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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. Flame synthesis of high purity, nanosized crystalline silicon carbide powder

    SciTech Connect

    Keil, D.G.; Calcote, H.F.; Gill, R.J.

    1996-12-31

    Self-propagating flames in pure silane-acetylene mixtures produce silicon carbide (SiC) powder and hydrogen as main products. Through precise control of the stoichiometry of the reactant gas mixture, it has been possible to produce white SiC at high yields. Characterization of such powders by TEM has shown that the nascent powder consists of polycrystalline hexagonal plates with a narrow size distribution (40 {+-} 7 nm diameter). Infrared spectroscopy of powders indicate microcrystalline SiC and little bound hydrogen. Chemical analysis by the ANSI method showed the powder to be >96 wt% SiC with an impurity of silica (3.9 weight%) due to air exposure of the powder. Traces (0.1 to 0.2 weight%) of both free carbon and free silicon were found. Metal impurities detected by SIMS were typically low: less than 10 ppba for aluminum, sodium, titanium and vanadium. Boron was observed at 10 ppma. Like the oxygen, the boron impurities are probably associated with exposure of the powders to the atmosphere.

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. Reaction synthesis of MoSi sub 2 from high purity elemental powders

    SciTech Connect

    Hardwick, D.A.; Martin, P.L.; Moores, R.J. )

    1992-08-15

    This paper reports that Molybdenum disilicide (MoSi{sub 2}) is an intermetallic compound that combines a high melting point (2293K) with excellent resistance to high temperature oxidation. With respect to mechanical properties the behavior of polycrystalline MoSi{sub 2} falls into one of three regimes, based on the sue temperature: t {lt} 925{degrees} C: strong + brittle; 925 {lt} T {lt} 1250{degrees} C:strong + ductile and T {gt} 1250{degrees} C:weak + ductile. The majority of recent investigations have focused on the properties of MoSi{sub 2}-based materials processed from commercially available powder. Commercial MoSi{sub 2} powder contains significant amounts of oxygen; for example, a chemical analysis of powder obtained from Cerac Inc. revealed an oxygen content of 0.6 wt%. Consolidation of such powder resulted in a substantial volume fraction of amorphous silica in the final product. MoSi{sub 2} powder produced by the crushing and grinding of arc-melted elemental Mo and Si also exhibited amorphous Si-rich particles after vacuum hot-pressing at 1973K and 30MPa. Grinding of the cast material to powder was done in ethanol but one this was driven off, the powder was air-handled. The high energy mechanical alloying in an argon atmosphere of elemental Mo and Si powder to produce MoSi{sub 2} has also been investigated. Following hot pressing, the MoSi{sub 2} made in this fashion still contained a substantial volume fraction of SiO{sub 2}.

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. 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.

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

    SciTech Connect

    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.

  19. 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.

  20. 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.

  1. 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.

  2. 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.

  3. 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.

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

    SciTech Connect

    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.

  5. 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.

  6. Processing of PZT ceramics: aqueous mixing procedures for powder consolidation

    SciTech Connect

    Bunker, B.C.; Lamppa, D.L.; Moore, R.H.

    1986-02-01

    Inhomogeneities in chemical compositions and microstructures can result in lot-to-lot variations in the charge release characteristics of ferroelectric lead-zirconate-titanate ceramics. One source of inhomogeneity is agglomeration and selective sedimentation which occurs during aqueous mixing of the constituent oxides. Procedures using electrostatic and steric stabilization of oxide powders were developed for fabricating homogeneous powder compacts. Use of lead carbonate instead of lead oxide minimizes problems encountered using various slurry stabilization techniques.

  7. 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

  8. 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

  9. A constitutive model for sintering of granulated ceramic powders

    NASA Astrophysics Data System (ADS)

    Shinagawa, K.; Hirashima, Y.

    1998-05-01

    Sintering behavior of granulated powder is investigated to develop a constitutive model for deformation analysis of ceramic powder compacts during sintering. Spray-dried alumina is compacted by CIPing (cold isostatic pressing) and sintered at various temperatures. Shrinkage and the change in grain size of the compacts during sintering are revealed in relation to the inhomogeneous microstructure consisting of fractured and unfractured granules as a consequence of the compaction. A constitutive model for the ceramic powder compacts having the internal structure is presented; The difference in grain growth in dense and sparse regions of the compacts is taken into consideration to the model. The results calculated by the model show good agreement with that obtained by experiment.

  10. 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.

  11. Aerosol flow reactor production of fine Y1Ba2Cu3O7 powder: Fabrication of superconducting ceramics

    NASA Astrophysics Data System (ADS)

    Kodas, T. T.; Engler, E. M.; Lee, V. Y.; Jacowitz, R.; Baum, T. H.; Roche, K.; Parkin, S. S. P.; Young, W. S.; Hughes, S.; Kleder, J.; Auser, W.

    1988-05-01

    An aerosol flow reactor operating at 900-1000 °C is used to prepare high-purity Y1Ba2Cu3O7 powders with a uniform chemical composition and a submicron to micron average particle size by thermally decomposing aerosol droplets of a solution consisting of the nitrate salts of Y, Ba, and Cu in a 1:2:3 ratio. The powders were at least 99% reacted based on thermogravimetric analysis, and the x-ray diffraction pattern is essentially that of Y1Ba2Cu3O7. Magnetic susceptibility measurements showed the powders to be superconducting with a transition at 90 K even for average reactor residence times as short as 20 s. Sintering cold-pressed pellets between 900 and 1000 °C provides dense, fine grained (average size on the order of 1 μm) superconducting ceramics with sharp 90 K transitions. The grain size and shape of a final sintered part could be varied depending on powder production, processing, and sintering conditions.

  12. 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

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. Sinterable Ceramic Powders from Laser Heated Gas Phase Reactions and Rapidly Solidified Ceramic Materials.

    DTIC Science & Technology

    1984-07-01

    ceramic materials. Unusual, attractive densification characteristics have already been observedl with the amorphous powders that can be produced by the...increase with oxygen partial pressure. In air, the effect of additives on surface tension parallelled their effect on the melting point. In most cases...the compositional effects were approximately linear; TiO 2 , an exception, caused a sharp decrease in I for small additions that were followed by

  18. 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.

  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. 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.

  1. Process for producing high purity aromatic compounds

    SciTech Connect

    Mayes, W.W.

    1980-05-20

    High-purity C7 and/or C8 aromatic hydrocarbons are produced by reforming a C7 or C8 full boiling carbon number naphtha feed fraction or combinations thereof under reforming conditions of sufficient severity to convert essentially all of the nonaromatic portion of the naphtha feed boiling in the C7 to C8 aromatic boiling range to C7 and/or C8 aromatics, and then separating the reformate by fractional distillation into highpurity fractions of C7 and/or C8 aromatic hydrocarbons. Preferably, the C7 and/or C8 full boiling carbon number naphtha feed fraction is reformed in a plurality of reformer reaction stages with increasingly more severe conditions in order to maximize the yield of the C7 and C8 aromatics.

  2. High purity silica reflective heat shield development

    NASA Technical Reports Server (NTRS)

    Blome, J.

    1974-01-01

    Progress is reported on the development of a high purity reflective heat shield material. Silicon dioxide was selected as the material because it is highly reflective in the correct wavelength band, has good ablation characteristics, is thermal shock resistant, and is readily fabricated to full size at reasonable cost. Conclusions indicate that: reflectance is affected by purity and morphology; the pure material is readily available; required purity and morphology can be maintained with reasonable care; high reflectances are determined (0.99 from 0.4 to 1.2 microns); major processing steps are defined; and the material appears to be cost effective. It is indicated that the materials are developed to the point of readiness for full scale fabrication and characterization.

  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. 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.

  5. 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.

  6. Biaxial deformation in high purity aluminum

    DOE PAGES

    Livescu, V.; Bingert, J. F.; Liu, C.; ...

    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

  7. 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.

  8. 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.

  9. 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.

  10. Synthesis of High Purity Sinterable Silicon Carbide Powder

    DTIC Science & Technology

    1989-11-01

    1972). Banque de donnees thermodynamiques , Thermodata, Bibliotheque uni- versitäre de Saint-Martin d’Hyeres, Grenoble (1977). Hirschfelder...34 University of Bari. Italy (1972). Fauchais, P. "Etude des proprietes thermodynamiques des plasmas d’arc" These d’Etat, Universite de...de l’equilibre thermodynamique des systemes chimiques soumis a des temperatures isothermes et isobare". 3.15 Moore C.E., Atomic Energy Levels, NBS

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. Promotion of powder crystallinity and its influence on the properties of Nd:YAG transparent ceramics

    NASA Astrophysics Data System (ADS)

    Ma, Benyuan; Wang, Bin; Zhang, Wei; Wei, Nian; Lu, Tiecheng; He, Junbao

    2017-02-01

    The Nd:YAG raw powders of various crystallinities were obtained from the co-precipitated precursor by calcining at 1100-1250 °C for 2-6 h. XRD, HRTEM and EDX were employed to analyze the powder crystallinity, e.g., its phases, changes of lattice constants, surface defects and morphologies. The subsequent ceramics were fabricated by simply vacuum sintering at 1780 °C for 10 h to well compare the initial intrinsic effect of various powder crystallinities. The induced defect states and corresponding properties of ceramics were explored and discussed. The results show that poorly crystallized powder involves a thick layer on particle surface, which is not well crystallized but can escape XRD detection. This poorly crystallized powder contributes more the inhomogeneous ceramic sintering and introduces more the defects in final ceramics, e.g., impure phase inclusions and dislocations. The results reveal that powder crystallinity should be promoted and considered as a further way to improve ceramic properties.

  16. Study on Microstructures and Properties of Porous TiC Ceramics Fabricated by Powder Metallurgy

    NASA Astrophysics Data System (ADS)

    Ma, Yana; Bao, Chonggao; Han, Longhao; Chen, Jie

    2017-02-01

    Powder metallurgy process was used to fabricate porous titanium carbide (TiC) ceramics, in which TiC powders were taken as the raw materials, nickel was used as the metallic binder and urea was the space-holder. Microstructure, composition and phase of porous TiC ceramics were characterized by scanning electron microscopy (SEM) and x-ray diffraction (XRD). Flexure strength of the porous TiC ceramics was tested by a three-point bending method. The results show that macropores and micropores coexist in the prepared porous TiC ceramics. Moreover, the pore number, size and distribution in porous TiC ceramics can be controlled on demand. Particularly, the factors such as the number or size of space-holder, compacting pressure and Ni content have significant effect on the porosity and flexure strength.

  17. Study on Microstructures and Properties of Porous TiC Ceramics Fabricated by Powder Metallurgy

    NASA Astrophysics Data System (ADS)

    Ma, Yana; Bao, Chonggao; Han, Longhao; Chen, Jie

    2017-01-01

    Powder metallurgy process was used to fabricate porous titanium carbide (TiC) ceramics, in which TiC powders were taken as the raw materials, nickel was used as the metallic binder and urea was the space-holder. Microstructure, composition and phase of porous TiC ceramics were characterized by scanning electron microscopy (SEM) and x-ray diffraction (XRD). Flexure strength of the porous TiC ceramics was tested by a three-point bending method. The results show that macropores and micropores coexist in the prepared porous TiC ceramics. Moreover, the pore number, size and distribution in porous TiC ceramics can be controlled on demand. Particularly, the factors such as the number or size of space-holder, compacting pressure and Ni content have significant effect on the porosity and flexure strength.

  18. 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.

  19. 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.

  20. 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.

  1. 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

  2. Production of High Purity Niobium Ingots at CBMM

    NASA Astrophysics Data System (ADS)

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

    2011-03-01

    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.

  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. 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.

  5. 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.

  6. 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.

  7. 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%.

  8. 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.

  9. 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.

  10. 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%.

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

    NASA Astrophysics Data System (ADS)

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

    2016-08-01

    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.

  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. Luminescence and photoconductivity of high-purity cadmium selenide

    SciTech Connect

    Martynov, V.N.

    1995-10-01

    Slightly off-stoichlometric high-purity cadmium and zinc chalcogenides are used as high-efficiency sensors in various optoelectronic devices. The procedure for preparing high-purity chalcogenides was described elsewhere. Such materials (wurtzite-type structure, sp. gr. C{sup 4}{sub 6v}) exhibit exciton luminescence and the photoconductivity associated with the A-, B-, and C-excitonic series over a wide temperature range. In this work, we studied the luminescence and photoconductivity (PC) of cadmium selenide prepared as described.

