200 degrees C. to form a strong and tough bond joint between the materials. The bond joint produced is characterized by a composite joint microstructure having relatively soft, compliant aluminum bearing particulate regions dispersed in a ceramic matrix.

  17. Low temperature joining of ceramic composites

    DOEpatents

    Barton, Thomas J.; Anderson, Iver E.; Ijadi-Maghsoodi, Sina; Nosrati, Mohammad; Unal, Ozer

    1999-01-12

    A method of joining similar or dissimilar ceramic and ceramic composite materials, such as SiC continuous fiber ceramic composites, at relatively low joining temperatures uses a solventless, three component bonding agent effective to promote mechanical bond toughness and elevated temperature strength to operating temperatures of approximately 1200 degrees C. The bonding agent comprises a preceramic precursor, an aluminum bearing powder, such as aluminum alloy powder, and mixtures of aluminum metal or alloy powders with another powder, and and boron powder in selected proportions. The bonding agent is disposed as an interlayer between similar or dissimilar ceramic or cermaic composite materials to be joined and is heated in ambient air or inert atmosphere to a temperature not exceeding about 1200 degrees C. to form a strong and tough bond joint between the materials. The bond joint produced is characterized by a composite joint microstructure having relatively soft, compliant aluminum bearing particulate regions dispersed in a ceramic matrix.

  18. Fabrication of large ceramic electrolyte disks

    NASA Technical Reports Server (NTRS)

    Ring, S. A.

    1972-01-01

    Process for sintering compressed ceramic powders produces large ceramic disks for use as electrolytes in high-temperature electrolytic cells. Thin, strain-free uniformly dense disks as large as 30 cm squared have been fabricated by slicing ceramic slugs produced by this technique.

  19. Effect of small additions of silicon, iron, and aluminum on the room-temperature tensile properties of high-purity uranium

    SciTech Connect

    Ludwig, R.L.

    1983-11-14

    Eleven binary and ternary alloys of uranium and very low concentrations of iron, silicon, and aluminum were prepared and tested for room-temperature tensile properties after various heat treatments. A yield strength approximately double that of high-purity derby uranium was obtained from a U-400 ppM Si-200 ppM Fe alloy after beta solution treatment and alpha aging. Higher silicon plus iron alloy contents resulted in increased yield strength, but showed an unacceptable loss of ductility.

  20. Novel, Ceramic Membrane System For Hydrogen Separation

    SciTech Connect

    Elangovan, S.

    2012-12-31

    Separation of hydrogen from coal gas represents one of the most promising ways to produce alternative sources of fuel. Ceramatec, teamed with CoorsTek and Sandia National Laboratories has developed materials technology for a pressure driven, high temperature proton-electron mixed conducting membrane system to remove hydrogen from the syngas. This system separates high purity hydrogen and isolates high pressure CO{sub 2} as the retentate, which is amenable to low cost capture and transport to storage sites. The team demonstrated a highly efficient, pressure-driven hydrogen separation membrane to generate high purity hydrogen from syngas using a novel ceramic-ceramic composite membrane. Recognizing the benefits and limitations of present membrane systems, the all-ceramic system has been developed to address the key technical challenges related to materials performance under actual operating conditions, while retaining the advantages of thermal and process compatibility offered by the ceramic membranes. The feasibility of the concept has already been demonstrated at Ceramatec. This project developed advanced materials composition for potential integration with water gas shift rectors to maximize the hydrogenproduction.

  1. Preparation of High Purity Crystalline Silicon by Electro-Catalytic Reduction of Sodium Hexafluorosilicate with Sodium below 180°C

    PubMed Central

    Chen, Yuan; Liu, Yang; Wang, Xin; Li, Kai; Chen, Pu

    2014-01-01

    The growing field of silicon solar cells requires a substantial reduction in the cost of semiconductor grade silicon, which has been mainly produced by the rod-based Siemens method. Because silicon can react with almost all of the elements and form a number of alloys at high temperatures, it is highly desired to obtain high purity crystalline silicon at relatively low temperatures through low cost process. Here we report a fast, complete and inexpensive reduction method for converting sodium hexafluorosilicate into silicon at a relatively low reaction temperature (∼200°C). This temperature could be further decreased to less than 180°C in combination with an electrochemical approach. The residue sodium fluoride is dissolved away by pure water and hydrochloric acid solution in later purifying processes below 15°C. High purity silicon in particle form can be obtained. The relative simplicity of this method might lead to a low cost process in producing high purity silicon. PMID:25153509

  2. Preparation of high purity crystalline silicon by electro-catalytic reduction of sodium hexafluorosilicate with sodium below 180 °C.

    PubMed

    Chen, Yuan; Liu, Yang; Wang, Xin; Li, Kai; Chen, Pu

    2014-01-01

    The growing field of silicon solar cells requires a substantial reduction in the cost of semiconductor grade silicon, which has been mainly produced by the rod-based Siemens method. Because silicon can react with almost all of the elements and form a number of alloys at high temperatures, it is highly desired to obtain high purity crystalline silicon at relatively low temperatures through low cost process. Here we report a fast, complete and inexpensive reduction method for converting sodium hexafluorosilicate into silicon at a relatively low reaction temperature (∼ 200 °C). This temperature could be further decreased to less than 180 °C in combination with an electrochemical approach. The residue sodium fluoride is dissolved away by pure water and hydrochloric acid solution in later purifying processes below 15 °C. High purity silicon in particle form can be obtained. The relative simplicity of this method might lead to a low cost process in producing high purity silicon. PMID:25153509

  3. Effect of starting powder characteristics on density, microstructure and low temperature oxidation behavior of a Si3N48w/o Y2O3 ceramic

    NASA Technical Reports Server (NTRS)

    Schuon, S.; Dutta, S.

    1980-01-01

    The densification and oxidation behavior of Si3N4 - 8w/oY2O3 prepared from three commercial starting powders were studied. Bars of SN 402, SN 502, and CP 85/15 were sintered for 3 to 4.5 hours at 1750 C. A second set was hot pressed for 2 hours at 1750 C. The microstructures were studied by transmission electron microscopy and scanning electron microscopy, densities were determined, and the phase compositions were determined by X-ray diffraction. Densification and microstructure were greatly influenced by the starting powder morphology and impurity content. Although SN 402 exhibited the maximum weight lose, the highest sintered and hot pressed densities were obtained with this powder. All powders had both equiaxed and elongated grains. Sintered bars were composed of beta silicon nitride and n-melelite. In contrast, hot pressed bars contained beta silicon nitride, H-phase, and J-phase, but no melelite. Yttria distribution in sintered bars was related to the presence of cation impurities such as Ca, Fe, and Mg. A limited oxidation study at 750 C in air showed no instability in these Si3N4 - 8 w/oY2O3 specimens, regardless of startin powder.

  4. Method for synthesizing ultrafine powder materials

    DOEpatents

    Buss, Richard J.; Ho, Pauline

    1988-01-01

    A method for synthesizing ultrafine powder materials, for example, ceramic and metal powders, comprises admitting gaseous reactants from which the powder material is to be formed into a vacuum reaction chamber maintained at a pressure less than atmospheric and at a temperature less than about 400.degree. K. (127.degree.C.). The gaseous reactants are directed through a glow discharge provided in the vacuum reaction chamber to form the ultrafine powder material.

  5. A study on in situ growth of TaC whiskers in Al{sub 2}O{sub 3} matrix powder for ceramic cutting tools

    SciTech Connect

    Zhao, Guolong; Huang, Chuanzhen; Liu, Hanlian; Xu, Liang; Chong, Xuewen; Zou, Bin; Zhu, Hongtao

    2012-08-15

    Graphical abstract: In situ growth of TaC whiskers (TaC{sub w}) was synthesized in an α-Al{sub 2}O{sub 3} matrix powder via a carbothermal reduction technique. The whiskers were 0.2–0.5 μm in diameter and 5–15 μm in length; they were straight and had smooth surfaces. Highlights: ► In situ growth of TaC whiskers was synthesized in an α-Al{sub 2}O{sub 3} matrix powder. ► The wet mixing method and 1450 °C were suitable for whiskers growth. ► The growth of TaC whiskers is not influenced by the Al{sub 2}O{sub 3} powder. ► The major impurities were TaC particles, nickel and unreacted carbon. -- Abstract: In situ growth of tantalum carbide (TaC) whiskers was synthesized in an α-Al{sub 2}O{sub 3} matrix powder via a carbothermal reduction technique within a temperature range of 1350–1500 °C in an argon atmosphere. The starting materials consisted of Ta{sub 2}O{sub 5}, C, Ni and NaCl powders. Different mixing methods and various reaction temperatures were employed. Most of the prepared whiskers were 0.2–0.5 μm in diameter and 5–15 μm in length. The reaction temperature of 1400–1450 °C was suitable for the growth of TaC whiskers and a wet mixing method was beneficial to increase the whisker yield. Some of the whiskers exhibited the needle shape while others exhibited the screw shape. The growth mechanism of the whiskers was a complex mechanism involving a helical screw dislocation mechanism and a vapor–liquid–solid process. No obvious influences of the Al{sub 2}O{sub 3} matrix powder on the growth of TaC whiskers were found and the major impurities in the obtained powder were TaC particles, nickel and unreacted carbon.

  6. PROCESS OF FORMING POWDERED MATERIAL

    DOEpatents

    Glatter, J.; Schaner, B.E.

    1961-07-14

    A process of forming high-density compacts of a powdered ceramic material is described by agglomerating the powdered ceramic material with a heat- decompossble binder, adding a heat-decompossble lubricant to the agglomerated material, placing a quantity of the material into a die cavity, pressing the material to form a compact, pretreating the compacts in a nonoxidizing atmosphere to remove the binder and lubricant, and sintering the compacts. When this process is used for making nuclear reactor fuel elements, the ceramic material is an oxide powder of a fissionsble material and after forming, the compacts are placed in a cladding tube which is closed at its ends by vapor tight end caps, so that the sintered compacts are held in close contact with each other and with the interior wall of the cladding tube.

  7. MESOSCALE SIMULATIONS OF POWDER COMPACTION

    SciTech Connect

    Lomov, Ilya; Fujino, Don; Antoun, Tarabay; Liu, Benjamin

    2009-12-28

    Mesoscale 3D simulations of shock compaction of metal and ceramic powders have been performed with an Eulerian hydrocode GEODYN. The approach was validated by simulating a well-characterized shock compaction experiment of a porous ductile metal. Simulation results using the Steinberg material model and handbook values for solid 2024 aluminum showed good agreement with experimental compaction curves and wave profiles. Brittle ceramic materials are not as well studied as metals, so a simple material model for solid ceramic (tungsten carbide) has been calibrated to match experimental compaction curves. Direct simulations of gas gun experiments with ceramic powders have been performed and showed good agreement with experimental data. The numerical shock wave profile has same character and thickness as that measured experimentally using VISAR. The numerical results show reshock states above the single-shock Hugoniot line as observed in experiments. We found that for good quantitative agreement with experiments 3D simulations are essential.

  8. Mesoscale Simulations of Powder Compaction

    NASA Astrophysics Data System (ADS)

    Lomov, Ilya.; Fujino, Don; Antoun, Tarabay; Liu, Benjamin

    2009-12-01

    Mesoscale 3D simulations of shock compaction of metal and ceramic powders have been performed with an Eulerian hydrocode GEODYN. The approach was validated by simulating a well-characterized shock compaction experiment of a porous ductile metal. Simulation results using the Steinberg material model and handbook values for solid 2024 aluminum showed good agreement with experimental compaction curves and wave profiles. Brittle ceramic materials are not as well studied as metals, so a simple material model for solid ceramic (tungsten carbide) has been calibrated to match experimental compaction curves. Direct simulations of gas gun experiments with ceramic powders have been performed and showed good agreement with experimental data. The numerical shock wave profile has same character and thickness as that measured experimentally using VISAR. The numerical results show reshock states above the single-shock Hugoniot line as observed in experiments. We found that for good quantitative agreement with experiments 3D simulations are essential.