  14. Preparation of ceramic grade UO 2 powder by atomization from uranyl nitrate solutions

    NASA Astrophysics Data System (ADS)

    Lainetti, P.; Riella, H. Gracher

    1991-02-01

    The thermal denitration of a nitrate solution by direct conversion to a ceramic grade uranium dioxide powder, in a furnace that combines atomization nozzle and gas stirred bed, is an attractive method because no liquid waste products are formed and it has relative simplicity. The UO 2 powder characteristics, such as size, shape, specific surface area and sinterability as a function of procedural variables were determined. This technique has been developed in the pelleting pilot plant of the IPEN/CNEN-SP and it appears to be practical and economically feasible for wet recovery of rejected UO 2 powders and pellets from production process, with the recovered powder being directly mixed to the powder from the AUC reduction process.

  15. Electrical Characteristics of NTC Thermistor Ceramics Made of Mechanically Activated Fe2O3 Powder Derived from Yarosite

    NASA Astrophysics Data System (ADS)

    Syarif, D. Gustaman; Ramelan, A.

    2008-03-01

    Electrical characteristics of ceramics for NTC thermistor made of mechanically activated Fe2O3 powder which was derived from yarosite mineral has been studied. The powder of Fe2O3 was derived from yarosite mineral by precipitation and calcination. The powder was mechanically activated by blending using an electric blending machine. The ceramics were produced by pressing the calcined and activated powders to produce pellets and sintering the pellets at 1100 °C and 1200 °C for 1 hour in air. Electrical characterization was done by measuring electrical resistivity of the ceramics at various temperatures (25 °C-100 °C). Microstructure and structural analyses were carried out by using a Scanning Electron Microscope (SEM) and X-ray diffraction (XRD), respectively. The XRD analyses showed that the sintered ceramics had crystal structure of hexagonal (hematite). The presence of second phase could not be identified from the XRD analyses. From SEM data, it was known that the ceramics from activated powder had larger grains due to small size of the activated powder. According to the electrical data, it was known that the ceramics made of the activated powder had lower thermistor constant (B) and room temperature electrical resistivity (ρRT). The value of B and ρRT of the produced ceramics fitted market requirement.

  16. Sinterable Ceramic Powders from Laser-Heated Gases.

    DTIC Science & Technology

    1988-02-01

    toughness ( Nitriding kinetics RBSN oxidation kinetics I SiC sintering kinetics , Particle surface chemistr Oxide melt density Anhydrous dispers Oxide melt...materials. Pure anhydrous solvent and solvent-dispersant systems were identified that could be used to fully disperse Si and SIC powders. Stabilization...powders (1), SiH4 mixed with methane (CH 4 ) or ethylene (C2H4) is used to make SiC (3), and SiH4 nixed with amonia is used to make Si 3 N4 (1,4). Under

  17. 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.

  18. 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.

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

    DOEpatents

    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).

  20. 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.

  1. Zirconia-Based Powders Produced by Plasma-Spray Pyrolisys and Properties of Sintered Ceramics

    NASA Astrophysics Data System (ADS)

    Kulkov, S. N.; Buyakova, S.; Gömze, L. A.

    2017-01-01

    It have been studied zirconia-based powders and sintered ceramic. It was shown that in the porous structure of zirconia-based ceramics there is a critical value of porosity the material divides into two sub-systems, being variously deformable under external loading. It have been shown that m-phase in ZrO2 is formed due to increase in the microdistortion level which destabilizes the nanocrystalline t phase. It has been found out the correlation between the sizes of crystallites and porosity, which associated with transition of the isolated porous structure to the continuous one and the porosity of 20%, corresponds to the first percolation threshold.

  2. Strontium substituted calcium phosphate biphasic ceramics obtained by a powder precipitation method.

    PubMed

    Kim, Hae-Won; Koh, Young-Hag; Kong, Young-Min; Kang, Jun-Gu; Kim, Hyoun-Ee

    2004-10-01

    Strontium (Sr) substituted calcium phosphate ceramics were fabricated using a powder precipitation method. The Sr ions were added up to 8 mol % to replace the Ca ions during the powder preparation. Composition analysis showed that the added Sr was not fully incorporated within the as-precipitated apatite structure, presumably being washed out during the powder preparation. After calcination, the Sr containing powders were crystallized into apatite and tricalcium phosphate (TCP), that is, biphasic calcium phosphates were formed. The amount of TCP increased with increasing the Sr addition. The lattice parameters of the calcined powders increased gradually with Sr substitution in both the a- and c-axis. However, the obtained values deviated slightly from the calculated ones at higher Sr additions (>4%) due to the partial substitution of Sr ions. The microstructure of the sintered bodies changed with the Sr addition due to the formation of TCP. The Vickers hardness increased slightly from 5.2 to 5.5 MPa with increasing Sr addition, which was driven by the HA+TCP biphasic formation. The osteoblast-like cells cultured on the Sr-substituted biphasic sample spread and grew actively. The proliferation rate of the cells was higher in the samples containing more Sr. The alkaline phosphate activity of the cells was expressed to a higher degree with increasing Sr addition. These observations confirmed the enhanced cell viability and differentiation of the Sr-substituted biphasic calcium phosphate ceramics.

  3. Effect of nanoscale powders and microwave sintering on densification of alumina ceramics

    NASA Astrophysics Data System (ADS)

    Yun, Han-Sol; Kim, Jong-Chan; Jeong, Dae-Yong; Cho, Nam-Hee

    2016-11-01

    Nanoscale alumina (Al2O3) powders with an average size of 100, 200, or 300 nm were sintered to investigate the effects of the initial powder size on the densification behavior under the application of microwaves (2.45 GHz, 2 kW). The sintering was performed using microwave-assisted sintering (MWS) and conventional sintering (CS) methods in the temperature range of 1100-1600 °C for 0-180 min. The Al2O3 samples prepared with the 100-nm-sized powders using MWS exhibited a relative density (RD) of over 90% when sintered at 1200 °C for 10 min; the same RD was achieved at 1500 °C when the sintering was performed for the same time using CS. However, a sintering temperature difference of 100 °C for a RD of 90% was observed between the MWS and CS methods for the 300-nm-sized powders. Nano-grained ( 290 nm) Al2O3 ceramics with a high density of ≥90% were obtained from nanoscale powders ( 100 nm) using MWS methods. The response of the nanoscale powders to microwaves was more significant as the initial powder size decreased from 300 to 100 nm.

  4. 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

  5. USE OF COMBUSTION SYNTHESIS IN PREPARING CERAMIC-MATRIX AND METAL-MATRIX COMPOSITE POWDERS

    SciTech Connect

    Weil, K. Scott; Hardy, John S.

    2005-03-01

    A standard combustion-based approach typically used to synthesize nanosize oxide powders has been modified to prepare composite oxide-metal powders for subsequent densification via sintering or hot-pressing into ceramic- or metal-matrix composites. Copper and cerium nitrate salts were dissolved in the appropriate ratio in water and combined with glycine, then heated to cause autoignition. The ratio of glycine-to-total nitrate concentration was found to have the largest effect on the composition, agglomerate size, crystallite size, and dispersivity of phases in the powder product. After consolidation and sintering under reducing conditions, the resulting composite compact consists of a well-dispersed mixture of sub-micron size reinforcement particles in a fine-grained matrix.

  6. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2008-03-01

    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 °C, 1200 °C, 1300 °C and 1350 °C) then characterized by varies analysis techniques. XRD analysis shows that spinel, μ-cordierite and cristobalite are formed at 1000 °C which spinel as predominant phase. At 1200 °C, μ-cordierite occured as predominant phase, spinel, sapphirine and cristobalite are formed as minor phases. It also confirmed that high purity α-cordierite formed at 1300 °C and clearly observed at 1350 °C. Result of EDX analysis proved that magnesium, aluminum, silicon and oxygen was existed in the cordierite.

  8. 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).

  9. 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.

  10. 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.

  11. Bulk and surface effects in segmented high purity germanium detectors

    NASA Astrophysics Data System (ADS)

    Abt, I.; Caldwell, A.; Dönmez, B.; Irlbeck, S.; Majorovits, B.; Volynets, O.

    2013-08-01

    Segmented high-purity germanium detectors have been developed for a variety of experiments. The segmentation is used to augment the excellent energy resolution of such a device with spatial information to disentangle event topologies. Several performance aspects of true-coaxial segmented detectors are presented, especially the effects due to the crystallographic axes and the problem of events close to the surfaces of the detector. A test stand and Monte Carlo tools developed to study such effects are introduced. The simulation tools can also be used to design novel detectors, such as segmented point-contact detectors. A particular design is presented and discussed.

  12. Plasma Processed Nanosized-Powders of Refractory Compounds for Obtaining Fine-Grained Advanced Ceramics

    NASA Astrophysics Data System (ADS)

    I, Zalite; J, Grabis; E, Palcevskis; M, Herrmann

    2011-10-01

    One of the ways for the production of ceramic materials with a fine-grained structure is the use of nanopowders. Different methods are used for the production of nanopowders. One of them is the method of plasmachemical synthesis. Different nanopowders of refractory materials can be obtained by this method. The preparation of nanosized powders of nitrides and oxides and their composites by the method of plasmachemical synthesis, the possibilities to receive nanopowders with different particle size and the potential advantages of nanopowders were investigated.

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. 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.

  18. 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.

  19. Blue upconversion emission from Tm3+ sensitized by Nd3+ in aluminum oxide crystalline ceramic powders

    NASA Astrophysics Data System (ADS)

    Rakov, N.; Gómez, L. A.; Rátiva, D. J.; Maciel, G. S.

    2009-02-01

    Upconversion (UC) emission in thulium (Tm3+) and neodymium (Nd3+) co-doped aluminum oxide ceramic powders prepared by combustion synthesis was investigated at room temperature using a continuous wave laser operating at 800 nm. Our sample containing Tm3+ (1 wt.%) did not show any UC emission but our sample co-doped with Tm3+ and Nd3+ in 1:2 wt.% proportion presented blue (˜480 nm) UC intensity more than one order of magnitude larger than our sample co-doped with Tm3+ and Nd3+ in 1:1 wt.% proportion. X-ray diffraction data showed the presence of α-Al2O3 and REAlO3 (RE=Tm or Nd) crystalline phases in co-doped powders, while the singly doped powder has only α-Al2O3 phase. Our results show that the UC emission efficiency of Tm3+ and the host crystalline structure can be tailored by manipulating the Nd3+ doping concentration.

  20. Automation of the Characterization of High Purity Germanium Detectors

    NASA Astrophysics Data System (ADS)

    Dugger, Charles ``Chip''

    2014-09-01

    Neutrinoless double beta decay is a rare hypothesized process that may yield valuable insight into the fundamental properties of the neutrino. Currently there are several experiments trying to observe this process, including the Majorana DEMONSTRAOR experiment, which uses high purity germanium (HPGe) detectors to generate and search for these events. Because the event happens internally, it is essential to have the lowest background possible. This is done through passive detector shielding, as well as event discrimination techniques that distinguish between multi-site events characteristic of gamma-radiation, and single-site events characteristic of neutrinoless double beta decay. Before fielding such an experiment, the radiation response of the detectors must be characterized. A robotic arm is being tested for future calibration of HPGe detectors. The arm will hold a source at locations relative to the crystal while data is acquired. Several radioactive sources of varying energy levels will be used to determine the characteristics of the crystal. In this poster, I will present our work with the robot, as well as the characterization of data we took with an underground HPGe detector at the WIPP facility in Carlsbad, NM (2013). Neutrinoless double beta decay is a rare hypothesized process that may yield valuable insight into the fundamental properties of the neutrino. Currently there are several experiments trying to observe this process, including the Majorana DEMONSTRAOR experiment, which uses high purity germanium (HPGe) detectors to generate and search for these events. Because the event happens internally, it is essential to have the lowest background possible. This is done through passive detector shielding, as well as event discrimination techniques that distinguish between multi-site events characteristic of gamma-radiation, and single-site events characteristic of neutrinoless double beta decay. Before fielding such an experiment, the radiation response of

  1. 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.

  2. 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.

  3. PERFORMANCES OF HIGH PURITY NIOBIUM CAVITIES WITH DIFFERENT GRAIN SIZES

    SciTech Connect

    Gianluigi Ciovati; Peter Kneisel; Ganapati Myneni; Swapan Chattopadhyay

    2006-08-21

    Grain boundaries have for some time been suspected of influencing the performance of RF cavities made from high purity niobium by limiting the temperature dependent BCS surface resistance to a residual resistance because of impurity segregation and by causing field limitations due to flux penetration. We have carried out a comparative study of the RF behavior of 2.2 GHz TM{sub 010} cavities of identical shape, fabricated from single crystal niobium, niobium of grain sizes of the order of several cm{sup 2} and standard poly-crystalline material. All the cavities were treated with buffered chemical polishing (BCP), post-purified at 1250 ?C and ?in-situ? baked at 120 C. This contribution reports about the results of the measurements of the temperature dependence of the surface resistance Rs(T) and the Q0 vs. Eacc behavior at 2 K. From the analysis of the Rs(T) data at low RF fields material parameters such as gap value, mean free path and residual resistance could be extracted. The dependence of the Q-value on RF field was analyzed with respect to the medium field Q-slope, Q-drop at high fields and the quench fields. The best performance resulted in a breakdown field of {approx}165 mT, corresponding to an accelerating gradient of E{sub acc} {approx} 38 MV/m.

  4. PERFORMANCES OF HIGH PURITY NIOBIUM CAVITIES WITH DIFFERENT GRAIN SIZES

    SciTech Connect

    Gianluigi Ciovati; Peter Kneisel; Ganapati Myneni; Ganapati Rao Myneni; Ganapati Rao Myneni; Swapan Chattopadhyay

    2006-08-04

    Grain boundaries have for some time been suspected of influencing the performance of RF cavities made from high purity niobium by limiting the temperature dependent BCS surface resistance to a residual resistance because of impurity segregation and by causing field limitations due to flux penetration. We have carried out a comparative study of the RF behavior of 2.2 GHz TM010 cavities of identical shape, fabricated from single crystal niobium, niobium of grain sizes of the order of several cm2 and standard poly-crystalline material. All the cavities were treated with buffered chemical polishing (BCP), post-purified at 1250 C and ''in-situ'' baked at 120 C. This contribution reports about the results of the measurements of the temperature dependence of the surface resistance Rs(T) and the Q0 vs. Eacc behavior at 2 K. From the analysis of the Rs(T) data at low RF fields material parameters such as gap value, mean free path and residual resistance could be extracted. The dependence of the Q-value on RF field was analyzed with respect to the medium field Q-slope, ''Q-drop'' at high fields and the ''quench'' fields. The best performance resulted in a breakdown field of {approx} 165 mT, corresponding to an accelerating gradient of Eacc {approx} 38 MV/m.

  5. 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).

  6. 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.

  7. 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.

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

    NASA Astrophysics Data System (ADS)

    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.

  9. 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.

  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.

    2000-05-01

    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.

  11. 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.

  12. 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.

  13. Reaction synthesis of dynamically densified titanium-based intermetallic and ceramic-forming powders

    NASA Astrophysics Data System (ADS)

    Namjoshi, Shantanu Ashok

    The mechanism(s) and kinetics of the reaction synthesis of dynamically-densified Ti-based intermetallic and ceramic forming powder mixtures were investigated in this study. Dynamic densification employing shock-compression produces a dense-packed and highly-activated state of powder mixture constituents resulting in significantly increased mass transport rates and enhanced chemical reactivity. Green density compacts (˜85--95% TMD) of Ti-Si, Ti-B, and Ti-Al powder mixtures, obtained using shock-densification under different loading conditions, were heat treated in an inert atmosphere, at their respective eutectic temperatures. Microstructural observation showed evidence of reaction initiating in the solid state, but eventually being taken over by a self sustained combustion type reaction mechanism. Activation energies determined using differential thermal analysis were used to correlate the reaction behavior in Ti-Si (as the model system), based on Carter's kinetic model for solid-state reactions and the Johnson-Mehl-Avrami kinetics for the combustion-type reaction, with experimental measurements of fraction of Ti5Si3 formed as a function of time and temperature. It was confirmed that in Ti-Si dynamically-densified powder compacts the reaction occurs in the solid-state up to temperatures <1000°C, but with further increase in temperature the reaction is taken over by a combustion-type reaction. The Ti-Si compacts thus produced are 92--95% dense and show a fully reacted Ti5Si3 microstructure, with ~6 mum grain size and ˜800 kg/mm2 microhardness. A predictive model was developed, incorporating a balance between rate of heat generation (due to reaction) and heat dissipation, to determine optimum synthesis conditions under which the reaction occurs in the solid state without being taken over by the combustion mode. The model considered synthesis temperature, compact porosity, and activation energy as the variables, to determine the fraction reacted as a function of

  14. 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.

  15. A light hydrocarbon fuel processor producing high-purity hydrogen

    NASA Astrophysics Data System (ADS)

    Löffler, Daniel G.; Taylor, Kyle; Mason, Dylan

    This paper discusses the design process and presents performance data for a dual fuel (natural gas and LPG) fuel processor for PEM fuel cells delivering between 2 and 8 kW electric power in stationary applications. The fuel processor resulted from a series of design compromises made to address different design constraints. First, the product quality was selected; then, the unit operations needed to achieve that product quality were chosen from the pool of available technologies. Next, the specific equipment needed for each unit operation was selected. Finally, the unit operations were thermally integrated to achieve high thermal efficiency. Early in the design process, it was decided that the fuel processor would deliver high-purity hydrogen. Hydrogen can be separated from other gases by pressure-driven processes based on either selective adsorption or permeation. The pressure requirement made steam reforming (SR) the preferred reforming technology because it does not require compression of combustion air; therefore, steam reforming is more efficient in a high-pressure fuel processor than alternative technologies like autothermal reforming (ATR) or partial oxidation (POX), where the combustion occurs at the pressure of the process stream. A low-temperature pre-reformer reactor is needed upstream of a steam reformer to suppress coke formation; yet, low temperatures facilitate the formation of metal sulfides that deactivate the catalyst. For this reason, a desulfurization unit is needed upstream of the pre-reformer. Hydrogen separation was implemented using a palladium alloy membrane. Packed beds were chosen for the pre-reformer and reformer reactors primarily because of their low cost, relatively simple operation and low maintenance. Commercial, off-the-shelf balance of plant (BOP) components (pumps, valves, and heat exchangers) were used to integrate the unit operations. The fuel processor delivers up to 100 slm hydrogen >99.9% pure with <1 ppm CO, <3 ppm CO 2. The

  16. 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).

  17. 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.

  18. Preparation of high purity lanthanum compounds for use in fluoride optical fibers

    SciTech Connect

    Ewing, K.J.; Buckner, L.; Jaganathan, J.; Ginther, R.; Aggarwal, I.D. . Optical Sciences Div.)

    1989-02-01

    The preparation of ultra-pure lanthanum nitrate by co-precipitation is described. Preparation of high purity lanthanum carbonate from the pure nitrate is also described. Hydrofluorination of pure lanthanum carbonate produces high purity lanthanum fluoride used in the preparation of heavy metal fluoride glasses.

  19. 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.

  20. 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

  1. 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.

  2. Synthesis of High Purity Silicon from Rice Husks

    NASA Astrophysics Data System (ADS)

    Larbi, Kingsley Kweku

    Impurity optimized silicon is needed for the advancement of terrestrial photovoltaic power generation. In this study the possibility of producing solar grade silicon from rice husks has been pursued. An integrated process flowsheet was developed and practiced that included initial leaching, reduction of Rice husk ash (RHA) and post-reduction purification of silicon. Metallothermic reduction of purified RHA with magnesium was investigated within the temperature range of 500-950 °C. The reduction product was purified by two stage acid leaching sequence. Analysis of the final silicon powder product by XRD and ICP-OES showed crystalline silicon with boron content to be less than 3ppm- corresponding to reduction by a factor greater than 10, whilst the phosphorus content was reduced by a factor of over 20 and reaching less than 73ppm. The effects of temperature, magnesium amount and leaching agents optimized in this study. A one step test melting was also carried out to convert the silicon powder into silicon chunks.

  3. The Response of Ceramic Powders to High-Level Quasi-Isentropic Dynamic Loads

    NASA Astrophysics Data System (ADS)

    Lawrence, R. J.; Grady, D. E.; Hall, C. A.

    2004-07-01

    The pulsed-power Z machine, in an isentropic compression experiment (ICE) mode, will allow the dynamic characterization of porous materials—here various ceramic powders, e.g., Al2O3, WC, ZrO2—at roughly half their solid densities. A cylindrical configuration can provide megabar-level loads on an annulus of the sample material. Data will be provided by velocity interferometers that measure free-surface (or possibly interface) particle velocities. Differing sample thicknesses using stepped or conical geometries yield experimental efficiency by allowing multiple data records on single shots. With the p/α model for porous materials, the one-dimensional Lagrangian hydrocode WONDY provides the needed analyses. Based on static data, both power-law and quadratic crush curves are employed. Within the model constraints, we suggest that the most important parameter for characterizing the material is the crush strength, ps. With adequate sample thicknesses, the planned velocity measurements differentiate among the various assumptions for ps.

  4. Low temperature fabrication from nano-size ceramic powders. Final report

    SciTech Connect

    Gonzalez, E.J.; Piermarini, G.J.; Hockey, B.; Malghan, S.G.; Danforth, S.C.; Pechenik, A.

    1995-04-28

    Understanding of compaction and rheology of ceramic powders is needed for production of defect-free greenware. High pressure and lubricating media (liq. N{sub 2}, pentane) were used for increased green body density. High green densities could be achieved with nanosize Si nitride and {gamma} alumina. A pressure/temperature system was built which uses an Instron screw-driven press and a piston/cylinder die. Max random packing density of 57 {plus_minus} 2% theoretical was achieved for dry compaction of Si nitride at 2.5 GPa and RT; compaction under liq. N{sub 2} gave 64 {plus_minus} 2%. Dry compaction of alumina was 64% theoretical at 2.5 GPa. Pressureless sintering of Si nitride green compacts did not result in further densification. Hot pressing increased the hardness. In alumina, increased compaction pressure enhances the {gamma}-{alpha} transition and increases the densification upon heat treatment. It is difficult to obtain dense material without coarsened pore/grain microstructure. SANS showed alumina results similar to those found for materials made by inert-gas-condensation. Theoretical studies were also made to model the compaction process. Future studies are outlined.

  5. 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.

  6. 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.

  7. 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

    2016-04-11

    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.

  8. 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.

  9. 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

  10. Effects of grinding on properties of Mg-PSZ ceramics prepared by the surface enrichment of zirconia powders

    SciTech Connect

    Deb, S.; Das, S.R.

    1995-10-01

    Commercial grade zirconia powders of mean particle size of 3.21 microns were super-ground in wet condition in alcoholic medium in a Planetary Ball-Mill for 12-hours using a zirconia pot as well as balls, in order to avoid contaminations from the grinding media. Sedigraph analysis data show the mean particle sizes within the range of 0.4 to 0.2 micron. The super-ground zirconia powders were then treated with appropriate acid and alkali solutions in order to enrich the surfaces of zirconia powders. The chemical analysis reports depict the enrichment phenomena of the processed zirconia powders. Magnesium oxide of different mole percentages (3 to 9%) have been incorporated to the above super-ground and enriched zirconia powder and green specimens were prepared by pressing with a suitable pressure of 200 MPa to yield the green compaction density of 3.06 gm/cm{sup 3}. The compacted green specimens were sintered without pressure at 1,480 C in air followed by normal cooling. X-ray diffraction patterns of the above sintered and cooled specimens have confirmed the formation of Mg-PSZ ceramics with 40% tetragonal phase. The sintered PSZ-products have shown very good surface properties but at the cost of transverse rupture strength. The effects of grinding were observed on the above Mg-PSZ ceramics which exhibit very little change in the tetragonal phase even after 30-minutes of grinding with a 60-mesh diamond wheel at a normal pressure of 4 kg/cm{sup 2}.

  11. Investigation by laser induced breakdown spectroscopy, X-ray fluorescence and X-ray powder diffraction of the chemical composition of white clay ceramic tiles from Veliki Preslav

    NASA Astrophysics Data System (ADS)

    Blagoev, K.; Grozeva, M.; Malcheva, G.; Neykova, S.