  9. Synthesis of few-layered, high-purity graphene oxide sheets from different graphite sources for biology

    NASA Astrophysics Data System (ADS)

    Jasim, Dhifaf A.; Lozano, Neus; Kostarelos, Kostas

    2016-03-01

    This work aimed to interrogate the role that the starting graphitic material played on the physicochemical properties of graphene oxide (GO) sheets and their impact on mammalian cell viability following exposure to those flakes. Three different GO thin sheets were synthesised from three starting graphite material: flakes (GO-f), ground (GO-g) and powder (GO-p) using a modified Hummers’ method. The synthetic yield of this methodology was found to differ according to type of starting material, with GO-p resulting in most efficient yields. Structural and morphological comparison of the three GO sheet types were carried out using transmission electron microscopy and atomic force microscopy. Optical properties were measured using UV/visible and fluorescence spectroscopy. Surface characteristics and chemistry were determined using a battery of techniques. Exposure to human cells was studied using the human A549 lung epithelial cultures. Our results revealed that all three GO samples were composed of few-layer sheets with similar physicochemical and surface characteristics. However, significant differences were observed in terms of their lateral dimensions with GO-p, prepared from graphite powder, being the largest among the GOs. No cytotoxicity was detected for any of the GO samples following exposure onto A549 cells up to 48 h. In conclusion, the form and type of the starting graphite material is shown to be an important factor that can determine the synthetic yield and the structural characteristics of the resulting GO sheets.

  10. Processing of nanocrystalline ceramics

    SciTech Connect

    Ciftcioglu, M. . Center for Micro-Engineered Ceramics); Mayo, M.J. )

    1990-01-01

    Methods of preparing non-agglomerated powders for three systems -- yttria, titania, and yttria-stabilized zirconia -- are reviewed. The non-agglomerated nature of these powders should make it possible to sinter them into dense ceramic bodies with nanocrystalline grain sizes. Experiments with yttria-stabilized zirconia have shown that this is indeed the case, with mean linear intercept grain sizes of 60 nm resulting from original powder particle diameters of 13 nm. This ultrafine-grained zirconia is shown, in turn, to have superplastic forming rates 34 times faster than a 0.3 {mu}m-grained commercial zirconia of the same composition. 7 refs., 9 figs.

  11. Silicon carbide ceramic production

    NASA Technical Reports Server (NTRS)

    Suzuki, K.; Shinohara, N.

    1984-01-01

    A method to produce sintered silicon carbide ceramics in which powdery carbonaceous components with a dispersant are mixed with silicon carbide powder, shaped as required with or without drying, and fired in nonoxidation atmosphere is described. Carbon black is used as the carbonaceous component.

  12. Investigations on the use of chemical modifiers for the direct determination of trace impurities in Al2O3 ceramic powders by slurry electrothermal evaporation coupled with inductively-coupled plasma mass spectrometry (ETV-ICP-MS).

    PubMed

    Wende, M C; Broekaert, J A

    2001-07-01

    The direct determination of trace impurities in Al2O3 ceramic basic powders by ICP-MS using electrothermal evaporation (ETV) with slurry sampling has been investigated. To increase interference-free analyte volatilization, the use of the palladium-group modifiers (PGM) IrCl3, Pd(NO3)2, and PdCl2 for the determination of Ca, Fe, Ga, Mg, Mn, Na, Ni, and V in Al2O3 powders was studied. Their role, which in ETV-ICP-MS and ETV-ICP-OES is to stabilize the investigated analyte during the ashing phase, to increase vaporization of the matrix, and to reduce transport losses was investigated. Optimum analysis results were obtained with PdCl2 modifier when 500 ng Pd was used for a sample weight of 100 microg Al2O3 injected into the ETV. Calibration was performed by standard addition with aqueous solutions of the analytes. The RSDs calculated from triplicate analysis ranged form 5 to 10%. Detection limits between 0.07 microg g(-1) (Ga) and 1.1 microg g(-1) (Na) were achieved. The accuracy was proven for the elements Ca, Fe, Ga, Mg, Mn, Na, Ni, and V by analyzing an NIST standard reference Al2O3 material (SRM 699) with a middle grain size of 16.4 microm. The analytical method was used for the analysis of Al2O3 powder (AKP 30, Sumitomo, Japan) with impurities in the low microg g(-1) range and a middle grain size of 1.1 microm. The results obtained for the elements Ca, Fe, Ga, Mg, Mn, Na, Ni, and V were comparable with those obtained by ICP-MS subsequent to conventional decomposition with hydrochloric acid at high pressure. PMID:11496980

  13. Fabrication of transparent ceramic laser media for high energy laser applications

    NASA Astrophysics Data System (ADS)

    Serivalsatit, Karn

    Sesquioxides of yttrium, scandium, and lutetium, i.e., Y2O 3, Sc2O3, and Lu2O3, have received a great deal of recent attention as potential high power solid state laser hosts. These oxides are receptive to lanthanide doping, including trivalent Er, Ho and Tm which have well known emissions at eye-safe wavelengths that can be excited using commercial diode lasers. These sesquioxides are considered superior to the more conventional yttrium aluminum garnet (YAG) due to their higher thermal conductivity, which is critical for high power laser system. Unfortunately, these oxides possess high melting temperatures, which make the growth of high purity and quality crystals using melt techniques difficult. Transparent ceramics are an attractive alternative route to laser hosts since the processing by-passes many of the challenges of refractory crystal melt growth. Moreover, transparent ceramics can possess added benefits relative to single crystals including faster production rates, the fabrication of larger sizes and composite laser structures, uniform doping concentrations, and better mechanical behavior. In order to fabricate highly transparent ceramics, the starting powders must have good dispersion and high reactivity. In this work, sesquioxide nanopowders with high sinterability were synthesized by solution precipitation techniques. For Y2O3, the nanopowders were prepared using yttrium nitrate and ammonium hydroxide with the addition of a small amount of ammonium sulfate. Doping sulfate ions was found to reduce the agglomeration of Y 2O3 nanopowders. The Y2O3 nanopowders with average particle size about 40 nm were obtained by calcining at 1050°C for 4 hours. Unfortunately, this method failed to prepare well-dispersed Sc 2O3 and Lu2O3 nanopowders. For Sc 2O3 and Lu2O3, the nanopowders were synthesized by using scandium or lutetium sulfate and hexamethylenetetramine (HMT). The precipitate precursors were calcined at 1100°C for 4 hours to yielded Sc2O3 and Lu2O3

  14. Advanced powder processing

    SciTech Connect

    Janney, M.A.

    1997-04-01

    Gelcasting is an advanced powder forming process. It is most commonly used to form ceramic or metal powders into complex, near-net shapes. Turbine rotors, gears, nozzles, and crucibles have been successfully gelcast in silicon nitride, alumina, nickel-based superalloy, and several steels. Gelcasting can also be used to make blanks that can be green machined to near-net shape and then high fired. Green machining has been successfully applied to both ceramic and metal gelcast blanks. Recently, the authors have used gelcasting to make tooling for metal casting applications. Most of the work has centered on H13 tool steel. They have demonstrated an ability to gelcast and sinter H13 to near net shape for metal casting tooling. Also, blanks of H13 have been cast, green machined into complex shape, and fired. Issues associated with forming, binder burnout, and sintering are addressed.

  15. Polymer precursors for ceramic composites

    NASA Technical Reports Server (NTRS)

    Hurwitz, Frances I.

    1986-01-01

    The fiber composite approach to reinforced ceramics provides the possibility of achieving ceramics with high fracture toughness relative to monolithics. Fabrication of ceramic composites, however, demands low processing temperatures to avoid fiber degradation. Formation of complex shapes further requires small diameter fibers as well as techniques for infiltrating the matrix between fibers. Polymers offer low temperature processability, control of rheology not available with ceramic powders, and should serve as precursors to matrix fibers. In recent years, a number of polysilanes and polysilezanes were investigated as potential presursors. A review of candidate polymers is presented, including recent studies of silsesquioxanes.

  16. Characteristics of Signals Originating near the Lithium-Diffused N+ Contact of High Purity Germanium P-Type Point Contact Detectors

    SciTech Connect

    Aguayo, E.; Amman, M.; Avignone, F. T.; Barton, P. J.; Beene, James R; Bertrand Jr, Fred E; Boswell, M.; Brudanin, V.; Busch, M.; Chan, Y-D; Christofferson, C. D.; Collar, Juan I.; Combs, D. C.; Detwiler, J.A.; Doe, P. J.; Efremenko, Yuri; Egorov, V.; Ejiri, H.; Elliott, S. R.; Esterline, J.; Fast, J.E.; Fields, N.; Finnerty, P.; Gehman, V. M.; Giovanetti, G. K.; Green, M. P.; Gusey, K.; Hallin, A. L.; Hazama, R.; Henning, R.; Hoppe, E.W.; Horton, M.; Howard, S.; Howe, M. A.; Keeter, K.J.; Kidd, M. F.; Knecht, A.; Kochetov, O.; Konovalov, S.I.; Kouzes, R. T.; LaFerriere, B. D.; Leon, J.; Leviner, L. E.; Looker, Q.; Luke, P.N.; MacMullin, S.; Martin, R.D.; Merriman, J. H.; Miller, M. L.; Mizouni, L.; Orrell, John L.; Overman, N. R.; Perumpilly, G.; Phillips II, D. G.; et al.

    2013-01-01

    A study of signals originating near the lithium-diffused n+ contact of p-type point contact (PPC) high purity germanium detectors (HPGe) is presented. The transition region between the active germanium and the fully dead layer of the n+ contact is examined. Energy depositions in this transition region are shown to result in partial charge collection. This provides a mechanism for events with a well defined energy to contribute to the continuum of the energy spectrum at lower energies. A novel technique to quantify the contribution from this source of background is introduced. Experiments that operate germanium detectors with a very low energy threshold may benefit from the methods presented herein.

  17. OXYGEN TRANSPORT CERAMIC MEMBRANES

    SciTech Connect

    Dr. Sukumar Bandopadhyay; Dr. Nagendra Nagabhushana

    2002-04-01

    This report covers the following tasks: Task 1--Design, fabricate and evaluate ceramic to metal seals based on graded ceramic powder/metal braze joints; Task 2--Evaluate the effect of defect configuration on ceramic membrane conductivity and long term chemical and structural stability; Task 3--Determine materials mechanical properties under conditions of high temperatures and reactive atmospheres; Task 4--Evaluate phase stability and thermal expansion of candidate perovskite membranes and develop techniques to support these materials on porous metal structures; Task 5--Assess the microstructure of membrane materials to evaluate the effects of vacancy-impurity association, defect clusters, and vacancy-dopant association on the membrane performance and stability; and Task 6--Measure kinetics of oxygen uptake and transport in ceramic membrane materials under commercially relevant conditions using isotope labeling techniques.

  18. Portfolio: Ceramics.

    ERIC Educational Resources Information Center

    Hardy, Jane; And Others

    1982-01-01

    Describes eight art activities using ceramics. Elementary students created ceramic tiles to depict ancient Egyptian and medieval European art, made ceramic cookie stamps, traced bisque plates on sketch paper, constructed clay room-tableaus, and designed clay relief masks. Secondary students pit-fired ceramic pots and designed ceramic Victorian…

  19. Structural ceramics derived from a preceramic polymer

    SciTech Connect

    Semen, J.; Loop, J.G.

    1990-10-01

    Test pieces were uniaxially dry-pressed from formulations consisting of 20-30 wt pct polysilazane preceramic material and SiC and Si3N4 ceramic powders. Thermal crosslinking/pyrolysis of the molded pieces at temperatures well below normal powder sintering temperatures produced fully ceramic composites consisting of fully dense, submicrometer size, crystalline ceramic particles embedded in a highly nanoporous, amorphous Si-N-C ceramic matrix material. The mechanical and physical properties, and their relationship to the microstructure, of these materials are discussed.