    2013-01-01

    The paper presents the results of the application of laser induced breakdown spectroscopy, X-ray fluorescence spectrometry, and X-ray powder diffraction in assessing the chemical and phase composition of white clay decorative ceramic tiles from the medieval archaeological site of Veliki Preslav, a Bulgarian capital in the period 893-972 AC, well-known for its original ceramic production. Numerous white clay ceramic tiles with highly varied decoration, produced for wall decoration of city's churches and palaces, were found during the archaeological excavations in the old capital. The examination of fourteen ceramic tiles discovered in one of the city's monasteries is aimed at characterization of the chemical profile of the white-clay decorative ceramics produced in Veliki Preslav. Combining different methods and comparing the obtained results provides complementary information regarding the white-clay ceramic production in Veliki Preslav and complete chemical characterization of the examined artefacts.

  12. Non-Polymeric Binders for Ceramic Powders: Utilization of Neutral and Ionic Species Derived from Decaborane(14)

    DTIC Science & Technology

    1989-05-13

    with Eurotherm controllers were used for all preparative scale (>1 g) pyrolyses (powder and bulk). For pyrolyses to 10000C, 3.75 cm o.d. quartz tubes and... pyrolyses were carried out under an atmosphere of flowing argon. For experiments to 10000C the flow rate was -6-8 L/h and for experiments to 15000C it...1 2 -2Ph 2 PCI [10]. The results of their pyrolyses (i.e., their ceramic yields and compositions) are given in Table I. 2.3. General Procedure for

  13. The Next Generation Safeguards Initiative s High-Purity Uranium-233 Preservation Effort

    SciTech Connect

    Krichinsky, Alan M; Bostick, Debra A; Giaquinto, Joseph; Bayne, Charles; Goldberg, Dr. Steven A.; Humphrey, Dr. Marc; Hutcheon, Dr. Ian D.; Sobolev, Taissa

    2012-01-01

    High-purity 233U serves as a crucial reference material for accurately quantifying and characterizing uranium. The most accurate analytical results which can be obtained only with high-purity 233U certified reference material (CRM) are required when used to confirm compliance with international safeguards obligations and international nonproliferation agreements. The U.S. supply of 233U CRM is almost depleted, and existing domestic stocks of this synthetic isotope are scheduled to be down-blended for disposition with depleted uranium beginning in 2015. Down blending batches of high-purity 233U will permanently eliminate the value of this material as a CRM. Furthermore, no replacement 233U stocks are expected to be produced in the future due to a lack of operating production capability and the high cost of replacing such capability. Therefore, preserving select batches of high-purity 233U is of great value and will assist in retaining current analytical capabilities for uranium-bearing samples. Any organization placing a priority on accurate results of uranium analyses, or on the confirmation of trace uranium in environmental samples, has a vested interest in preserving this material. This paper describes the need for high-purity 233U, the consequences organizations and agencies face if this material is not preserved, and the progress and future plans for preserving select batches of the purest 233U materials from disposition. This work is supported by the Next Generation Safeguards Initiative, Office of Nonproliferation and International Security, National Nuclear Security Administration.

  14. 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..

  15. Investigation of the effects of pressure on the compaction and subsequent sintering of nanosize powders. Final report

    SciTech Connect

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

    1996-02-26

    With current technology and available raw materials, one knows that it is very difficult, if not impossible, to produce a monolithic ceramic material with an average grain size of less than 100 nm. The grains of ceramic materials cannot be refined by cold working as is typically done in metals. Hence, the starting ceramic powder must be of a smaller or similar particle size as the desired grain size for the final product. The availability of nanosize (<100 nm) ceramic powders, however, is limited. In many cases, the powders consist of polymorphic mixtures, precursors, or amorphous phases of the desired material. Phase transformation during sintering is difficult to control, and when it does occur it usually is accompanied by significant microstructural changes and grain growth. An example of such a powder is Al{sub 2}O{sub 3}. To the best of the authors` knowledge, high purity nanosize {alpha}-Al{sub 2}O{sub 3} powder is unavailable commercially. However, a variety of nanosize transitional forms of Al{sub 2}O{sub 3}, including the {gamma} and {delta} polymorphs, are commercially available in large quantities as mixtures. Results on the compaction and sintering of nanosize {gamma}-Al{sub 2}O{sub 3} powder are reported here.

  16. Persistent luminescence in powdered and ceramic polycrystalline Gd3Al2Ga3O12:Ce

    NASA Astrophysics Data System (ADS)

    Dosovitskiy, G.; Fedorov, A.; Mechinsky, V.; Borisevich, A.; Dosovitskiy, A.; Tret’jak, E.; Korjik, M.

    2017-02-01

    This paper studies powders of Gd3Ga3Al2O12:Ce, a promising scintillator composition, as a possible object for express pre-characterization of scintillation kinetics and level of persistent luminescence. Garnet phase powders with uniform microstructure, consisting of 1-2 μm grains, were obtained by co-precipitation approach. It was shown, that both scintillation decay time and presence of persistent luminescence are influenced by both powder thermal treatment temperature and strong Ga deficit.

  17. Mechanical and tribological behavior of red clay ceramic tiles coated with fly ash powders by thermal spraying technique.

    NASA Astrophysics Data System (ADS)

    Peña-Rodríguez, G.; Dulce-Moreno, H.; Daza-Ramírez, J.; Orozco-Hernández, S.; Vargas-Galvis, F.

    2017-01-01

    The mechanical and tribological performance of red clay ceramic tiles uncoated and coated by oxy-fuel thermal spraying process from fly ash powders was evaluated. The ceramic tile substrates were manufactured by uniaxial pressing at 26.17 bar pressure, and sintered at 1100 °C. The coating thickness was determined based on the number of projection-cycles oxyacetylene flame over substrate. Coal fly ash coatings were deposited, with average thickness of 56.18±12.18 μm, 180.42±20.32 μm, and 258.26±25.88μm. The mechanical resistance to bending and wear by abrasion deep, were studied using ISO 10545-4 standards and ISO 10545-6 respectively; adhesion was measured using Elcometer equipment Type III according to ASTM D-4541-02 and the average roughness (Ra) was found according to ASTM standard D7127-13, using the profilometer Mitutoyo SJ 201. The surface morphology presented the heterogeneous molten or semi molten splats with average size of 35.262±3.48 micrometers with good adhesion, justifying increased mechanical resistance to bending by 5%, as well as wear by abrasion deep. These results contribute to the development of ceramic products with added value, to be used in various technological applications.

  18. 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.

  19. 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.

  20. 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.

  1. 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.

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. Synthesis of Li 2TiO 3 ceramic breeder powders by the combustion process

    NASA Astrophysics Data System (ADS)

    Jung, C. H.; Park, J. Y.; Oh, S. J.; Park, H. K.; Kim, Y. S.; Kim, D. K.; Kim, J. H.

    1998-03-01

    The synthesis of the ultra-fine Li 2TiO 3 powder by the combustion reaction of lithium nitrate, titanium nitrate and specific fuels was investigated. Ultrafine Li 2TiO 3 powders could be synthesized using glycine or a mixture of urea and citric acid. A pure Li 2TiO 3 phase was obtained by the simple process without further calcination reaction. The specific surface area of the as-synthesized powder was 10 to 14 m 2/g and the primary particle size was about 30 nm. The Li 2TiO 3 body sintered at 800°C for 3 h had dense agglomerates which were formed by the inter-agglomerate sintering process. Each of the agglomerates consisted of very fine grains with a size of 0.3 to 0.5 μm.

  8. 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.

  9. 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.

  10. 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.

  11. Radiotracer study of the preparation of high-purity lanthanum fluoride

    SciTech Connect

    Ewing, K.J.; Jaganathan, J.; Peitersen, L.; Aggarwal, I.D. ); Sommers, J.A.; Fahey, J.V. )

    1992-06-01

    This paper reports that the behavior of the impurities iron, cobalt, yttrium, and cerium is determined via radiotracer techniques for the preparation of high-purity lanthanum fluoride. The behavior of nickel and copper during the coprecipitation of a lanthanum nitrate solution is determined by graphite furnace atomic absorption spectrometric (GFAAS) analysis. There is no commercially available radiotracer for neodymium, a key impurity associated with absorption losses in fluoride glasses. However, the chemical behavior of neodymium and that of yttrium are very similar and, therefore, it is reasonable to assume that the behavior of yttrium throughout the processing is indicative of the behavior of neodymium. The concentrations of impurities in lanthanum nitrate, carbonate, and fluoride are estimated using the radiotracer and GFAAS data for each processing step. Results indicate that while high-purity lanthanum carbonate can be prepared, any impurities present in the lanthanum carbonate will be carried quantitatively into lanthanum fluoride upon hydrofluorination.

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

    PubMed

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

    2011-09-21

    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 axes. 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.

  13. 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.

  14. [Simultaneously preparation of grams of high purity tyrosol, crenulatin and salidroside from Rhodiola crenulata].

    PubMed

    Luo, Xin; Wang, Xue-jing; Li, Shi-ping; Zhang, Qiao; Zhao, Yi-wu; Huang Wen-zhe; Wang, Zhen-zhong; Xiao, Wei

    2015-04-01

    Tyrosol, crenulatin and salidroside are the main active constituents of Rhodiola crenulata, with extensive pharmacological activities. In the study, grams of high purity tyrosol, crenulatin and salidroside were simultaneously separated from R. crenulata by the first time. Firstly, R. crenulata was extracted by 70% alcohol. Then, with the yields of three compounds as the index, the macroporous resin was optimized. At last, grams of high purity tyrosol, crenulatin and salidroside were isolated by D-101 macroporousresin, purified by column chromatography. Detected by HPLC, the purity of three compounds were higher than 98%. This method has the advantages of simple process and operation, less dosage of organic solvent, highly yield and reproducibility, suitable for the simultaneously preparation of tyrosol, crenulatin and salidroside.

  15. 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

  16. 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.

  17. Diels-Alder reactions as an efficient route to high purity cyclic polymers.

    PubMed

    Glassner, Mathias; Blinco, James P; Barner-Kowollik, Christopher

    2011-05-18

    A simple and efficient route for the synthesis of cyclic polymer systems is presented. Linear furan protected α-maleimide-ω-cyclopentadienyl functionalized precursors (poly(methyl methacrylate) and poly(tert-butyl acrylate)) were synthesized via atom transfer radical polymerization (ATRP) and subsequent substitution of the bromine end-group with cyclopentadiene. Upon heating at high dilution, deprotection of the dieneophile occurs followed by an intramolecular Diels-Alder reaction yielding a high purity cyclic product.

  18. 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.

  19. Simple HPLC method for detection of trace ephedrine and pseudoephedrine in high-purity methamphetamine.

    PubMed

    Makino, Yukiko

    2012-03-01

    A simple and sensitive HPLC technique was developed for the qualitative determination of ephedrine and pseudoephedrine (ephedrines), used as precursors of clandestine d-methamphetamine hydrochloride of high purity. Good separation of ephedrines from bulk d-methamphetamine was achieved, without any extraction or derivatization procedure on a CAPCELLPACK C18 MGII (250 × 4.6 mm) column. The mobile phase consisted of 50 mM KH2 PO4-acetonitrile (94:6 v/v %) using an isocratic pump system within 20 min for detecting two analytes. One run took about 50 min as it was necessary to wash out overloaded methamphetamine for column conditioning. The analytes were detected by UV absorbance measurement at 210 nm. A sample (20 mg) was simply dissolved in 1 mL of water, and a 50 μL aliquot of the solution was injected into the HPLC. The detection limits for ephedrine and pseudoephedrine in bulk d-methamphetamine were as low as 3 ppm each. This analytical separation technique made it possible to detect ephedrine and/or pseudoephedrine in seven samples of high-purity d-methamphetamine hydrochloride seized in Japan. The presence of trace ephedrines in illicit methamphetamine may strongly indicate a synthetic route via ephedrine in methamphetamine profiling. This method is simple and sensitive, requiring only commonly available equipment, and should be useful for high-purity methamphetamine profiling.

  20. Effect of Coprecipitation Parameters on Powder Characteristics and on Densification of PZT Ceramics.

    DTIC Science & Technology

    1982-09-01

    34* diffraction using a Phillips Norelco Diffractometer with filtered Ni K radiati-n. The powders were also subjected to DTA and TGA analysis using... TGA analysis showed the first two peaks to be associated with weight loss, the maximum loss occurring near 300oC. From Fig. 4a it is evident that I0

  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. Development ceramic composites based on Al2O3, SiO2 and IG-017 additive

    NASA Astrophysics Data System (ADS)

    Kurovics, E.; Shmakova, A.; Kanev, B.; Gömze, L. A.

    2017-02-01

    Based on high purity alumina and quartz powders and IG-017 bio-original additives the authors have developed new ceramic composite materials for different industrial purposes. The main goal was to fine a material and morphological structures of high performance ceramic composites as frames for development complex materials for extreme consumptions in the future. For this the mixed powders of Al2O3 , SiO2 and IG-017 bio-original additive were uniaxially pressed at different compaction pressures into disc shapes and were sintered in electric kiln under air (1) and nitrogrn (2) atmosphere. The grain size distributions of the raw materials were determined by laser granulometry. There thermo-physical properties were also determined by derivatography. The prepared and sintered specimens were tested on geometrical sizes, microstructure and morphology by scanning electron microscopy, porosity and water absorption. In this work the authors present the results of their research and investigation.

  3. Effect of Powder Characteristics on Microstructure and Properties in Alkoxide Prepared PZT Ceramics.

    DTIC Science & Technology

    1984-12-01

    Gel Processing of Thin Dielectric Films From Col loid Precursors; 2) Effect of Al 20 on Strength of Sintered ZrO2 ; * 3) Processing and Synthesis...Effect of pH of precipitating solution on the pressed and fired densities (9500 C/ h) of PZT (+ 0.25 wt% V2o5 ). * Figure 12. Plot of dielectric... Films by RF Sputtering for Memory Applications," M.S. Thesis, University of Illinois, Department of Ceramic Engineering, Urbana, IL, 1984. I. D. E

  4. Piezoelectric Properties of CuO-Doped (K,Na)NbO3 Lead-Free Ceramics Synthesized with Hydrothermal Powders

    NASA Astrophysics Data System (ADS)

    Yokouchi, Yuriko; Maeda, Takafumi; Bornmann, Peter; Hemsel, Tobias; Morita, Takeshi

    2013-07-01

    We report the piezoelectric properties of CuO-doped hydrothermal (K,Na)NbO3 ceramics that can be applied as hard-type lead-free piezoelectric ceramics. To date, we have succeeded in synthesizing high-quality KNbO3 and NaNbO3 powders by the hydrothermal method, which is based on an ionic reaction at high temperature (around 210 °C) and pressure. Increasing both the piezoelectric constant d and the mechanical quality factor (Qm) is important for resonance-type piezoelectric devices, such as ultrasonic motors and transformers. CuO doping into hydrothermal (K,Na)NbO3 ceramics was examined to realize hard-type lead-free piezoelectric ceramics. By doping with 1.2 mol % CuO, Qm was increased and the dielectric loss (tan δ) was decreased to 0.5%. The grain size was also influenced by the amount of CuO doping, which indicates that Qm is related to the density. To achieve a higher Qm value, the grain size is required to be less than 5 µm however, excessive CuO doping leads to anomalous grain growth. Optimal piezoelectric properties were obtained for 1.2 mol % CuO-doped (K,Na)NbO3; k31 = 0.32, d31 = -44 pC/N, Qm (radial) = 959, and tan δ= 0.5%. These characteristics showed that CuO doping with hydrothermal powders is effective for obtaining hard-type ceramics, and the mechanical quality factor is more than ten times higher than that of nondoped hydrothermal (K,Na)NbO3 ceramics. Therefore, compared with the conventional solid-state method, we could succeed in obtaining hard-type ceramics by a simple and short process.

  5. A controllable vibratory calciner for processing high-temperature superconductors and other ceramic powders

    NASA Astrophysics Data System (ADS)

    Spencer, Nicholas D.; Beeckman, Jean W.; Peders, Thorvald S.; Cameron, Craig P.

    1990-05-01

    A novel vibratory calcination apparatus is described, that enables reactant powders to be heated at or above their sintering temperatures without excessive agglomeration. In addition, the vibration-induced fluidization leads to greatly improved gas-solid contact, which can significantly speed up reactions that are limited by the ingress or egress of gases. Unlike its gas-fluidized counterpart, the vibratory calciner does not lead to excessive loss of fines. Vibration is generated by means of a function generator-amplifier-loudspeaker voice coil system, which allows amplitude, frequency, and time dependence of frequency to be precisely controlled. The system has been used extensively in the laboratory for the calcination of high-temperature superconducting powders, where its use has led to greatly reduced calcination times and a much lower degree of agglomeration in the finished material.

  6. Photocatalytic Activity of LaSr2 AlO5 :Eu Ceramic Powders.

    PubMed

    García, Carlos R; Oliva, Jorge; Díaz-Torres, Luis A

    2015-01-01

    The photocatalytic activity, of undoped and Europium-doped LaSr2 AlO5 powders, has been investigated by degrading methylene blue dye in water solutions. Those powders were fabricated by a combustion method and an annealing treatment in air. All samples showed a tetragonal single phase according to by X-ray diffraction measurements (XRD). Scanning electron microscopy (SEM) revealed irregular semi-oval grains with sizes in the range of 3.5-4.27 μm. Photoluminescence spectrum showed sharp emission peaks at 588 nm and at 617 nm which are associated with (7) F1 ,(7) F2 → (5) D0 Eu(3+) ion forbidden transitions, respectively, under UV light excitation of 322 nm. The methylene blue (MB) degradation under UV light (254 nm) was studied by monitoring changes in the absorbance peak of MB at 665 nm. Finally, LaSr2 AlO5 :Eu powders were used three times and the efficiency for the degradation of MB decreased from 100 to 61% after the third cycle of use.

  7. 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.

  8. 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.

  9. Toxicology and occupational hazards of new materials and processes in metal surface treatment, powder metallurgy, technical ceramics, and fiber-reinforced plastics.

    PubMed

    Midtgård, U; Jelnes, J E

    1991-12-01

    Many new materials and processes are about to find their way from the research laboratory into industry. The present paper describes some of these processes and provides an overview of possible occupational hazards and a list of chemicals used or produced in the processes. The technological areas that are considered are metal surface treatment (ion implantation, physical and chemical vapor deposition, plasma spraying), powder metallurgy, advanced technical ceramics, and fiber-reinforced plastics.

  10. Understanding Friction and Wear Mechanisms of High-Purity Titanium against Steel in Liquid Nitrogen Temperature

    NASA Astrophysics Data System (ADS)

    Basu, Bikramjit; Sarkar, J.; Mishra, Ravi

    2009-02-01

    Although the friction and wear properties of several metallic alloys in unlubricated conditions are widely investigated, such understanding for high-purity metals in cryogenic environment is rather limited. This article reports the tribological properties of high-purity α-titanium ( α-Ti), prepared by cold rolling and recrystallization annealing, under liquid nitrogen (LN2) and room temperature (RT) environments against steel (bearing grade: SAE 52100) at varying loads (up to 15 N) and sliding speeds (0.6 to 4.19 m/s). It has been found that the steady-state coefficient of friction (COF) of titanium under LN2 environment (˜0.27 to 0.33) is lower than that at RT COF (˜0.33 to 0.58) irrespective of sliding speed. For cryogenic sliding conditions, the COF decreased steadily with sliding speed to a mean value of about 0.28 and no appreciable variation in COF is noticed for sliding speed of more than 1.5 m/s. The wear rate under both environment conditions was of the order of 10-3 mm3 N-1 m-1 irrespective of variation in operating parameters, but the RT wear rate was found to be higher compared to the LN2 case. Overall, the experimental results demonstrate improved tribological properties of high-purity titanium at LN2 temperature compared to the RT. Flow localization at tribological interfaces because of the large strain rate and subsequent damage accumulation at the titanium test piece are some of the attributes of the wear of Ti at LN2 temperature. In addition, the galling of titanium was also observed to occur under large contact stress and sliding speed conditions.

  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. Homogeneity of ball milled ceramic powders: Effect of jar shape and milling conditions.

    PubMed

    Broseghini, M; D'Incau, M; Gelisio, L; Pugno, N M; Scardi, P

    2017-02-01

    This paper contains data and supporting information of and complementary to the research article entitled "Effect of jar shape on high-energy planetary ball milling efficiency: simulations and experiments" (Broseghini et al.,) [1]. Calcium fluoride (CaF2) was ground using two jars of different shape (cylindrical and half-moon) installed on a planetary ball-mill, exploring different operating conditions (jar-to-plate angular velocity ratio and milling time). Scanning Electron Microscopy (SEM) images and X-Ray Powder Diffraction data (XRPD) were collected to assess the effect of milling conditions on the end-product crystallite size. Due to the inhomogeneity of the end product, the Whole Powder Pattern Model (WPPM, (Scardi, 2008) [2]) analysis of XRPD data required the hypothesis of a bimodal distribution of sizes - respectively ground (fine fraction) and less-to-not ground (coarse fraction) - confirmed by SEM images and suggested by the previous literature (Abdellatief et al., 2013) [3,4]. Predominance of fine fraction clearly indicates optimal milling conditions.

  13. Compensation Mechanism in High Purity Semi-Insulating 4H-SiC

    DTIC Science & Technology

    2007-01-01

    online 15 March 2007 A study of deep levels in high purity semi-insulating 4H-SiC has been made using temperature dependent Hall effect TDH , thermal and...optical admittance spectroscopies, and secondary ion mass spectrometry SIMS. Thermal activation energies from TDH varied from a low of 0.55 eV to a...high of 1.65 eV. All samples studied showed n-type conduction with the Fermi level in the upper half of the band gap. Fits of the TDH data to

  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. High-precision efficiency calibration of a high-purity co-axial germanium detector

    NASA Astrophysics Data System (ADS)

    Blank, B.; Souin, J.; Ascher, P.; Audirac, L.; Canchel, G.; Gerbaux, M.; Grévy, S.; Giovinazzo, J.; Guérin, H.; Nieto, T. Kurtukian; Matea, I.; Bouzomita, H.; Delahaye, P.; Grinyer, G. F.; Thomas, J. C.

    2015-03-01

    A high-purity co-axial germanium detector has been calibrated in efficiency to a precision of about 0.15% over a wide energy range. High-precision scans of the detector crystal and γ-ray source measurements have been compared to Monte-Carlo simulations to adjust the dimensions of a detector model. For this purpose, standard calibration sources and short-lived online sources have been used. The resulting efficiency calibration reaches the precision needed e.g. for branching ratio measurements of super-allowed β decays for tests of the weak-interaction standard model.

  16. High-purity cobalt thin films with perpendicular magnetic anisotropy prepared by chemical vapor deposition

    NASA Astrophysics Data System (ADS)

    Ootera, Yasuaki; Shimada, Takuya; Kado, Masaki; Quinsat, Michael; Morise, Hirofumi; Nakamura, Shiho; Kondo, Tsuyoshi

    2015-11-01

    A study of the chemical vapor deposition (CVD) of high-purity cobalt thin films is described. The Co layer prepared by a thermal CVD technique with a Pt/Ta underlayer and a Pt cap layer shows a saturation magnetization (Ms) of ∼1.8 T and perpendicular magnetic anisotropy (PMA) with an anisotropy energy (Ku) of ∼105 J/m3. The cobalt thickness dependence of Ku reveals that the interfacial anisotropy at the Pt/Co interface is most likely the origin of the obtained PMA.

  17. 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.

  18. 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.

  19. 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.

  20. 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.

  1. 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.

  2. Streamer knotwilg branching: sudden transition in morphology of positive streamers in high-purity nitrogen

    NASA Astrophysics Data System (ADS)

    Heijmans, L. C. J.; Clevis, T. T. J.; Nijdam, S.; van Veldhuizen, E. M.; Ebert, U.