  20. Determination of trace phosphorus in high purity tantalum materials by inductively coupled plasma mass spectrometry subsequent to matrix separation with on-line anion exchange/coprecipitation.

    PubMed

    Kozono, Shuji; Takahashi, Shigeto; Haraguchi, Hiroki

    2002-02-01

    An on-line matrix separation/inductively coupled plasma mass spectrometry (ICP-MS) method is proposed for the determination of trace amounts of phosphorus in high purity tantalum metal, tantalum (V) oxide, and tantalum pentaethoxide. In the present method, the matrix tantalum in the sample solution was adsorbed on the anion exchange resin, and phosphorus (phosphate ion) was eluted with the carrier solution of HF and HNO3 mixture. Then, the effluent solution was subsequently mixed with bismuth solution and aqueous ammonia solution to coprecipitate phosphate together with bismuth hydroxide. The precipitate formed was collected on the in-line membrane filter to wash out nitric acid with pure water, and then dissolved with hydrochloric acid. The obtained phosphorus sample solution was introduced directly into the nebulizer of ICP-MS for the determination of phosphorus. Phosphorus was determined at the molecular ion signal of 31P16O+ (m/z 47). The detection limit (3sigma) of phosphorus in the present method was 1.3 ng mL(-1) as the sample solution basis, and the relative standard deviation for 30 ng mL(-1) of phosphorus in the standard solution was 4.3% in the replicate measurements (n=11). The present method was applied to the analysis of high purity tantalum materials. The concentrations of phosphorus in tantalum samples were in fairly good agreement with those obtained by glow discharge mass spectrometry (GDMS). PMID:11939629

  1. Development and validation of a reversed-phase high-performance liquid chromatography method for routine identification and purity assessment of high-purity steviol glycoside sweeteners.

    PubMed

    Bililign, Tsion; Moore, Jeffrey C; Tan, Shane; Leeks, Allan T

    2014-02-12

    The widespread application of stevia-based sweeteners in food products has resulted in the need for reliable analytical methods for measuring the purity and identity of high-purity steviol glycoside ingredients. The objective of this research was to develop and validate a new reversed-phase separation method capable of separating and quantifying nine steviol glycosides present in typical high-purity stevia extract ingredients. Results of the study established the linearity of the method at a correlation factor of 1.000 for the two major components and other minor components of this food ingredient. Method accuracy values were in the range of 99.1-100.9%. The percent relative standard deviation for six independent assay determinations was 1.0%. The method was determined to be robust for minor changes in column temperature, initial acetonitrile content, flow rate, and wavelength. The validated high-performance liquid chromatography method was found to be suitable to be included by USP as a Food Chemicals Codex compendial standard for steviol glycosides. PMID:24443893

  2. Integrally cored ceramic investment casting mold fabricated by ceramic stereolithography

    NASA Astrophysics Data System (ADS)

    Bae, Chang-Jun

    Superalloy airfoils are produced by investment casting (IC), which uses ceramic cores and wax patterns with ceramic shell molds. Hollow cored superalloy airfoils in a gas turbine engine are an example of complex IC parts. The complex internal hollow cavities of the airfoil are designed to conduct cooling air through one or more passageways. These complex internal passageways have been fabricated by a lost wax process requiring several processing steps; core preparation, injection molding for wax pattern, and dipping process for ceramic shell molds. Several steps generate problems such as high cost and decreased accuracy of the ceramic mold. For example, costly tooling and production delay are required to produce mold dies for complex cores and wax patterns used in injection molding, resulting in a big obstacle for prototypes and smaller production runs. Rather than using separate cores, patterns, and shell molds, it would be advantageous to directly produce a mold that has the casting cavity and the ceramic core by one process. Ceramic stereolithography (CerSLA) can be used to directly fabricate the integrally cored ceramic casting mold (ICCM). CerSLA builds ceramic green objects from CAD files from many thin liquid layers of powder in monomer, which are solidified by polymerization with a UV laser, thereby "writing" the design for each slice. This dissertation addresses the integrally cored casting ceramic mold (ICCM), the ceramic core with a ceramic mold shell in a single patternless construction, fabricated by ceramic stereolithography (CerSLA). CerSLA is considered as an alternative method to replace lost wax processes, for small production runs or designs too complex for conventional cores and patterns. The main topic is the development of methods to successfully fabricate an ICCM by CerSLA from refractory silica, as well as related issues. The related issues are the segregation of coarse fused silica powders in a layer, the degree of segregation parameter to

  3. Electrothermal vaporization coupled with inductively coupled plasma array-detector mass spectrometry for the multielement analysis of Al2O3 ceramic powders

    SciTech Connect

    Peschel, Birgit U.; Andrade, Francisco J.; Wetzel, William C.; Schilling, G D.; Hieftje, Gary M.; Broekaert, Jose AC; Sperline, Roger; Denton, M BONNER.; Barinaga, Charles J.; Koppenaal, David W.

    2006-01-01

    An electrothermal vaporization (ETV) system useful for the analysis of solutions and slurries has been coupled with a sector-field inductively coupled plasma mass spectrometer (ICP-MS) equipped with an array detector. The ability of this instrument to record the transient signals produced in ETV-ICP-MS is demonstrated. Detection limits for Mn, Fe, Co, Ni, Cu, Zn and Ga are in the range of 4-60 pg ?L-1 for aqueous solutions and in the low ?g g-1 range for the analysis of 10 mg mL-1 slurries of Al2O3 powders. The dynamic ranges measured for Fe, Cu and Ga spanned 3-5 orders of magnitude when the detector was operated in the low-gain mode and appear to be limited by the ETV system. Trace amounts of Fe, Cu and Ga could be directly determined in Al2O3 powders at the 2-270 ?g g-1 level without the use of thermochemical reagents. The results well agree with literature values for Fe, whereas deviations of 30-50% at the 2-90 ?g g-1 level for Cu and Ga were found.

  4. Process for preparing fine grain titanium carbide powder

    DOEpatents

    Janey, Mark A.

    1986-01-01

    A method for preparing finely divided titanium carbide powder in which an organotitanate is reacted with a carbon precursor polymer to provide an admixture of the titanium and the polymer at a molecular-level due to a crosslinking reaction between the organotitanate and the polymer. The resulting gel is dried, pyrolyzed to drive off volatile components and provide carbon. The resulting solids are then heated at an elevated temperature to convert the titanium and carbon to high-purity titanium carbide powder in a submicron size range.

  5. Process for preparing fine grain titanium carbide powder

    DOEpatents

    Janney, M.A.

    1985-03-12

    A method for preparing finely divided titanium carbide powder in which an organotitanate is reacted with a carbon precursor polymer to provide an admixture of the titanium and the polymer at a molecular level due to a crosslinking reaction between the organotitanate and the polymer. The resulting gel is dried, pyrolyzed to drive off volatile components and provide carbon. The resulting solids are then heated at an elevated temperature to convert the titanium and carbon to high-purity titanium carbide powder in a submicron size range.

  6. Multielement trace determinations in A1 2O 3 ceramic powders by inductively coupled plasma mass spectrometry with special reference to on-line trace preconcentration

    NASA Astrophysics Data System (ADS)

    Pollmann, D.; Leis, F.; Tölg, G.; Tschöpel, P.; Broekaert, J. A. C.

    1994-12-01

    The use of inductively coupled plasma mass spectrometry (ICP-MS) for the determination of trace elements in Al 2O 3 powders is reported. Special interest is given to a preconcentration of the trace elements by on-line coupling of chromatography to ICP-MS. This is based on the complexation of Co, Cu, Cr, Fe, Ga, Mn, Ni, V and Zn with hexamethylene-dithiocarbamate (HMDC), their preconcentration on a C18 RP column by reversed phase liquid chromatography and their elution with CH 3OH-H 2O mixtures. A direct coupling of the HPLC system to the ICP-MS has been realized by high pressure pneumatic nebulization using desolvation. With the Chromatographie method developed, removal of the AI by at least 99% was achieved. For the trace elements V, Fe, Ni, Co, Cu and Ga, high and reproducible recoveries (ranging from 96-99%) were reached. The method developed has been shown to considerably enhance the power of detection as compared with direct procedures, namely down to 0.02-0.16 ( μg/g for V and Fe, respectively. The possibilities of the method are shown by the determinations of V, Mn, Fe, Ni, Co, Cu, Zn and Ga at the μg/g level in A1 2O 3 powders. The accuracy of the method at the 0.06 to 9.0 μg/g level for Co and Fe, respectively, is demonstrated by a comparison with results of independent methods from the literature.

  7. Study of the mechanical stability and bioactivity of Bioglass(®) based glass-ceramic scaffolds produced via powder metallurgy-inspired technology.

    PubMed

    Boccardi, Elena; Melli, Virginia; Catignoli, Gabriele; Altomare, Lina; Jahromi, Maryam Tavafoghi; Cerruti, Marta; Lefebvre, Louis-Philippe; De Nardo, Luigi

    2016-02-01

    Large bone defects are challenging to heal, and often require an osteoconductive and stable support to help the repair of damaged tissue. Bioglass-based scaffolds are particularly promising for this purpose due to their ability to stimulate bone regeneration. However, processing technologies adopted so far do not allow for the synthesis of scaffolds with suitable mechanical properties. Also, conventional sintering processes result in glass de-vitrification, which generates concerns about bioactivity. In this work, we studied the bioactivity and the mechanical properties of Bioglass(®) based scaffolds, produced via a powder technology inspired process. The scaffolds showed compressive strengths in the range of 5-40 MPa, i.e. in the upper range of values reported so far for these materials, had tunable porosity, in the range between 55 and 77%, and pore sizes that are optimal for bone tissue regeneration (100-500 μm). We immersed the scaffolds in simulated body fluid (SBF) for 28 d and analyzed the evolution of the scaffold mechanical properties and microstructure. Even if, after sintering, partial de-vitrification occurred, immersion in SBF caused ion release and the formation of a Ca-P coating within 2 d, which reached a thickness of 10-15 μm after 28 d. This coating contained both hydroxyapatite and an amorphous background, indicating microstructural amorphization of the base material. Scaffolds retained a good compressive strength and structural integrity also after 28 d of immersion (6 MPa compressive strength). The decrease in mechanical properties was mainly related to the increase in porosity, caused by its dissolution, rather than to the amorphization process and the formation of a Ca-P coating. These results suggest that Bioglass(®) based scaffolds produced via powder metallurgy-inspired technique are excellent candidates for bone regeneration applications. PMID:26836444

  8. Clinical and laboratory considerations in the use of a new all-ceramic restorative system.

    PubMed

    Prestipino, V; Ingber, A; Kravitz, J

    1998-01-01

    Ceramic systems are continually under development in an effort to refine their clinical application. An all-ceramic full-coverage crown system (Procera, Nobel Biocare, Westmont, IL) that utilizes computer technology and industrial presses to fabricate precise copings has recently been introduced. Using this system, aluminous porcelain is baked over a high-strength, high-purity aluminum oxide coping to fabricate a functional, biocompatible, and aesthetic restoration. This article presents a discussion of the clinical and laboratory considerations that are involved in the utilization of this all-ceramic system. PMID:9728137

  9. MHD oxidant intermediate temperature ceramic heater study

    NASA Technical Reports Server (NTRS)

    Carlson, A. W.; Chait, I. L.; Saari, D. P.; Marksberry, C. L.

    1981-01-01

    The use of three types of directly fired ceramic heaters for preheating oxygen enriched air to an intermediate temperature of 1144K was investigated. The three types of ceramic heaters are: (1) a fixed bed, periodic flow ceramic brick regenerative heater; (2) a ceramic pebble regenerative heater. The heater design, performance and operating characteristics under conditions in which the particulate matter is not solidified are evaluated. A comparison and overall evaluation of the three types of ceramic heaters and temperature range determination at which the particulate matter in the MHD exhaust gas is estimated to be a dry powder are presented.

  10. Possible influence of surface oxides on the optical response of high-purity niobium material used in the fabrication of superconducting radio frequency cavity

    NASA Astrophysics Data System (ADS)

    Singh, Nageshwar; Deo, M. N.; Roy, S. B.

    2016-09-01

    We have investigated the possible influence of surface oxides on the optical properties of a high-purity niobium (Nb) material for fabrication of superconducting radio frequency (SCRF) cavities. Various peaks in the infrared region were identified using Fourier transform infrared and Raman spectroscopy. Optical response functions such as complex refractive index, dielectric and conductivity of niobium were compared with the existing results on oxides free Nb and Cu. It was observed that the presence of a mixture of niobium-oxides, and probably near other surface impurities, appreciably influence the conducting properties of the material causing deviation from the typical metallic characteristics. In this way, the key result of this work is the observation, identification of vibrational modes of some of surface complexes and study of its influences on the optical responses of materials. This method of spectroscopic investigation will help in understanding the origin of degradation of performance of SCRF cavities.

  11. Measured Attenuation of Coplanar Waveguide on 6H, p-type SiC and High Purity Semi-Insulating 4H SiC through 800 K

    NASA Technical Reports Server (NTRS)

    Ponchak, George E.; Schwartz, Zachary D.; Alterovitz, Samuel A.; Downey, Alan N.

    2004-01-01

    Wireless sensors for high temperature applications such as oil drilling and mining, automobiles, and jet engine performance monitoring require circuits built on wide bandgap semiconductors. In this paper, the characteristics of microwave transmission lines on 4H-High Purity Semi-Insulating SiC and 6H, p-type SiC is presented as a function of temperature and frequency. It is shown that the attenuation of 6H, p-type substrates is too high for microwave circuits, large leakage current will flow through the substrate, and that unusual attenuation characteristics are due to trapping in the SiC. The 4H-HPSI SiC is shown to have low attenuation and leakage currents over the entire temperature range.

  12. Integrated Approach To Producing High-Purity Trehalose from Maltose by the Yeast Yarrowia lipolytica Displaying Trehalose Synthase (TreS) on the Cell Surface.

    PubMed

    Li, Ning; Wang, Hengwei; Li, Lijuan; Cheng, Huiling; Liu, Dawen; Cheng, Hairong; Deng, Zixin

    2016-08-10

    An alternative strategy that integrated enzyme production, trehalose biotransformation, and bioremoval in one bioreactor was developed in this study, thus simplifying the traditional procedures used for trehalose production. The trehalose synthase gene from a thermophilic archaea, Picrophilus torridus, was first fused to the YlPir1 anchor gene and then inserted into the genome of Yarrowia lipolytica, thus yielding an engineered yeast strain. The trehalose yield reached 73% under optimal conditions. The thermal and pH stabilities of the displayed enzyme were improved compared to those of its free form purified from recombinant Escherichia coli. After biotransformation, the glucose byproduct and residual maltose were directly fermented to ethanol by a Saccharomyces cerevisiae strain. Ethanol can be separated by distillation, and high-purity trehalose can easily be obtained from the fermentation broth. The results show that this one-pot procedure is an efficient approach to the economical production of trehalose from maltose. PMID:27472444

  13. An improved back-flush-to-vent gas chromatographic method for determination of trace permanent gases and carbon dioxide in ultra-high purity ammonia.

    PubMed

    Trubyanov, Maxim M; Mochalov, Georgy M; Vorotyntsev, Ilya V; Vorotyntsev, Andrey V; Suvorov, Sergey S; Smirnov, Konstantin Y; Vorotyntsev, Vladimir M

    2016-05-20

    A novel method for rapid, quantitative determination of trace permanent gases and carbon dioxide in ultra-high purity ammonia by dual-channel two-dimensional GC-PDHID is presented. An improved matrix back-flush-to-vent approach combining back-flush column switching technique with auxiliary NaHSO4 ammonia trap is described. The NaHSO4 trap prevents traces of ammonia from entering the analytical column and is shown not to affect the impurity content of the sample. The approach allows shortening the analysis time and increasing the amount of measurements without extensive maintenance of the GC-system. The performance of the configuration has been evaluated utilizing ammonia- and helium-based calibration standards. The method has been applied for the analysis of 99.9999+% ammonia purified by high-pressure distillation at the production site. PMID:27083259

  14. Characteristics of signals originating near the lithium-diffused N+ contact of high purity germanium p-type point contact detectors

    DOE PAGESBeta

    Aguayo, E.; Amman, M.; Avignone, F. T.; Barabash, A. S.; Barton, P. J.; Beene, J. R.; Bertrand, F. E.; Boswell, M.; Brudanin, V.; Busch, M.; et al

    2012-11-09

    A study of signals originating near the lithium-diffused n+ contact of p-type point contact (PPC) high purity germanium detectors (HPGe) is presented. The transition region between the active germanium and the fully dead layer of the n+ contact is examined. Energy depositions in this transition region are shown to result in partial charge collection. This provides a mechanism for events with a well defined energy to contribute to the continuum of the energy spectrum at lower energies. A novel technique to quantify the contribution from this source of background is introduced. Furthermore, experiments that operate germanium detectors with a verymore » low energy threshold may benefit from the methods presented herein.« less

  15. Characteristics of signals originating near the lithium-diffused N+ contact of high purity germanium p-type point contact detectors

    SciTech Connect

    Aguayo, E.; Amman, M.; Avignone, F. T.; Barabash, A. S.; Barton, P. J.; Beene, J. R.; Bertrand, F. E.; Boswell, M.; Brudanin, V.; Busch, M.; Chan, Y. -D.; Christofferson, C. D.; Collar, J. I.; Combs, D. C.; Cooper, R. J.; Detwiler, J. A.; Doe, P. J.; Efremenko, Yu.; Egorov, V.; Ejiri, H.; Elliott, S. R.; Esterline, J.; Fast, J. E.; Fields, N.; Finnerty, P.; Fraenkle, F. M.; Galindo-Uribarri, A.; Gehman, V. M.; Giovanetti, G. K.; Green, M. P.; Guiseppe, V. E.; Gusey, K.; Hallin, A. L.; Hazama, R.; Henning, R.; Hoppe, E. W.; Horton, M.; Howard, S.; Howe, M. A.; Johnson, R. A.; Keeter, K. J.; Kidd, M. F.; Knecht, A.; Kochetov, O.; Konovalov, S. I.; Kouzes, R. T.; LaFerriere, B. D.; Leon, J.; Leviner, L. E.; Loach, J. C.; Looker, Q.; Luke, P. N.; MacMullin, S.; Marino, M. G.; Martin, R. D.; Merriman, J. H.; Miller, M. L.; Mizouni, L.; Nomachi, M.; Orrell, J. L.; Overman, N. R.; Perumpilly, G.; Phillips, D. G.; Poon, A. W. P.; Radford, D. C.; Rielage, K.; Robertson, R. G. H.; Ronquest, M. C.; Schubert, A. G.; Shima, T.; Shirchenko, M.; Snavely, K. J.; Steele, D.; Strain, J.; Timkin, V.; Tornow, W.; Varner, R. L.; Vetter, K.; Vorren, K.; Wilkerson, J. F.; Yakushev, E.; Yaver, H.; Young, A. R.; Yu, C. -H.; Yumatov, V.

    2012-11-09

    A study of signals originating near the lithium-diffused n+ contact of p-type point contact (PPC) high purity germanium detectors (HPGe) is presented. The transition region between the active germanium and the fully dead layer of the n+ contact is examined. Energy depositions in this transition region are shown to result in partial charge collection. This provides a mechanism for events with a well defined energy to contribute to the continuum of the energy spectrum at lower energies. A novel technique to quantify the contribution from this source of background is introduced. Furthermore, experiments that operate germanium detectors with a very low energy threshold may benefit from the methods presented herein.

  16. First laser operation and spectroscopic characterization of mixed garnet Yb:LuYAG ceramics

    NASA Astrophysics Data System (ADS)

    Toci, Guido; Pirri, Angela; Li, Jiang; Xie, Tengfei; Pan, Yubai; Nikl, Martin; Babin, Vladimir; Beitlerová, Alena; Vannini, Matteo

    2016-03-01

    We present the optical and spectroscopic characterization and the first example of laser operation of Yb doped LuYAG ceramics, with two different compositions, namely (Lu0.25Y0.75)3Al5O12 and (Lu0.50Y0.50)3Al5O12, both with 15% Yb doping. Ceramic samples were prepared by reactive sintering from high purity α-Al2O3, Lu2O3, Y2O3, Yb2O3 powders using Tetraethoxysilane (TEOS) and MgO as sintering aids. After ball milling, the slurry was dried, uniaxially pressed into 20 mm diameter pellets at 20 MPa, and then cold isostatically pressed at 200 MPa. Sintering was conducted at 1850°C for 30 h under vacuum, followed by annealing in air (1500 °C, 10 h) to remove the oxygen vacancies. Laser tests were carried out in a laser cavity end pumped by a fiber coupled diode laser emitting at 936 nm. A slope efficiency as high as 65.2% with a maximum output power of 8.7 W (in quasi-CW pumping conditions) was obtained from the sample with composition (Lu0.25Y0.75)3Al5O12, whereas the sample with composition (Lu0.50Y0.50)3Al5O12 had a maximum slope efficiency of 49.5% (due to the higher scattering losses), and 6.7 W of maximum output power. Furthermore we characterized the tuning range of the two samples.

  17. Batch compositions for cordierite ceramics

    DOEpatents

    Hickman, David L.

    1994-07-26

    Ceramic products consisting principally of cordierite and a method for making them are provided, the method employing batches comprising a mineral component and a chemical component, the mineral component comprising clay and talc and the chemical component consisting essentially of a combination of the powdered oxides, hydroxides, or hydrous oxides of magnesium, aluminum and silicon. Ceramics made by extrusion and firing of the batches can exhibit low porosity, high strength and low thermal expansion coefficients.

  18. Extruded ceramic honeycomb and method

    DOEpatents

    Day, J. Paul

    1995-04-04

    Extruded low-expansion ceramic honeycombs comprising beta-spodumene solid solution as the principal crystal phase and with less than 7 weight percent of included mullite are produced by compounding an extrusion batch comprising a lithium aluminosilicate glass powder and a clay additive, extruding a green honeycomb body from the batch, and drying and firing the green extruded cellular honeycomb to crystallize the glass and clay into a low-expansion spodumene ceramic honeycomb body.

  19. A combined arc-melting and tilt-casting furnace for the manufacture of high-purity bulk metallic glass materials

    NASA Astrophysics Data System (ADS)

    Soinila, E.; Pihlajamäki, T.; Bossuyt, S.; Hänninen, H.

    2011-07-01

    An arc-melting furnace which includes a tilt-casting facility was designed and built, for the purpose of producing bulk metallic glass specimens. Tilt-casting was chosen because reportedly, in combination with high-purity processing, it produces the best fatigue endurance in Zr-based bulk metallic glasses. Incorporating the alloying and casting facilities in a single piece of equipment reduces the amount of laboratory space and capital investment needed. Eliminating the sample transfer step from the production process also saves time and reduces sample contamination. This is important because the glass forming ability in many alloy systems, such as Zr-based glass-forming alloys, deteriorates rapidly with increasing oxygen content of the specimen. The challenge was to create a versatile instrument, in which high purity conditions can be maintained throughout the process, even when melting alloys with high affinity for oxygen. Therefore, the design provides a high-vacuum chamber to be filled with a low-oxygen inert atmosphere, and takes special care to keep the system hermetically sealed throughout the process. In particular, movements of the arc-melting electrode and sample manipulator arm are accommodated by deformable metal bellows, rather than sliding O-ring seals, and the whole furnace is tilted for tilt-casting. This performance of the furnace is demonstrated by alloying and casting Zr55Cu30Al10Ni5 directly into rods up to ø 10 mm which are verified to be amorphous by x-ray diffraction and differential scanning calorimetry, and to exhibit locally ductile fracture at liquid nitrogen temperature.