    2015-09-01

    We describe a peculiar branching phenomenon in positive repetitive streamer discharges in high purity nitrogen. We name it knotwilg branching after the Dutch word for a pollard willow tree. In a knotwilg branching a thick streamer suddenly splits into many thin streamers. Under some conditions this happens for all streamers in a discharge at about the same distance from the high-voltage electrode tip. At this distance, the thick streamers suddenly bend sharply and appear to propagate over a virtual surface surrounding the high-voltage electrode, rather than following the background electric field lines. From these bent thick streamers many, much thinner, streamers emerge that roughly follow the background electric field lines, creating the characteristic knotwilg branching. We have only found this particular morphology in high purity nitrogen at pressures in the range 50 to 200 mbar and for pulse repetition rates above 1 Hz; the experiments were performed for an electrode distance of 16 cm and for fast voltage pulses of 20 or 30 kV. These observations clearly disagree with common knowledge on streamer propagation. We have analyzed the data of several tens of thousands of discharges to clarify the phenomena. We also present some thoughts on how the ionization of the previous discharges could concentrate into some pre-ionization region near the needle electrode and create the knotwilg morphology, but we present no final explanation.

  3. Recovery of high purity sulfuric acid from the waste acid in toluene nitration process by rectification.

    PubMed

    Song, Kai; Meng, Qingqiang; Shu, Fan; Ye, Zhengfang

    2013-01-01

    Waste sulfuric acid is a byproduct generated from numerous industrial chemical processes. It is essential to remove the impurities and recover the sulfuric acid from the waste acid. In this study the rectification method was introduced to recover high purity sulfuric acid from the waste acid generated in toluene nitration process by using rectification column. The waste acid quality before and after rectification were evaluated using UV-Vis spectroscopy, GC/MS, HPLC and other physical and chemical analysis. It was shown that five nitro aromatic compounds in the waste acid were substantially removed and high purity sulfuric acid was also recovered in the rectification process at the same time. The COD was removed by 94% and the chrominance was reduced from 1000° to 1°. The recovered sulfuric acid with the concentration reaching 98.2 wt% had a comparable quality with commercial sulfuric acid and could be recycled back into the toluene nitration process, which could avoid waste of resources and reduce the environmental impact and pollution.

  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. Photoconductive response of compensating impurities in photothermal ionization spectroscopy of high-purity silicon and germanium

    SciTech Connect

    Darken, L.S.; Hyder, S.A.

    1983-04-15

    In photothermal ionization spectroscopy both positive and negative photoconductivity responses have been reported from compensating centers neutralized by minority carriers generated by band-edge light. Here, the response of compensating impurities in both n-type and p-type high-purity (Vertical BarN/sub A/-N/sub D/Vertical Bar roughly-equal10/sup 10/--10/sup 12/ cm/sup -3/) nuclear-detector-grade silicon and germanium is reported. Negative photoconductive responses from compensating impurities were observed only when the distance the photothermally generated majority carriers traveled before recapture by shallow levels was longer than the sample length (contact to contact). We propose that in high-purity semiconductors, such as used in this study, it is the contact configuration that is responsible for the apparent rapid recombination of minority carriers which causes negative minority-carrier photoconductivity. n/sup +/nn/sup +/ or p/sup +/pp/sup +/ structures allow multiple traversals through the sample by only majority carriers. The dependence of the band-edge light generated excess carrier density on applied electric field supports this mechanism.

  6. 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.

  7. 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.

  8. 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.

  9. Solution and slurry sampling electrothermal atomic absorption spectrometry for the analysis of high purity quartz

    NASA Astrophysics Data System (ADS)

    Hauptkorn, Susanne; Krivan, Viliam

    1996-07-01

    A slurry sampling electrothermal atomic absorption spectrometry (ETAAS) method for the determination of Al, Cr, Cu, Fe, K, Li, Mg, Mn and Na at trace and ultratrace level in high purity quartz samples has been developed. The influence of atomization temperature, internal gas flow during atomization and carbide modification of the graphite tube on the background absorption has been studied. Simple quantification via calibration curves, recorded with aqueous standards, is possible for all elements except Al. The performance and the accuracy of the slurry sampling technique are compared to those of the analysis of hydrofluoric acid digests. With both methods, the blanks could be substantially reduced by minimization of sample handling. Because of essentially higher applicable sample portions, the solution technique provides lower limits of detection for all elements excluding Al, Na and K. For the slurry sampling technique, the achievable limits of detection are in the range of 2 (Mg) to 500 (Fe) ng g -1 and for the solution technique, they are between 0.4 (Mg) and 500 (Al) ng g -1. Thus, both developed methods are well suited for ultratrace analysis of high purity quartz for microelectronic applications. The results obtained by these two ETAAS techniques are compared with those of independent methods including neutron activation analysis.

  10. Efficient purification of high-purity compounds from the stem of Lonicera japonica Thunb using two-dimensional preparative chromatography.

    PubMed

    Jin, Hongli; Liu, Yanfang; Feng, Jiatao; Guo, Zhimou; Wang, Chaoran; Zhong, Zhengsheng; Peng, Xiaojun; Dang, Jun; Tao, Yanduo; Liang, Xinmiao

    2013-08-01

    Purification of high-purity compounds from traditional Chinese medicines (TCMs) plays an important role in investigating their bioactivity. Nevertheless, it is often quite difficult to isolate compounds with high purity because of the complexity of TCMs in chemical composition. In this work, a two-dimensional preparation method was successfully developed for the preparation of high-purity compounds from the stem of Lonicera japonica Thunb, based on two novel polar copolymerized RP stationary phases, XAqua C3 and XAqua C18. An XAqua C3 prep column was used to separate the sample in the first-dimensional preparation, and 14 g of sample was fractionated into eight fractions with a recovery of 82%. An XAqua C18 prep column was selected to prepare high-purity compounds in the second-dimensional preparation for its good orthogonality with the XAqua C3 stationary phase. As a result, major compounds in the sample were isolated with more than 99% purity. This method is a potent method to realize the efficient purification of compounds with high purity from the stem of L. japonica Thunb and it shows great potential in the separation of high-purity compounds from complex samples.

  11. Solid state synthesis and thermal stability of HAP and HAP - beta-TCP composite ceramic powders.

    PubMed

    Rao, R R; Roopa, H N; Kannan, T S

    1997-08-01

    Powders of pure beta-tricalcium phosphate (beta-TCP), hydroxyapatite (HAP) and a biphasic composite mixture of HAP+beta-TCP were prepared by solid state reaction between two commercially available calcium-based precursors namely, tricalcium phosphate (TCP) and calcium hydroxide (Ca(OH)2). These reactants mixed in the molar ratios ranging from 3 : 0 to 3 : 4 (designated T0 to T4) in deionized water, milled and slip-cast into discs were heat treated in the temperature range of 600 degrees C to 1250 degrees C. The products formed were characterized by X-ray diffraction (XRD) and i.r. spectroscopic techniques for identification of phases formed and functional groups present in them. While tricalcium phosphate and calcium hydroxide taken in the molar ratio of 3 : 2 and 3 : 3 resulted in pure HAP when heat treated at 1000 degrees C for 8 h, the 3 : 1 and 3 : 1.5 molar ratio compositions resulted in a biphasic mixture of HAP+beta-TCP for similar heat treatments. Heat treatment of 3 : 4 molar ratio composition of tricalcium phosphate and calcium hydroxide at 1000 degrees C yielded HAP with free CaO as the secondary phase. Products of heat treatment at higher temperatures (1150 and 1250 degrees C) for even shorter duration (2 h) while not differing from the products obtained from T0 and T2 cases at 1000 degrees C (pure beta-TCP and pure HAP), change in the case of T1, T1.5, T3 and T4 to products with lesser percentages of HAP containing beta-TCP (in the case of T1 and T1.5) or CaO (in the case of T3 and T4) as the secondary phase.

  12. 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

  13. 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.

  14. Annealing Behavior at Triple Junctions in High-Purity Aluminum After Slight Cold Rolling

    NASA Astrophysics Data System (ADS)

    Yin, Wenhong; Wang, Weiguo; Fang, Xiaoying; Qin, Congxiang

    2017-02-01

    High-purity polycrystalline aluminum samples with a typical grain size of approximately 30 μm were slightly cold-rolled with a thickness reduction of 15%, and then, off-line in situ electron backscatter diffraction was used to identify the annealing behavior at triple junctions during annealing at 400 °C. The results show that recrystallization nuclei are developed at some triple junctions during annealing. High-angle grain boundaries migrate from harder grains to softer grains at the triple junctions leading to the formation of nuclei. All such nuclei show Σ3 orientation relationships with the parent grains, and the bounded Σ3 boundaries are found to be incoherent. During further annealing, these nuclei are consumed by other growing grains, indicating that their presence is just a release of the strain concentration at the triple junctions.

  15. 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.

  16. 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

    2017-02-01

    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.

  17. Efficient single photon emission from a high-purity hexagonal boron nitride crystal

    NASA Astrophysics Data System (ADS)

    Martínez, L. J.; Pelini, T.; Waselowski, V.; Maze, J. R.; Gil, B.; Cassabois, G.; Jacques, V.

    2016-09-01

    Among a variety of layered materials used as building blocks in van der Waals heterostructures, hexagonal boron nitride (hBN) appears as an ideal platform for hosting optically active defects owing to its large band gap (˜6 eV ). Here we study the optical response of a high-purity hBN crystal under green laser illumination. By means of photon correlation measurements, we identify individual defects emitting a highly photostable fluorescence under ambient conditions. A detailed analysis of the photophysical properties reveals a high quantum efficiency of the radiative transition, leading to a single photon source with very high brightness (˜4 ×106 counts s-1). These results illustrate how the wide range of applications offered by hBN could be further extended to photonic-based quantum information science and metrology.

  18. Nodular graphite formation in vacuum melted high purity Fe-C-Si alloys

    NASA Astrophysics Data System (ADS)

    Dhindaw, B.; Verhoeven, J. D.

    1980-06-01

    This paper describes a study of the cast structure of vacuum melted high purity Fe-C-Si alloys with emphasis on hypoeutectic and eutectic compositions. Nodular graphite was observed to form at high cooling rates and coral graphite at low cooling rates. This result was also confirmed by a limited study on directional solidification of alloys prepared from the same starting materials. The formation of nodular graphite at the high cooling rates was suppressed to near zero by changing the starting iron from 99.94 pct electrolytic iron to an ultra-pure zone refined iron, or by holding the melt at a low super-heat prior to cooling. Chemical analysis showed only that the impurity responsible for nodular formation was present at the low ppm level. An attempt is made to explain the appearance of the various microstructures in terms of the nucleation and growth of nodular graphite, coral graphite and the carbide structure of white iron.

  19. 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.

  20. 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.

  1. High-purity InAs1-xSbx epilayer grown by a LPE technique

    NASA Astrophysics Data System (ADS)

    Lv, Y. F.; Hu, S. H.; Xu, Y. G.; Zhou, W.; Wang, Y.; Wang, R.; Yu, G. L.; Dai, N.

    2015-04-01

    High-purity InAs1-xSbx films with x=0.06 were successfully grown on InAs (100) substrates by liquid phase epitaxy (LPE). Procedures were applied to purify InAs1-xSbx precursor material, which included prolonging baking time in hydrogen and adding rare-earth element gadolinium (Gd) to the growth melt. Electrical transport properties of InAs1-xSbx film were investigated by Hall measurements in the condition of the conductive InAs substrate being removed completely by chemical mechanical polishing (CMP) to eliminate its influence on the measurements. Hall measurement results show carrier concentration and mobility of our InAs1-xSbx samples are superior to the other reported values when a combinational purification procedure is applied.

  2. Detection of moisture content in high-purity ammonia by means of diode-laser spectroscopy

    NASA Astrophysics Data System (ADS)

    Berezin, A. G.; Nadezhdinskii, A. I.; Ponurovskii, Y. Y.; Stavrovskii, D. B.; Vyazov, I. E.; Kotkov, A. P.; Ivanov, V. A.; Grishnova, N. D.; Polezhaev, D. M.; Sidorov, V. A.; Kotkov, D. A.

    2008-02-01

    The aim of this work was the development of an as-simple-as-possible instrument for trace moisture concentration measurements in high-purity ammonia. A near-infrared diode-laser-based instrument has been applied to measure the humidity in a process of on-line detection of water in ammonia during industrial purification. The results of water concentration measurements were compared with alternative techniques (primarily dew-point detection) and good agreement was achieved. The long-term sensitivity of such a diode-laser-based instrument was estimated to be 5 ppm. The calculation of the water concentration from measurements of the integrated volume of water contained in the heavy fraction, extracted during the purification process, yields an even lower detection limit of less than 0.1 ppm, depending on the initial ammonia purity.