  20. High-purity isolation of anthocyanins mixtures from fruits and vegetables--a novel solid-phase extraction method using mixed mode cation-exchange chromatography.

    PubMed

    He, Jian; Giusti, M Monica

    2011-11-01

    Research on biological activity of anthocyanins requires the availability of high purity materials. However, current methods to isolate anthocyanins or anthocyanin mixtures are tedious and expensive or insufficient for complete isolation. We applied a novel cation-exchange/reversed-phase combination solid-phase extraction (SPE) technique, and optimized the use of water/organic buffer mobile phases to selectively separate anthocyanins. Crude extracts of various representative anthocyanin sources were purified with this technique and compared to 3 commonly used SPE techniques: C(18), HLB, and LH-20. Purified anthocyanin fractions were analyzed with high performance liquid chromatography (HPLC) coupled to photodiode array (PDA) and mass spectrometry (MS) detectors and by Fourier transform infrared (FT-IR) spectroscopy. The UV-visible chromatograms quantitatively demonstrated that our novel technique achieved significantly higher (P<0.05) anthocyanin purity than the C(18) cartridge, the next best method, for 11 of the 12 anthocyanin sources tested. Among them, eight were purified to greater than 99% purity (based on UV-visible chromatograms). The new method efficiently removed non-anthocyanin phenolics. MS and FT-IR results semi-quantitatively confirmed extensive reduction of impurities. Due to strong ionic interaction, our sorbent capacity was superior to others, resulting in the highest throughput and least use of organic solvents. This new methodology for isolation of anthocyanin mixtures drastically increased purity and efficiency while maintaining excellent recovery rate and low cost. The availability of high purity anthocyanin mixtures will facilitate anthocyanin studies and promote the application of anthocyanins in the food and nutraceutical industries. PMID:21968344

  1. Design, fabrication, performance and reliability of Pt- and RuO2-coated microrelays tested in ultra-high purity gas environments

    NASA Astrophysics Data System (ADS)

    de Boer, M. P.; Czaplewski, D. A.; Baker, M. S.; Wolfley, S. L.; Ohlhausen, J. A.

    2012-10-01

    We have fabricated, tested and analyzed the reliability of Pt- and RuO2-coated ohmic microrelays in ultra-high purity gas environments. RuO2-coated relays could survive 3 × 108 contact cycles without electrical degradation, while Pt-coated devices degraded after 105 cycles. Thermally actuated microrelays were fabricated using a process that employed a polysilicon surface-micromachined substructure. After releasing the devices, just a few blanket metal depositions were required to create the different coatings. This method allowed direct comparisons between different coating materials, and was enabled by a self-aligned shadow mask that provides electrical isolation between different traces. Testing was performed in a clean environment achieved through in situ ultra-high vacuum bakeouts, chamber cooling to <5 × 10-9 Torr and chamber refill with ultra-high purity gases. The RuO2 coatings were formed by two avenues—reactive sputtering and thermal oxidation. No significant difference in contact resistance or reliability was detected for these two deposition methods. For all coatings, post-test analysis by scanning electron microscopy and Auger electron spectroscopy indicated no difference in carbon concentration on real contact versus non-contacting areas, implying that carbon did not play a role in limiting the switches’ reliability. The Pt-coated switch reliability limit was attributed to surface wear rather than to the growth of a contaminating film. For the RuO2 switches, trace resistance was reduced by ten times using an Al underlayer, so that the total device resistance was compatible with commercial device requirements. Because RuO2 is expected to be resistant to hydrocarbon contamination, this work shows that the RuO2 coating provides a promising path toward achieving ultra-high reliability ohmic microswitches.

  2. Determination of boron in high-purity tantalum materials by on-line matrix separation/inductively coupled plasma mass spectrometry.

    PubMed

    Kozono, Shuji; Takahashi, Shigeto; Haraguchi, Hiroki

    2002-07-01

    A method for the determination of ultratrace amounts of boron in high-purity tantalum materials [tantalum metal, tantalum(v) oxide, tantalum pentachloride and tantalum pentaethoxide] is described. On-line anion-exchange matrix separation combined with inductively coupled plasma mass spectrometry (ICP-MS) was employed for the determination of boron at the ng g(-1) level. Tantalum materials were dissolved using HF and/or HNO3 prior to analysis. The loss of boron in the sample preparation procedure was examined as the recovery of boron by adding a definite amount of boron to each tantalum material sample before decomposition, and it was almost negligible. In an anion-exchange method using 0.1 M HF carrier solution, tantalum and boron in the sample solution were first adsorbed on a strongly basic anion-exchange resin. Next, boron was eluted from the resin with 5 M HCl, whereas tantalum was retained strongly adsorbed. The eluted boron was introduced directly into the ICP-MS system for quantitative analysis at m/z 10 and 11. Because of the long elution time of boron, the transient signal was integrated in the time range 70-300 s on the chromatogram. Although the elution of boron in the time range was ca. 40% of total boron in the sample solution injected, the determination limits (10sigma) obtained by the present method were 30, 25, 15 and 13 ng g(-1) for tantalum metal, tantalum(v) oxide, tantalum pentachloride and tantalum pentaethoxide, respectively. The method was applied to the determination of boron in commercially available high-purity tantalum materials and it was found that the concentrations of boron were in the ng g(-1)-microg g(-1) range. PMID:12173652

  3. Fabrication of large-volume, low-cost ceramic lanthanum halide scintillators for gamma ray detection : final report for DHS/DNDO/TRDD project TA-01-SL01.

    SciTech Connect

    Boyle, Timothy J.; Ottley, Leigh Anna M.; Yang, Pin; Chen, Ching-Fong; Sanchez, Margaret R.; Bell, Nelson Simmons

    2008-10-01

    This project uses advanced ceramic processes to fabricate large, optical-quality, polycrystalline lanthanum halide scintillators to replace small single crystals produced by the conventional Bridgman growth method. The new approach not only removes the size constraint imposed by the growth method, but also offers the potential advantages of both reducing manufacturing cost and increasing production rate. The project goal is to fabricate dense lanthanum halide ceramics with a preferred crystal orientation by applying texture engineering and solid-state conversion to reduce the thermal mechanical stress in the ceramic and minimize scintillation light scattering at grain boundaries. Ultimately, this method could deliver the sought-after high sensitivity and <3% energy resolution at 662 keV of lanthanum halide scintillators and unleash their full potential for advanced gamma ray detection, enabling rapid identification of radioactive materials in a variety of practical applications. This report documents processing details from powder synthesis, seed particle growth, to final densification and texture development of cerium doped lanthanum bromide (LaBr{sub 3}:Ce{sup +3}) ceramics. This investigation demonstrated that: (1) A rapid, flexible, cost efficient synthesis method of anhydrous lanthanum halides and their solid solutions was developed. Several batches of ultrafine LaBr{sub 3}:Ce{sup +3} powder, free of oxyhalide, were produced by a rigorously controlled process. (2) Micron size ({approx} 5 {micro}m), platelet shape LaBr{sub 3} seed particles of high purity can be synthesized by a vapor phase transport process. (3) High aspect-ratio seed particles can be effectively aligned in the shear direction in the ceramic matrix, using a rotational shear-forming process. (4) Small size, highly translucent LaBr{sub 3} (0.25-inch diameter, 0.08-inch thick) samples were successfully fabricated by the equal channel angular consolidation process. (5) Large size, high density

  4. Porosity and mechanical properties of zirconium ceramics

    SciTech Connect

    Buyakova, S. Kulkov, S.; Sablina, T.

    2015-11-17

    Has been studied a porous ceramics obtained from ultra-fine powders. Porous ceramic ZrO{sub 2}(MgO), ZrO{sub 2}(Y{sub 2}O{sub 3}) powder was prepared by pressing and subsequent sintering of compacts homologous temperatures ranging from 0.63 to 0.56 during the isothermal holding duration of 1 to 5 hours. The porosity of ceramic samples was from 15 to 80%. The structure of the ceramic materials produced from plasma-sprayed ZrO{sub 2} powder was represented as a system of cell and rod structure elements. Cellular structure formed by stacking hollow powder particles can be easily seen at the images of fracture surfaces of obtained ceramics. There were three types of pores in ceramics: large cellular hollow spaces, small interparticle pores which are not filled with powder particles and the smallest pores in the shells of cells. The cells generally did not have regular shapes. The size of the interior of the cells many times exceeded the thickness of the walls which was a single-layer packing of ZrO{sub 2} grains. A distinctive feature of all deformation diagrams obtained in the experiment was their nonlinearity at low deformations which was described by the parabolic law. It was shown that the observed nonlinear elasticity for low deformation on deformation diagrams is due to mechanical instability of the cellular elements in the ceramic carcass.

  5. Porosity and mechanical properties of zirconium ceramics

    NASA Astrophysics Data System (ADS)

    Buyakova, S.; Sablina, T.; Kulkov, S.

    2015-11-01

    Has been studied a porous ceramics obtained from ultra-fine powders. Porous ceramic ZrO2(MgO), ZrO2(Y2O3) powder was prepared by pressing and subsequent sintering of compacts homologous temperatures ranging from 0.63 to 0.56 during the isothermal holding duration of 1 to 5 hours. The porosity of ceramic samples was from 15 to 80%. The structure of the ceramic materials produced from plasma-sprayed ZrO2 powder was represented as a system of cell and rod structure elements. Cellular structure formed by stacking hollow powder particles can be easily seen at the images of fracture surfaces of obtained ceramics. There were three types of pores in ceramics: large cellular hollow spaces, small interparticle pores which are not filled with powder particles and the smallest pores in the shells of cells. The cells generally did not have regular shapes. The size of the interior of the cells many times exceeded the thickness of the walls which was a single-layer packing of ZrO2 grains. A distinctive feature of all deformation diagrams obtained in the experiment was their nonlinearity at low deformations which was described by the parabolic law. It was shown that the observed nonlinear elasticity for low deformation on deformation diagrams is due to mechanical instability of the cellular elements in the ceramic carcass.

  6. Method of manufacturing ceramic shaped articles

    NASA Technical Reports Server (NTRS)

    Inoue, K.

    1983-01-01

    A method of manufacturing ceramic shaped articles, wherein tapes of ceramic powder material in mixture with a binder material and special additives are shaped and then articles are stamped out from said tapes and sintered in a sintering furnace is described.

  7. Process for making a ceramic composition for immobilization of actinides

    DOEpatents

    Ebbinghaus, Bartley B.; Van Konynenburg, Richard A.; Vance, Eric R.; Stewart, Martin W.; Walls, Philip A.; Brummond, William Allen; Armantrout, Guy A.; Herman, Connie Cicero; Hobson, Beverly F.; Herman, David Thomas; Curtis, Paul G.; Farmer, Joseph

    2001-01-01

    Disclosed is a process for making a ceramic composition for the immobilization of actinides, particularly uranium and plutonium. The ceramic is a titanate material comprising pyrochlore, brannerite and rutile. The process comprises oxidizing the actinides, milling the oxides to a powder, blending them with ceramic precursors, cold pressing the blend and sintering the pressed material.

  8. Process for Making a Ceramic Composition for Immobilization of Actinides

    SciTech Connect

    Ebbinghaus, Bartley B.; Van Konynenburg, Richard A.; Vance, Eric R.; Stewart, Martin W.; Walls, Philip A.; Brummond, William Allen; Armantrout, Guy A.; Curtis, Paul G.; Hobson, Beverly F.; Farmer, Joseph; Herman, Connie Cicero; Herman, David Thomas

    1999-06-22

    Disclosed is a process for making a ceramic composition for the immobilization of actinides, particularly uranium and plutonium. The ceramic is a titanate material comprising pyrochlore, brannerite and rutile. The process comprises oxidizing the actinides, milling the oxides to a powder, blending them with ceramic precursors, cold pressing the blend and sintering the pressed material.

  9. Braze material for joining ceramic to metal and ceramic to ceramic surfaces and joined ceramic to metal and ceramic to ceramic article

    DOEpatents

    Hunt, T.K.; Novak, R.F.

    1991-05-07

    An improved active metal braze filler material is provided in which the coefficient of thermal expansion of the braze filler is more closely matched with that of the ceramic and metal, or two ceramics, to provide ceramic to metal, or ceramic to ceramic, sealed joints and articles which can withstand both high temperatures and repeated thermal cycling without failing. The braze filler material comprises a mixture of a material, preferably in the form of a powder, selected from the group consisting of molybdenum, tungsten, silicon carbide and mixtures thereof, and an active metal filler material selected from the group consisting of alloys or mixtures of nickel and titanium, alloys or mixtures of nickel and zirconium, alloys or mixtures of nickel, titanium, and copper, alloys or mixtures of nickel, titanium, and zirconium, alloys or mixtures of niobium and nickel, alloys or mixtures of niobium and zirconium, alloys or mixtures of niobium and titanium, alloys or mixtures of niobium, titanium, and nickel, alloys or mixtures of niobium, zirconium, and nickel, and alloys or mixtures of niobium, titanium, zirconium, and nickel. The powder component is selected such that its coefficient of thermal expansion will effect the overall coefficient of thermal expansion of the braze material so that it more closely matches the coefficients of thermal expansion of the ceramic and metal parts to be joined. 3 figures.

  10. Braze material for joining ceramic to metal and ceramic to ceramic surfaces and joined ceramic to metal and ceramic to ceramic article

    DOEpatents

    Hunt, Thomas K.; Novak, Robert F.

    1991-01-01

    An improved active metal braze filler material is provided in which the coefficient of thermal expansion of the braze filler is more closely matched with that of the ceramic and metal, or two ceramics, to provide ceramic to metal, or ceramic to ceramic, sealed joints and articles which can withstand both high temperatures and repeated thermal cycling without failing. The braze filler material comprises a mixture of a material, preferably in the form of a powder, selected from the group consisting of molybdenum, tungsten, silicon carbide and mixtures thereof, and an active metal filler material selected from the group consisting of alloys or mixtures of nickel and titanium, alloys or mixtures of nickel and zirconium, alloys or mixtures of nickel, titanium, and copper, alloys or mixtures of nickel, titanium, and zirconium, alloys or mixtures of niobium and nickel, alloys or mixtures of niobium and zirconium, alloys or mixtures of niobium and titanium, alloys or mixtures of niobium, titanium, and nickel, alloys or mixtures of niobium, zirconium, and nickel, and alloys or mixtures of niobium, titanium, zirconium, and nickel. The powder component is selected such that its coefficient of thermal expansion will effect the overall coefficient of thermal expansion of the braze material so that it more closely matches the coefficients of thermal expansion of the ceramic and metal parts to be joined.

  11. Structural, thermal, electrical and magnetic properties of pure and 50% La doped BiFeO3 ceramics

    NASA Astrophysics Data System (ADS)

    Jangid, S.; Barbar, S. K.; Bala, Indu; Roy, M.

    2012-09-01

    Polycrystalline ceramic samples of pure and 50% La substituted BiFeO3 have been prepared by standard solid state reaction method using high purity oxides and carbonates. The formation of the single phase compound as well as its chemical analysis has been checked by X-ray diffraction and energy dispersive X-ray microanalysis (EDAX) techniques. A better agreement between observed and calculated X-ray powder diffraction patterns was obtained by performing the Rietveld refinement with a structural model using the non-centrosymmetric space group R3c. The lattice parameters in both the cases have been refined but the over-all structure remains the same. The microstructural studies have been carried out using scanning electron microscopy (SEM). Modulated differential scanning calorimetry (MDSC) has been used to detect the Neel/transition temperature in the compounds. The activation energies calculated from log σ vs 1/T curve are 0.81 eV and 1.13 eV respectively. Vibrating sample magnetometer (VSM) has been used to study the magnetic behaviour of the compounds. It has been observed that by 50% La substitution the insulating behaviour of the material has been improved and showing the antiferromagnetic to weak ferromagnetic behaviour.

  12. Protective coating for ceramic materials

    NASA Technical Reports Server (NTRS)

    Kourtides, Demetrius A. (Inventor); Churchward, Rex A. (Inventor); Lowe, David M. (Inventor)

    1994-01-01

    A protective coating for ceramic materials such as those made of silicon carbide, aluminum oxide, zirconium oxide, aluminoborosilicate and silicon dioxide, and a thermal control structure comprising a ceramic material having coated thereon the protective coating. The protective coating contains, in admixture, silicon dioxide powder, colloidal silicon dioxide, water, and one or more emittance agents selected from silicon tetraboride, silicon hexaboride, silicon carbide, molybdenum disilicide, tungsten disilicide and zirconium diboride. In another aspect, the protective coating is coated on a flexible ceramic fabric which is the outer cover of a composite insulation. In yet another aspect, a metallic foil is bonded to the outer surface of a ceramic fabric outer cover of a composite insulation via the protective coating. A primary application of this invention is as a protective coating for ceramic materials used in a heat shield for space vehicles subjected to very high aero-convective heating environments.

  13. Mesoscale simulations of powder compaction

    NASA Astrophysics Data System (ADS)

    Lomov, Ilya; Antoun, Tarabay; Liu, Benjamin

    2009-06-01

    Mesoscale 3D simulations of metal and ceramic powder compaction in shock waves have been performed with an Eulerian hydrocode GEODYN. The approach was validated by simulating shock compaction of porous well-characterized ductile metal using Steinberg material model. Results of the simulations with handbook values for parameters of solid 2024 aluminum have good agreement with experimental compaction curves and wave profiles. Brittle ceramic materials are not so well studied as metals, so material model for ceramic (tungsten carbide) has been fitted to shock compression experiments of non-porous samples and further calibrated to experimental match compaction curves. Direct simulations of gas gun experiments with ceramic powder have been performed and showed good agreement with experimental data. Numerical shock wave profile has same character and thickness as measured with VISAR. Numerical results show evidence of hard-to-explain reshock states above the single-shock Hugoniot line, which have also been observed in the experiments. We found that to receive good quantitative agreement with experiment it is essential to perform 3D simulations, since 2D results tend to underpredict stress levels for high-porosity powders regardless of material properties. We developed a process to extract macroscale information for the simulation which can be directly used in calibration of continuum model for heterogeneous media.

  14. Measurement of the high-field Q-drop in a high-purity large-grain niobium cavity for different oxidation processes

    SciTech Connect

    Ciovati, Gianluigi; Kneisel, Peter; gurevich, alex

    2007-06-01

    The most challenging issue for understanding the performance of superconducting radio-frequency (rf) cavities made of high-purity (residual resistivity ratio > 200) niobium is due to a sharp degradation (“Q-drop”) of the cavity quality factor Q0(Bp) as the peak surface magnetic field (Bp) exceeds about 90 mT, in the absence of field emission. In addition, a low-temperature (100 – 140 C) “in-situ” baking of the cavity was found to be beneficial in reducing the Q-drop. In this contribution, we present the results from a series of rf tests at 1.7 K and 2.0 K on a single-cell cavity made of high-purity large (with area of the order of few cm2) grain niobium which underwent various oxidation processes, after initial buffered chemical polishing, such as anodization, baking in pure oxygen atmosphere and baking in air up to 180 °C, with the objective of clearly identifying the role of oxygen and the oxide layer on the Q-drop. During each rf test a temperature mapping system allows measuring the local temperature rise of the cavity outer surface due to rf losses, which gives information about the losses location, their field dependence and space distribution. The results confirmed that the depth affected by baking is about 20 – 30 nm from the surface and showed that the Q-drop did not re-appear in a previously baked cavity by further baking at 120 °C in pure oxygen atmosphere or in air up to 180 °C. These treatments increased the oxide thickness and oxygen concentration, measured on niobium samples which were processed with the cavity and were analyzed with Transmission Electron Microscope (TEM) and Secondary Ion Mass Spectroscopy (SIMS). Nevertheless, the performance of the cavity after air baking at 180 °C degraded significantly and the temperature maps showed high losses, uniformly distributed on the surface, which could be completely recovered only by a post-purification treatment at 1250 °C. A statistic of the position of the “hot-spots” on the

  15. Advantages of combined micro-XRF and micro-XRD for phase characterization of Ti-B-C ceramics compared with conventional X-ray diffraction.

    PubMed

    Jaroszewicz, Jakub; De Nolf, Wout; Janssens, Koen; Michalski, Andrzej; Falkenberg, Gerald

    2008-06-01

    Design and processing of new materials with improved high-temperature properties is one of the most challenging tasks of modern engineering. Among such materials, nonoxidic ceramics hold an important place. When optimizing the synthesis conditions of these new materials in an largely empirical manner, the use of analytical methods that can fully document the resulting phase compositions is of great importance. In this paper, we demonstrate the advantages of using combined microbeam X-ray diffraction and X-ray fluorescence over conventional X-ray diffraction as the characterization method in the specific case of Ti-B-C ceramics. Ceramic samples were synthesized by the pulse plasma method starting from high-purity powders of titanium, boron, graphite, and nickel. Different mixtures were heated in a pulsed fashion and sintered by combustion synthesis at various temperatures and time durations, as is the case during empirical optimization of a synthesis procedure. Conventional X-ray diffraction showed the presence of two phases at the end of the sintering process, TiB(2) and TiC, irrespective of the conditions employed. Scanning micro-XRF/micro-XRD on the other hand allowed one to detect and visualize the distribution of additional phases present in the sintering products, during which a dependence on sintering conditions was apparent. The micro-XRD results showed that three phases (TiB(2), TiC, and TiB) instead of two were present in samples sintered during a short time interval. The addition of metallic Ni to the initial mixture as a sintering facilitator resulted in the formation of a Ni(3)B phase. All phases proved to have strongly heterogeneous distributions above the 15-microm level with the presence of TiB(2) anticorrelated to that of TiC and TiB, emphasizing the necessity of the use of laterally resolved methods of characterization. PMID:18458886

  16. OXYGEN TRANSPORT CERAMIC MEMBRANES

    SciTech Connect

    Dr. Sukumar Bandopadhyay; Dr. Nagendra Nagabhushana

    2000-10-01

    This is the third quarterly report on oxygen Transport Ceramic Membranes. In the following, the report describes the progress made by our university partners in Tasks 1 through 6, experimental apparatus that was designed and built for various tasks of this project, thermodynamic calculations, where applicable and work planned for the future. (Task 1) Design, fabricate and evaluate ceramic to metal seals based on graded ceramic powder/metal braze joints. (Task 2) Evaluate the effect of defect configuration on ceramic membrane conductivity and long term chemical and structural stability. (Task 3) Determine materials mechanical properties under conditions of high temperatures and reactive atmospheres. (Task 4) Evaluate phase stability and thermal expansion of candidate perovskite membranes and develop techniques to support these materials on porous metal structures. (Task 5) Assess the microstructure of membrane materials to evaluate the effects of vacancy-impurity association, defect clusters, and vacancy-dopant association on the membrane performance and stability. (Task 6) Measure kinetics of oxygen uptake and transport in ceramic membrane materials under commercially relevant conditions using isotope labeling techniques.

  17. Manufacture of high-density ceramic sinters

    NASA Technical Reports Server (NTRS)

    Hibata, Y.