  3. Statistics of high purity nickel microstructure from high energy x-ray diffraction microscopy.

    SciTech Connect

    Hefferan, C. M.; Li, S. F.; Lind, J. F.; Lienert, U.; Rollett, A. D.; Winblatt, P.; Suter, R. M.; X-Ray Science Division; Univ. of Pittsburgh; Carnegie Mellon Univ.

    2009-01-01

    We have measured and reconstructed via forward modeling a small volume of microstructure of high purity, well annealed nickel using high energy xray diffraction microscopy (HEDM). Statistical distributions characterizing grain orientations, intra-granular misorientations, and nearest neighbor grain misorientations are extracted. Results are consistent with recent electron backscatter diffraction measurements. Peaks in the grain neighbor misorientation angle distribution at 60 degrees (S3) and 39 degrees (S9) have resolution limited widths of {approx}0:14 degree FWHM. The analysis demonstrates that HEDM can recover grain and grain boundary statistics comparable to OIM volume measurements; more extensive data sets will lead to full, five parameter grain boundary character distributions. Due to its non-destructive nature, HEDM can then watch, both statistically and through tracking of individual grains and boundaries, the evolution of such distributions with processing of the sample.

  4. 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.

  5. Role of deformation twins in static recrystallization kinetics of high-purity alpha titanium

    NASA Astrophysics Data System (ADS)

    Won, Jong Woo; Lee, Taekyung; Hong, Seong-Gu; Lee, Yongmoon; Lee, Jeong Hun; Lee, Chong Soo

    2016-11-01

    The importance of deformation twins in static recrystallization kinetics of high-purity alpha titanium was investigated by carrying out thermal annealing tests of deformed materials in combination with electron-backscatterdiffraction- based microstructural analysis. Prior to thermal annealing, the material was compressed to a true strain of 0.22 along three directions to introduce different twinning characteristics. Our results showed that deformation twins substantially promoted the static recrystallization process by deepening the microstructural inhomogeneity induced by the formation of twin boundaries and twinning-induced crystallographic lattice reorientation. Twin morphology was also observed to be important because it influenced the extent of microstructural inhomogeneity. Intersecting twin morphology, caused by the activation of multiple twin variants, was more effective than parallel twin morphology, caused by the activation of a single twin variant (or a twin variant pair), because it gave rise to more twin boundaries, more twin boundary junctions (intersections, triple junctions, etc.), and greater in-grain crystallographic orientation spread.

  6. 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.

  7. 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.

  8. Defects interaction processes in deformed high purity polycrystalline molybdenum at elevated temperatures

    NASA Astrophysics Data System (ADS)

    Lambri, O. A.; Bonifacich, F. G.; Bozzano, P. B.; Zelada, G. I.; Plazaola, F.; García, J. A.

    2014-10-01

    Mechanical spectroscopy (damping and elastic modulus as a function of temperature) and transmission electron microscopy studies have been performed in high purity polycrystalline molybdenum plastically deformed to different values of tensile and torsion strain. Mechanical spectroscopy measurements were performed from room temperature up to 1285 K. A relaxation peak in polycrystalline molybdenum related to the movement of dislocations into lower energy configurations near grain boundaries has been discovered to appear around 1170 K. The activation energy of the peak is 4.2 eV ± 0.5 eV. This relaxation phenomenon involves the interaction between vacancies and mobile dislocations near the grain boundaries. It should be highlighted that this relaxation process is controlled by the arrangement of vacancies and dislocations which occur at temperature below 1070 K.

  9. Scalable fabrication of high purity diamond nanocrystals with long-spin-coherence nitrogen vacancy centers.

    PubMed

    Trusheim, Matthew E; Li, Luozhou; Laraoui, Abdelghani; Chen, Edward H; Bakhru, Hassaram; Schröder, Tim; Gaathon, Ophir; Meriles, Carlos A; Englund, Dirk

    2014-01-08

    The combination of long spin coherence time and nanoscale size has made nitrogen vacancy (NV) centers in nanodiamonds the subject of much interest for quantum information and sensing applications. However, currently available high-pressure high-temperature (HPHT) nanodiamonds have a high concentration of paramagnetic impurities that limit their spin coherence time to the order of microseconds, less than 1% of that observed in bulk diamond. In this work, we use a porous metal mask and a reactive ion etching process to fabricate nanocrystals from high-purity chemical vapor deposition (CVD) diamond. We show that NV centers in these CVD nanodiamonds exhibit record-long spin coherence times in excess of 200 μs, enabling magnetic field sensitivities of 290 nT Hz(-1/2) with the spatial resolution characteristic of a 50 nm diameter probe.

  10. 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.

  11. Re-examination of creep behaviour of high purity aluminium at low temperature

    NASA Astrophysics Data System (ADS)

    Ueda, S.; Kameyama, T.; Matsunaga, T.; Kitazono, K.; Sato, E.

    2010-07-01

    The deformation behaviour of high-purity aluminium at low temperatures was investigated in order to re-examine Ashby-type deformation mechanism map. All specimens with different purities showed significant creep below room temperature. Under the same stress and temperature, the steady-state creep rate increased with increasing purity of the material. They showed stress exponents around 5.0 and apparent activation energies around 20 kJ/mol at temperatures below about 400 K, and 4.0 and 70-80 kJ/mol at temperatures above that temperature. The grain size had no effect in the low temperature region. From the microstructural observation, secondary slip system was observed. These features imply that pure aluminium deforms in the different mode from the ambient temperature creep of h.c.p. metals which has similar activation energy.

  12. 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.

  13. 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.

  14. 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).

  15. Magneto-Optical Study High-Purity Niobium for Superconducting RF Application

    NASA Astrophysics Data System (ADS)

    Polyanskii, A. A.; Lee, P. J.; Gurevich, A.; Sung, Zu-Hawn; Larbalestier, D. C.

    2011-03-01

    In this review we present a summary of our recent Magneto-Optical (MO) imaging of high-purity Nb for SRF cavity application. Superconducting RF cavities have been chosen as the accelerating technology for the International Linear Collider, and it is of vital importance to understand the limiting factors to the performance of these devices. We have been using a combination of MO, imaging, magnetization measurements and a variety of non-contact surface topology measurement techniques to characterize samples of high purity Nb supplied by Fermi National Accelerator Laboratory (FNAL) and Thomas Jefferson National Accelerator Facility (TJNAF). Localized non-uniformities in the superconducting properties were revealed on samples which were cut from rolled polycrystalline sheets (FNAL) and subjected to buffered chemical polishing (BCP) and heat treatments (HT) steps designed to simulate typical SRF cavity production. MO examination of the polycrystalline Nb sheets in perpendicular and in-plane fields reveals the perturbations in the critical currents caused by topological defects such as the steps between adjacent grains produced by BCP. MO examination of bi-crystals prepared from a disc cut directly from a very large grain size ingot (manufactured for TJNAF by CBMM) showed preferential flux penetration at grain boundaries for bi-crystal samples in which the GB interface was almost parallel to the externally applied field. This result was the first direct evidence of depressed superconductivity at GBs. By developing an understanding of how and why such behavior occurs, we hope to be able to improve the properties of cavity accelerators.

  16. 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.

  17. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2017-03-01

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

  19. 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.

  20. Powder XRD, SEM, and Multinuclear MAS-NMR Investigations of the Interactions Between Glass and Crystalline Phases of Li, Na, or K Ceramic Waste Forms

    SciTech Connect

    Lambregts, Marsha J.; Frank, Steve M.

    2005-08-01

    Interactions between the glass and crystalline phases of ceramic waste forms were investigated via powder X-ray diffraction, scanning electron microscopy, and Si-29, Al-27, Na-23, Li-7, and Cl-35 magic angle spinning nuclear magnetic resonance spectroscopy. LiCl, NaCl, or KCl waste form samples were made with or without glass. The waste forms containing glass consist of sodalite and glass phases with minor amounts of nepheline. Samples without glass form varying amounts of sodalite and nepheline. The glass frit, intended to bind the zeolite particles together, changes in composition, showing marked increases in aluminum and alkali content.

  1. 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.

  2. 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.

  3. Preparation & characterization of high purity Cu2 ZnSn(SxSe1-x)4 nanoparticles

    NASA Astrophysics Data System (ADS)

    Negash, Bethlehem G.

    Research in thin film solar cells applies novel techniques to synthesize cost effective and highly efficient absorber materials in order to generate electricity directly from solar energy. Of these materials, copper zinc tin sulfoselenide (Cu2ZnSn(SxSe1-x) 4) nanoparticles have shown great promise in solar cell applications due to optimal material properties as well as low cost & relative abundance of materials.1,2 Sulfoselenide nanoparticles have also a broader impact in other industries including electronics3, LED 4, and biomedical research5. Of the many routes of manufacturing these class of semiconductors, colloidal synthesis of Cu 2ZnSn(SxSe1-x)4 offers a scalable, low cost and high-throughput route for manufacturing high efficiency thin-film solar cells. Hydrazine processed Cu2ZnSn(SxSe1-x )4 devices have reached a record power conversion efficiency (PCE) of 12.6%, much higher than the 9.6% reported for physical vapor deposition (PVD) systems.6,7. Despite high efficiencies, wet synthesis of nanoparticles, however, is made more complicated in multi-element, quaternary and quinary systems such as copper zinc tin sulfoselenide (CZTSSe) and copper indium gallium diselenide (CIGSe). One major disadvantage in these systems is growth of the desired quaternary or quinary phase in competition with unwanted binary and ternary phases with low energy of formation.8,9 Moreover, various reaction parameters such as reaction time, temperature, and choice of ligand also affect, chemical as well as physical properties of resulting nanoparticles. Understanding of the formation mechanisms of the particles is necessary in order to address some of these challenges in wet synthesis of CZTSSe nanoparticles. In this study, we investigate synthesis conditions & reaction parameters which yield high purity Cu2ZnSn(SxSe1-x) 4 nanoparticles as well as attempt to understand the growth mechanism of these nanoparticles. This was achieved by manipulating anion precursor preparation routes as

  4. αTCP ceramic doped with dicalcium silicate for bone regeneration applications prepared by powder metallurgy method: in vitro and in vivo studies.

    PubMed

    Velasquez, Pablo; Luklinska, Zofia B; Meseguer-Olmo, Luis; Mate-Sanchez de Val, Jose E; Delgado-Ruiz, Rafael A; Calvo-Guirado, Jose L; Ramirez-Fernandez, Ma P; de Aza, Piedad N

    2013-07-01

    This study reports on the in vitro and in vivo behavior of α-tricalcium phosphate (αTCP) and also αTCP doped with either 1.5 or 3.0 wt % of dicalcium silicate (C2 S). The ceramics were successfully prepared by powder metallurgy method combined with homogenization and heat treatment procedures. All materials were composed of a single-phase, αTCP in the case of a pure material, or solid solution of C2 S in αTCP for the doped αTCP, which were stable at room temperature. The ceramics were tested for bioactivity in simulated body fluid, cell culture medium containing adult mesenchymal stem cells of human origin, and in animals. Analytical scanning electron microscopy combined with chemical elemental analysis was used and Fourier transform infrared and conventional histology methods. The in vivo behavior of the ceramics matched the in vitro results, independently of the C2 S content in αTCP. Carbonated hydroxyapatite (CHA) layer was formed on the surface and within the inner parts of the specimens in all cases. A fully mineralized new bone growing in direct contact with the implants was found under the in vivo conditions. The bioactivity and biocompatibility of the implants increased with the C2 S content in αTCP. The C2 S doped ceramics also favoured a phase transformation of αTCP into CHA, important for full implant integration during the natural bone healing processes. αTCP ceramic doped with 3.0 wt % C2 S showed the best bioactive in vitro and in vivo properties of all the compositions and hence could be of interest in specific applications for bone restorative purposes.

  5. Influence of short chain organic acids and bases on the wetting properties and surface energy of submicrometer ceramic powders.