    1986-01-01

    High density ceramic sinters are manufactured by coating premolded or presintered porous ceramics with a sealing material of high SiO2 porous glass or nitride glass and then sintering by hot isostatic pressing. The ceramics have excellent abrasion and corrosion resistances. Thus LC-10 (Si3N2 powder) and Y2O3-Al2O3 type sintering were mixed and molded to give a premolded porous ceramic (porosity 37%, relative bulk density 63%). The ceramic was dipped in a slurry containing high SiO2 porous glass and an alcohol solution of cellulose acetate and dried. The coated ceramic was treated in a nitrogen atmosphere and then sintered by hot isostatic pressing to give a dense ceramic sinter.

  18. Zirconia-based sintered ceramics for biomedical applications

    NASA Astrophysics Data System (ADS)

    Kulkov, Sergey; Buyakova, Svetlana

    2016-08-01

    A porous ceramics obtained from ultra-fine powders has been studied. The porosity of ceramic samples was from 15 to 80%. The structure of the ceramic materials was a cellular structure. A distinctive feature of all deformation diagrams obtained in the experiment was their nonlinearity at low deformations which was described by the parabolic law. It was shown that the observed nonlinear elasticity for low deformations on deformation diagrams is due to mechanical instability of the cellular elements in the ceramic carcass.

  19. On Ceramics.

    ERIC Educational Resources Information Center

    School Arts, 1982

    1982-01-01

    Presents four ceramics activities for secondary-level art classes. Included are directions for primitive kiln construction and glaze making. Two ceramics design activities are described in which students make bizarrely-shaped lidded jars, feet, and footwear. (AM)

  20. Calcining influence on the powder properties of hydroxyapatite.

    PubMed

    Patel, N; Gibson, I R; Ke, S; Best, S M; Bonfield, W

    2001-02-01

    The effect of different calcination temperatures on the powder characteristics and the sintered density of synthetic hydroxyapatite (HA) powders, produced using two different processing routes, was examined. Powders were produced by either drying, milling and sieving an as-precipitated HA or by spray-drying a slurry of precipitated HA. Calcining the two powders at temperatures between 400 and 1000 degrees C did not significantly affect the powder particle size. The specific surface areas of the two powders, however, were reduced from 70-80 m2/g for a calcination temperature of 400 degrees C to approximately 5-7 m2/g for 1000 degrees C. Analysis of the surfaces of the HA powders using scanning electron microscopy (SEM) illustrated the coarsening and subsequent sintering of the sub-micron crystallites that constitute a powder particle as the calcination temperature increased, corresponding to the decrease in surface area of the powders. The sintered densities of the final ceramics were not significantly affected by calcining the powders. Microhardness measurements of ceramics prepared from powders calcined at different temperatures showed no significant variations with calcination temperature or powder processing method. The results of this study have illustrated that for applications where HA may be used in powder form, for example in plasma-spraying and for the production of HA-polymer composites, calcining the HA will significantly affect the powder properties, namely the surface area and morphology of the powders. For applications requiring HA in a dense ceramic form, for example as granules or blocks, calcining the powders does not significantly affect the properties of the final ceramic. PMID:15348326

  1. A method for high purity intestinal epithelial cell culture from adult human and murine tissues for the investigation of innate immune function

    PubMed Central

    Graves, Christina L.; Harden, Scott W.; LaPato, Melissa; Nelson, Michael; Amador, Byron; Sorenson, Heather; Frazier, Charles J.; Wallet, Shannon M.

    2015-01-01

    Intestinal epithelial cells (IECs) serve as an important physiologic barrier between environmental antigens and the host intestinal immune system. Thus, IECs serve as a first line of defense and may act as sentinel cells during inflammatory insults. Despite recent renewed interest in IEC contributions to host immune function, the study of primary IEC has been hindered by lack of a robust culture technique, particularly for small intestinal and adult tissues. Here, a novel adaptation for culture of primary IEC is described for human duodenal organ donor tissue as well as duodenum and colon of adult mice. These epithelial cell cultures display characteristic phenotypes and are of high purity. In addition, the innate immune function of human primary IEC, specifically with regard to Toll-like receptor (TLR) expression and microbial ligand responsiveness, is contrasted with a commonly used intestinal epithelial cell line (HT-29). Specifically, TLR expression at the mRNA level and production of cytokine (IFNγ and TNFα) in response to TLR agonist stimulation is assessed. Differential expression of TLRs as well as innate immune responses to ligand stimulation is observed in human-derived cultures compared to that of HT-29. Thus, use of this adapted method to culture primary epithelial cells from adult human donors and from adult mice will allow for more appropriate studies of IECs as innate immune effectors. PMID:25193428

  2. Analysis of thermal detrapping of holes created by electron irradiation in high purity amorphous SiO2 using the induced and secondary current measurements

    NASA Astrophysics Data System (ADS)

    Said, K.; Moya, G.; Si Ahmed, A.; Damamme, G.; Kallel, A.

    2016-01-01

    Isothermal detrapping of holes after electron irradiation (using a SEM) in high purity amorphous SiO2 is evaluated at different temperatures (in the range 300-663 K) by means of the induced and secondary current measurements. In order to single out the hole detrapping, the specific charging conditions (1 keV defocused electron beam of low density) leading to positive charging are adopted. The thermal detrapping, which stems from a single trap, begins at 523 K and is completed at 663 K. After annealing in air at 973 K during 48 h, two detrapping stages are revealed: the former is connected with an additional shallow trap, while the latter requires temperatures above 663 K for a complete detrapping. The first order kinetics describes reasonably well the detrapping process. The frequency factors (near 1010 s-1) and the activation energies (about 1.6 eV) deduced from this analysis could be assigned, respectively, to the relaxation connected to detrapping and to the trap energy level of the charged oxygen vacancy.

  3. Microfluidic device with integrated microfilter of conical-shaped holes for high efficiency and high purity capture of circulating tumor cells

    NASA Astrophysics Data System (ADS)

    Tang, Yadong; Shi, Jian; Li, Sisi; Wang, Li; Cayre, Yvon E.; Chen, Yong

    2014-08-01

    Capture of circulating tumor cells (CTCs) from peripheral blood of cancer patients has major implications for metastatic detection and therapy analyses. Here we demonstrated a microfluidic device for high efficiency and high purity capture of CTCs. The key novelty of this approach lies on the integration of a microfilter with conical-shaped holes and a micro-injector with cross-flow components for size dependent capture of tumor cells without significant retention of non-tumor cells. Under conditions of constant flow rate, tumor cells spiked into phosphate buffered saline could be recovered and then cultured for further analyses. When tumor cells were spiked in blood of healthy donors, they could also be recovered at high efficiency and high clearance efficiency of white blood cells. When the same device was used for clinical validation, CTCs could be detected in blood samples of cancer patients but not in that of healthy donors. Finally, the capture efficiency of tumor cells is cell-type dependent but the hole size of the filter should be more closely correlated to the nuclei size of the tumor cells. Together with the advantage of easy operation, low-cost and high potential of integration, this approach offers unprecedented opportunities for metastatic detection and cancer treatment monitoring.

  4. Heterogeneous nucleation of entrained eutectic Si in high purity melt spun Al-Si alloys investigated by entrained droplet technique and DSC

    NASA Astrophysics Data System (ADS)

    Li, J. H.; Albu, M.; Ludwig, T. H.; Hofer, F.; Arnberg, L.; Schumacher, P.

    2016-03-01

    Entrained droplet technique and DSC analyses were employed to investigate the influence of trace elements of Sr, Eu and P on the heterogeneous nucleation of entrained eutectic Si in high purity melt spun Al-5wt.% Si alloys. Sr and Eu addition was found to exert negative effects on the nucleation process, while an increased undercooling was observed. This can be attributed to the formation of phosphide compounds having a lower free energy and hence may preferentially form compared to AlP. Only a trace P addition was found to have a profound effect on the nucleation process. The nucleation kinetics is discussed on the basis of the classical nucleation theory and the free growth model, respectively. The estimated AlP patch size was found to be sufficient for the free growth of Si to occur within the droplets, which strongly indicates that the nucleation of Si on an AlP patch or AlP particle is a limiting step for free growth. The maximum nucleation site density within one droplet is directly related to the size distribution of AlP particles or AlP patches for Si nucleation, but is independent of the cooling rates. Although the nucleation conditions were optimized in entrained droplet experiments, the observed mechanisms are also valid at moderate cooling conditions, such as in shape casting.

  5. Genotypic and phenotypic diversity of Ralstonia pickettii and Ralstonia insidiosa isolates from clinical and environmental sources including High-purity Water. Diversity in Ralstonia pickettii

    PubMed Central

    2011-01-01

    Background Ralstonia pickettii is a nosocomial infectious agent and a significant industrial contaminant. It has been found in many different environments including clinical situations, soil and industrial High Purity Water. This study compares the phenotypic and genotypic diversity of a selection of strains of Ralstonia collected from a variety of sources. Results Ralstonia isolates (fifty-nine) from clinical, industrial and environmental origins were compared genotypically using i) Species-specific-PCR, ii) PCR and sequencing of the 16S-23S rRNA Interspatial region (ISR) iii) the fliC gene genes, iv) RAPD and BOX-PCR and v) phenotypically using biochemical testing. The species specific-PCR identified fifteen out of fifty-nine designated R. pickettii isolates as actually being the closely related species R. insidiosa. PCR-ribotyping of the 16S-23S rRNA ISR indicated few major differences between the isolates. Analysis of all isolates demonstrated different banding patterns for both the RAPD and BOX primers however these were found not to vary significantly. Conclusions R. pickettii species isolated from wide geographic and environmental sources appear to be reasonably homogenous based on genotypic and phenotypic characteristics. R. insidiosa can at present only be distinguished from R. pickettii using species specific PCR. R. pickettii and R. insidiosa isolates do not differ significantly phenotypically or genotypically based on environmental or geographical origin. PMID:21878094

  6. In vitro and in vivo studies on the degradation of high-purity Mg (99.99wt.%) screw with femoral intracondylar fractured rabbit model.

    PubMed

    Han, Pei; Cheng, Pengfei; Zhang, Shaoxiang; Zhao, Changli; Ni, Jiahua; Zhang, Yuanzhuang; Zhong, Wanrun; Hou, Peng; Zhang, Xiaonong; Zheng, Yufeng; Chai, Yimin

    2015-09-01

    High-purity magnesium (HP Mg) takes advantage in no alloying toxic elements and slower degradation rate in lack of second phases and micro-galvanic corrosion. In this study, as rolled HP Mg was fabricated into screws and went through in vitro immersion tests, cytotoxicity test and bioactive analysis. The HP Mg screws performed uniform corrosion behavior in vitro, and its extraction promoted cell viability, bone alkaline phosphatase (ALP) activity, and mRNA expression of osteogenic differentiation related gene, i.e. ALP, osteopontin (OPN) and RUNX2 of human bone marrow mesenchymal stem cells (hBMSCs). Then HP Mg screws were implanted in vivo as load-bearing implant to fix bone fracture and subsequently gross observation, range of motion (ROM), X-ray scanning, qualitative micro-computed tomography (μCT) analysis, histological analysis, bending-force test and SEM morphology of retrieved screws were performed respectively at 4, 8, 16 and 24 weeks. As a result, the retrieved HP Mg screws in fixation of rabbit femoral intracondylar fracture showed uniform degradation morphology and enough bending force. However, part of PLLA screws was broken in bolt, although its screw thread was still intact. Good osseointegration was revealed surrounding HP Mg screws and increased bone volume and bone mineral density were detected at fracture gap, indicating the rigid fixation and enhanced fracture healing process provided by HP Mg screws. Consequently, the HP Mg showed great potential as internal fixation devices in intra-articular fracture operation. PMID:26117658

  7. Robust Low-Cost Water-Gas Shift Membrane Reactor for High-Purity Hydrogen Production form Coal-Derived Syngas

    SciTech Connect

    James Torkelson; Neng Ye; Zhijiang Li; Decio Coutinho; Mark Fokema

    2008-05-31

    This report details work performed in an effort to develop a low-cost, robust water gas shift membrane reactor to convert coal-derived syngas into high purity hydrogen. A sulfur- and halide-tolerant water gas shift catalyst and a sulfur-tolerant dense metallic hydrogen-permeable membrane were developed. The materials were integrated into a water gas shift membrane reactor in order to demonstrate the production of >99.97% pure hydrogen from a simulated coal-derived syngas stream containing 2000 ppm hydrogen sulfide. The objectives of the program were to (1) develop a contaminant-tolerant water gas shift catalyst that is able to achieve equilibrium carbon monoxide conversion at high space velocity and low steam to carbon monoxide ratio, (2) develop a contaminant-tolerant hydrogen-permeable membrane with a higher permeability than palladium, (3) demonstrate 1 L/h purified hydrogen production from coal-derived syngas in an integrated catalytic membrane reactor, and (4) conduct a cost analysis of the developed technology.

  8. Process for diffusing metallic coatings into ceramics to improve their voltage withstanding capabilities

    DOEpatents

    Miller, H. Craig; Zuhr, Herbert F.

    1978-01-01

    The disclosure relates to a method for diffusing a coating of manganese powder and titanium powder into a ceramic to improve its voltage hold off withstanding capability. The powder coated ceramic is fired for from about 30 to about 90 minutes within about one atmosphere of wet hydrogen at a temperature within the range of from about 1450.degree. to about 1520.degree. C to cause the mixture to penetrate into the ceramic to a depth on the order of a millimeter.

  9. Ceramic fiber-reinforced monoclinic celsian phase glass-ceramic matrix composite material

    NASA Technical Reports Server (NTRS)

    Bansal, Narottam P. (Inventor); Dicarlo, James A. (Inventor)

    1994-01-01

    A hyridopolysilazane-derived ceramic fiber reinforced monoclinic celsian phase barium aluminum silicate glass-ceramic matrix composite material is prepared by ball-milling an aqueous slurry of BAS glass powder and fine monoclinic celsian seeds. The fibers improve the mechanical strength and fracture toughness and with the matrix provide superior dielectric properties.

  10. Structural Ceramics

    NASA Technical Reports Server (NTRS)

    1986-01-01

    This publication is a compilation of abstracts and slides of papers presented at the NASA Lewis Structural Ceramics Workshop. Collectively, these papers depict the scope of NASA Lewis' structural ceramics program. The technical areas include monolithic SiC and Si3N4 development, ceramic matrix composites, tribology, design methodology, nondestructive evaluation (NDE), fracture mechanics, and corrosion.

  11. Activation of consolidation processes of alumina ceramics

    NASA Astrophysics Data System (ADS)

    Matrenin, S. V.; Zenin, B. S.; Tayukin, R. V.

    2016-02-01

    The methods for activating sintering ceramics based on Al2O3 by mechanical activation in the planetary mill, by adding in the mixture of nanopowders (NP) Al, Al2O3, and submicron powder TiO2, and by applying the technology of spark plasma sintering (SPS) are developed. It has been shown that adding the nanopowder up to 20 wt. % Al2O3 in a coarse powder α-Al2O3 activates the sintering process resulting in increased density and hardness of the sintered alumina ceramics. Substantial effect of increasing density of alumina ceramics due to adding the submicron powder TiO2 in the compound of initial powder mixtures has been established.

  12. High temperature insulation for ceramic matrix composites

    DOEpatents

    Merrill, Gary B.; Morrison, Jay Alan

    2001-01-01

    A ceramic composition is provided to insulate ceramic matrix composites under high temperature, high heat flux environments. The composition comprises a plurality of hollow oxide-based spheres of various dimensions, a phosphate binder, and at least one oxide filler powder, whereby the phosphate binder partially fills gaps between the spheres and the filler powders. The spheres are situated in the phosphate binder and the filler powders such that each sphere is in contact with at least one other sphere. The spheres may be any combination of Mullite spheres, Alumina spheres, or stabilized Zirconia spheres. The filler powder may be any combination of Alumina, Mullite, Ceria, or Hafnia. Preferably, the phosphate binder is Aluminum Ortho-Phosphate. A method of manufacturing the ceramic insulating composition and its application to CMC substrates are also provided.

  13. High temperature insulation for ceramic matrix composites

    DOEpatents

    Merrill, Gary B.; Morrison, Jay Alan

    2004-01-13

    A ceramic composition is provided to insulate ceramic matrix composites under high temperature, high heat flux environments. The composition comprises a plurality of hollow oxide-based spheres of various dimensions, a phosphate binder, and at least one oxide filler powder, whereby the phosphate binder partially fills gaps between the spheres and the filler powders. The spheres are situated in the phosphate binder and the filler powders such that each sphere is in contact with at least one other sphere. The spheres may be any combination of Mullite spheres, Alumina spheres, or stabilized Zirconia spheres. The filler powder may be any combination of Alumina, Mullite, Ceria, or Hafnia. Preferably, the phosphate binder is Aluminum Ortho-Phosphate. A method of manufacturing the ceramic insulating composition and its application to CMC substrates are also provided.

  14. High temperature insulation for ceramic matrix composites

    DOEpatents

    Merrill, Gary B.; Morrison, Jay Alan

    2000-01-01

    A ceramic composition is provided to insulate ceramic matrix composites under high temperature, high heat flux environments. The composite comprises a plurality of hollow oxide-based spheres of varios dimentions, a phosphate binder, and at least one oxide filler powder, whereby the phosphate binder partially fills gaps between the spheres and the filler powders. The spheres are situated in the phosphate binder and the filler powders such that each sphere is in contact with at least one other sphere. The spheres may be any combination of Mullite spheres, Alumina spheres, or stabilized Zirconia spheres. The filler powder may be any combination of Alumina, Mullite, Ceria, or Hafnia. Preferably, the phosphate binder is Aluminum Ortho-Phosphate. A method of manufacturing the ceramic insulating composition and its application to CMC substates are also provided.

  15. Synthesis, structural and electrical properties of La and Nb modified Bi4Ti3O12 ferroelectric ceramics

    NASA Astrophysics Data System (ADS)

    Roy, M.; Bala, Indu; Barbar, S. K.; Jangid, S.; Dave, P.

    2011-11-01

    Polycrystalline ceramic samples of Bi4-xLaxTi3O12 (x=0.0, 0.5 and 1) and Bi3.5La0.5Ti3-yNbyO12 (y=0.02 and 0.04) have been synthesized by standard high temperature solid state reaction method using high purity oxides and carbonates. The effect of lanthanum doping on Bi-site and Nb doping on Ti-site on the structural and electrical properties of Bi4Ti3O12 powders was investigated by X-ray diffraction, scanning electron microscopy, dc conductivity and dielectric studies. A better agreement between the observed and calculated X-ray diffraction pattern was obtained by performing the Rietveld refinement with a structural model using the non-centrosymmetric space group Fmmm in all the cases. A better agreement between observed and calculated d-values also shows that the lattice parameters calculated using the Rietveld refinement analysis are better. The increase in lanthanum and niobium contents does not lead to any secondary phases. It is found that La3+ doping reduces the material grain size and changes its morphology from the plate-like form to a spherical staking like form. The substitution of Nb for Ti ions affected the degree of disorder and modified the dielectric properties leading to more resistive ceramic compounds. The shape and size of the grains are strongly influenced by the addition of niobium to the system. The activation energies of all the compounds were calculated by measuring their dc electrical conductivities. The frequency and temperature dependent dielectric behavior of all the compounds have also been studied and the results are discussed in detail. The substitution of La and Nb on the Bi and Ti sites decreased the Tc and improved the dielectric and ferroelectric behavior.

  16. Porosity and mechanical properties of zirconium ceramics

    SciTech Connect

    Kalatur, Ekaterina Narikovich, Anton; Buyakova, Svetlana E-mail: kulkov@ispms.tsc.ru; Kulkov, Sergey E-mail: kulkov@ispms.tsc.ru

    2014-11-14

    The article studies the porous ceramics consisting of ultra-fine ZrO{sub 2} powders. The porosity of ceramic samples varied from 15% to 80%. The structure of the ceramic materials had a cellular configuration. The distinctive feature of all experimentally obtained strain diagrams is their nonlinearity at low deformations characterized by the parabolic law. It was shown that the observed nonlinear elasticity for low deformations shown in strain diagrams is due to the mechanical instability of cellular elements of the ceramic framework.

  17. Hot isostatic pressing of ceramics

    NASA Technical Reports Server (NTRS)

    Honma, K.

    1985-01-01

    A mixture containing glass 70 to 95 and BN or B4C powder (0.1-10 microns) 5 to 30 vol. % is used as a secondary pressure medium in hot isostatic pressing of ceramics. Thus, Pyrex beads were mixed with 15% vol. BN powder (average diameter 2 microns), fused at 1400 deg for 2 h, cooled, crushed, and put into a graphite crucible. A Si3N4 sintered body was embedded in the powder, heated in vacuum at 1200 deg for 2 h, treated in a hot isostatic press furnace at 1700 deg and 1000 atm. for 1 h, and cooled to give a Si3N4 ceramic. It was easily separated from the crucible.

  18. Coating system to permit direct brazing of ceramics

    DOEpatents

    Cadden, Charles H.; Hosking, F. Michael

    2003-01-01

    This invention relates to a method for preparing the surface of a ceramic component that enables direct brazing using a non-active braze alloy. The present invention also relates to a method for directly brazing a ceramic component to a ceramic or metal member using this method of surface preparation, and to articles produced by using this brazing method. The ceramic can be high purity alumina. The method comprises applying a first coating of a silicon-bearing oxide material (e.g. silicon dioxide or mullite (3Al.sub.2 O.sub.3.2SiO.sub.2) to the ceramic. Next, a thin coating of active metal (e.g. Ti or V) is applied. Finally, a thicker coating of a non-active metal (e.g. Au or Cu) is applied. The coatings can be applied by physical vapor deposition (PVD). Alternatively, the active and non-active metals can be co-deposited (e.g. by sputtering a target made of mullite). After all of the coatings have been applied, the ceramic can be fired at a high temperature in a non-oxidizing environment to promote diffusion, and to enhance bonding of the coatings to the substrate. After firing, the metallized ceramic component can be brazed to other components using a conventional non-active braze alloy. Alternatively, the firing and brazing steps can be combined into a single step. This process can replace the need to perform a "moly-manganese" metallization step.

  19. Corrosion of Silicon-Based Ceramics in Combustion Environments

    NASA Technical Reports Server (NTRS)

    Jacobson, Nathan S.

    1993-01-01

    The processes of passive oxidation, deposit-induced corrosion, active oxidation, scale/substance interactions, and scale volatility are presently studied in the case of high-purity SiC and Si3N4 in pure oxygen, giving attention to such secondary elements in the ceramics as water and CO2 oxidants, combustion environment impurities, and thermal cycling. Deposit-induced corrosion is discussed for the cases of NaSO4 as well as vanadate and oxide-slag deposits; issues associated with the active-to-passive oxidation transition are noted.

  20. Titanium diboride ceramic fiber composites for Hall-Heroult cells

    DOEpatents

    Besmann, T.M.; Lowden, R.A.

    1990-05-29

    An improved cathode structure is described for Hall-Heroult cells for the electrolytic production of aluminum metal. This cathode structure is a preform fiber base material that is infiltrated with electrically conductive titanium diboride using chemical vapor infiltration techniques. The structure exhibits good fracture toughness, and is sufficiently resistant to attack by molten aluminum. Typically, the base can be made from a mat of high purity silicon carbide fibers. Other ceramic or carbon fibers that do not degrade at temperatures below about 1000 C can be used.