    PubMed

    Neirinck, Bram; Soccol, Dimitri; Fransaer, Jan; Van der Biest, Omer; Vleugels, Jef

    2010-08-15

    The effect of short chained organic acids and bases on the surface energy and wetting properties of submicrometer alumina powder was assessed. The surface chemistry of treated powders was determined by means of Diffuse Reflectance Infrared Fourier Transform spectroscopy and compared to untreated powder. The wetting of powders was measured using a modified Washburn method, based on the use of precompacted powder samples. The geometric factor needed to calculate the contact angle was derived from measurements of the porous properties of the powder compacts. Contact angle measurements with several probe liquids before and after modification allowed a theoretical estimation of the surface energy based on the surface tension component theory. Trends in the surface energy components were linked to observations in infrared spectra. The results showed that the hydrophobic character of the precompacted powder depends on both the chain length and polar group of the modifying agent.

  6. 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.

  7. 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.

  8. Microstructure and helium irradiation performance of high purity tungsten processed by cold rolling

    NASA Astrophysics Data System (ADS)

    Chen, Zhe; Han, Wenjia; Yu, Jiangang; Kecskes, Laszlo; Zhu, Kaigui; Wei, Qiuming

    2016-10-01

    This work aims to investigate the effects of confined cold rolling on the evolution of microstructure, hardness, and helium irradiation performance of high purity tungsten (W). Using a final rolling temperature of 450 °C, W samples were severely deformed by confined cold rolling up to equivalent strains (εeq) of 1.6 and 3.3. Experimental results indicate that the average grain size of W specimens processed by confined cold rolling has been greatly reduced, and the rolled W samples with εeq ∼3.3 do not show an "ideal texture" of (001)[110] which is the expected texture of bcc metals processed by conventional cold rolling. The irradiation resistance against 60 keV He+ ions with up to a dose of 1.5 × 1022 ions·m-2 of the rolled W is compared to that of the as-received W. Results show that, due to an improvement of the metal's ductility, blister bursting with a partially opened lid forms on the surface of the rolled W, whereas blister bursting with a fully opened lid forms on the surface of the as-received W.

  9. 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.

  10. Influence of Ta content in high purity niobium on cavity performance: preliminary results

    SciTech Connect

    Carneiro, Tadeu; Klinkenberg, Christian; Kneisel, Peter; Myneni, Ganapati; Singer, Waldemar; Singer, Xenia; Proch, Dieter

    2004-08-01

    In a previous paper [1] a program for reducing the costs of high purity niobium was outlined. This program was based on the fact that niobium prices could be reduced, if a higher content of Ta, which does not significantly affect the RRR-value, could be tolerated for high performance cavities. This contribution reports on the execution of this program and its present status. Four ingots with different Ta contents have been melted and transformed into sheets. In each manufacturing step material quality has been monitored, using chemical analysis, thermal conductivity measurements and evaluation of mechanical properties. The niobium sheets have been scanned for defects by an eddy current device. Two single cell cavities (CEBAF geometry) have been fabricated from each of three ingots, with Ta concentrations of 150, 600 and 1300 wtppm. A series of tests have been performed on each cavity with increasing amount of material removal. This contribution reports on the test results and gives an analysis of the data.

  11. Microwave photoconductivity decay characterization of high-purity 4H-SiC substrates

    NASA Astrophysics Data System (ADS)

    Kumar, R. J.; Borrego, J. M.; Gutmann, R. J.; Jenny, J. R.; Malta, D. P.; Hobgood, H. McD.; Carter, C. H.

    2007-07-01

    A microwave photoconductivity decay (MPCD) technique, which probes conductivity change in wafers in response to either an above-band-gap or below-band-gap laser pulse, has been used to characterize recombination lifetime in high-purity 4H-SiC substrates produced with three different anneal processes. The above-band-gap (266nm) decay times vary from ˜10ns to tens of microseconds in the 4H-SiC substrates depending on the wafer growth parameters. Wafers produced using the three processes A (as-grown), B (annealed at 2000°C), and C (annealed at 2600°C) have decay times of 10-20ns, 50-500ns, and tens of microseconds, respectively. The differences in decay times are attributed to low, medium, and high densities of recombination centers in process C, B, and A wafers, respectively. The MPCD results correlate with other characterization results such as deep level transient spectroscopy, which also showed that the 2600°C anneal process significantly reduces defect densities, resulting in the enhanced recombination lifetimes. Modeling and one-dimensional simulations indicate a trapping center closer to the conduction band results in a longer MPCD decay transient, but such a trapping based model for the enhanced lifetimes is not compatible with the wide range of experimental characterization results described in this work, which indicate an annealing out of recombination centers at 2600°C.

  12. 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.

  13. 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.

  14. Preparation of the high purity gingerols from ginger by dummy molecularly imprinted polymers.

    PubMed

    Ji, Wenhua; Ma, Xiuli; Zhang, Jinghua; Xie, Hongkai; Liu, Feng; Wang, Xiao

    2015-03-27

    In this work, a dummy molecularly imprinted polymers (MIPs) were developed as the selective sorbents for preparation of the high purity gingerols from ginger for the first time. The dummy template molecule with similar structural skeleton to gingerols, N-vanillylnonanamide, has been designed and synthesized. The performance of the MIPs and non-imprinted polymers (NIPs) were evaluated including selective recognition capacity, adsorption isotherm, and adsorption kinetics. Optimization of various parameters affecting dummy molecular imprinted solid phase extraction (MISPE), such as the type and flow rate of the loading solvent, the composition and volume of the eluting solvent, and the composition and volume of the washing solvent were investigated. Gingerols with the percent recovery of 80 and the percent purity of 99.1 were obtained from the extracts of ginger by MISPE. Besides, gingerols obtained by MISPE had more powerful activity of eliminating free radical compared with extracts before extraction with the MISPE column. Application of MIPs with a high affinity toward three gingerols provides a novel method for obtaining a group of compounds which have likely active groups from natural products.

  15. 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.

  16. In vivo recovery with products of very high purity--assay discrepancies.

    PubMed

    Lusher, J M; Hillman-Wiseman, C; Hurst, D

    1998-07-01

    In view of reports of FVIII assay discrepancies in post-infusion plasma samples depending on methods used, we compared FVIII results run by each of four different methods following infusion of rFVIII (Kogenate). Nine persons with haemophilia A were infused with each of two lots of product. Plasma samples were obtained at baseline, and at 10 min, 30 min, 1, 2, 4, 8, 12, 14, 30 and 48 h post-infusion for measurement of FVIII. FVIII assay methods were chromogenic, and one-stage APTT using three different types of activators: micronized, silica, ellagic acid, and kaolin. The same reference plasma standard was used throughout. Results demonstrated a consistent difference in FVIII values, with chromogenic assays being considerably higher than those run by one-stage assays. The discrepancy was greatest when kaolin was the activator. These results point out the problems in attempting to determine the "correct" FVIII level in patient plasma samples following infusion of high purity FVIII preparations. Potential "pitfalls" include the standard used for defining product potency, the methods, reagents, instrumentation and standards used in assaying plasma samples and, in some instances, the characteristics of the product itself. This situation has considerable cost implications, potential impact on patient care, and makes it difficult to compare results between laboratories.

  17. 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.

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

    PubMed

    Campbell, D L; Peterson, T E

    2014-11-21

    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.

  19. Compensation mechanism in high purity semi-insulating 4H-SiC

    NASA Astrophysics Data System (ADS)

    Mitchel, W. C.; Mitchell, William D.; Smith, H. E.; Landis, G.; Smith, S. R.; Glaser, E. R.

    2007-03-01

    A study of deep levels in high purity semi-insulating 4H-SiC has been made using temperature dependent Hall effect (TDH), thermal and optical admittance spectroscopies, and secondary ion mass spectrometry (SIMS). Thermal activation energies from TDH varied from a low of 0.55eV to a high of 1.65eV. All samples studied showed n-type conduction with the Fermi level in the upper half of the band gap. Fits of the TDH data to different charge balance equations and comparison of the fitting results with SIMS measurements indicated that the deep levels are acceptorlike even though they are in the upper half of the band gap. Carrier concentration measurements indicated that the deep levels are present in concentrations in the low 1015cm-3 range, while SIMS results demonstrate nitrogen and boron concentrations in the low to mid-1015-cm-3 range. The results suggest that compensation in this material is a complex process involving multiple deep levels.

  20. 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.

  1. 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.

  2. 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.

  3. A solvent-extraction module for cyclotron production of high-purity technetium-99m.

    PubMed

    Martini, Petra; Boschi, Alessandra; Cicoria, Gianfranco; Uccelli, Licia; Pasquali, Micòl; Duatti, Adriano; Pupillo, Gaia; Marengo, Mario; Loriggiola, Massimo; Esposito, Juan

    2016-12-01

    The design and fabrication of a fully-automated, remotely controlled module for the extraction and purification of technetium-99m (Tc-99m), produced by proton bombardment of enriched Mo-100 molybdenum metallic targets in a low-energy medical cyclotron, is here described. After dissolution of the irradiated solid target in hydrogen peroxide, Tc-99m was obtained under the chemical form of (99m)TcO4(-), in high radionuclidic and radiochemical purity, by solvent extraction with methyl ethyl ketone (MEK). The extraction process was accomplished inside a glass column-shaped vial especially designed to allow for an easy automation of the whole procedure. Recovery yields were always >90% of the loaded activity. The final pertechnetate saline solution Na(99m)TcO4, purified using the automated module here described, is within the Pharmacopoeia quality control parameters and is therefore a valid alternative to generator-produced (99m)Tc. The resulting automated module is cost-effective and easily replicable for in-house production of high-purity Tc-99m by cyclotrons.

  4. Electron spin resonance spectroscopy of high purity crystals at millikelvin temperatures

    NASA Astrophysics Data System (ADS)

    Farr, Warrick G.; Creedon, Daniel L.; Goryachev, Maxim; Benmessai, Karim; Tobar, Michael E.

    2013-12-01

    Progress in the emerging field of engineered quantum systems requires the development of devices that can act as quantum memories. The realisation of such devices by doping solid state cavities with paramagnetic ions imposes a trade-off between ion concentration and cavity coherence time. Here, we investigate an alternative approach involving interactions between photons and naturally occurring impurity ions in ultra-pure crystalline microwave cavities exhibiting exceptionally high quality factors. We implement a hybrid Whispering Gallery/Electron Spin Resonance method to perform rigorous spectroscopy of an undoped single-crystal sapphire resonator over the frequency range 8{19 GHz, and at external applied DC magnetic fields up to 0.9 T. Measurements of a high purity sapphire cooled close to 100 mK reveal the presence of Fe3+, Cr3+, and V2+ impurities. A host of electron transitions are measured and identified, including the two-photon classically forbidden quadrupole transition (Δms = 2) for Fe3+, as well as hyperfine transitions of V2+.

  5. 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.

  6. Water-Assisted Preparation of High-Purity Semiconducting (14,4) Carbon Nanotubes.

    PubMed

    Yang, Feng; Wang, Xiao; Si, Jia; Zhao, Xiulan; Qi, Kuo; Jin, Chuanhong; Zhang, Zeyao; Li, Meihui; Zhang, Daqi; Yang, Juan; Zhang, Zhiyong; Xu, Zhi; Peng, Lian-Mao; Bai, Xuedong; Li, Yan

    2017-01-24

    Semiconducting single-walled carbon nanotubes (s-SWNTs) with diameters of 1.0-1.5 nm (with similar bandgap to crystalline silicon) are highly desired for nanoelectronics. Up to date, the highest reported content of s-SWNTs as-grown is ∼97%, which is still far below the daunting requirements of high-end applications. Herein, we report a feasible and green pathway to use H2O vapor to modulate the structure of the intermetallic W6Co7 nanocrystals. By using the resultant W6Co7 nanocatalysts with a high percentage of (1 0 10) planes as structural templates, we realized the direct growth of s-SWNT with the purity of ∼99%, in which ∼97% is (14,4) tubes (diameter 1.29 nm). H2O can also act as an environmentally friendly and facile etchant for eliminating metallic SWNTs, and the content of s-SWNTs was further improved to 99.8% and (14,4) tubes to 98.6%. High purity s-SWNTs with even bandgap determined by their uniform structure can be used for the exquisite applications in different fields.

  7. 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

  8. 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.

  9. High-purity semi-insulating 4H-SiC for microwave device applications

    NASA Astrophysics Data System (ADS)

    Jenny, J. R.; Malta, D. P.; Müller, St G.; Powell, A. R.; Tsvetkov, V. F.; Hobgood, H. Mcd; Glass, R. C.; Carter, C. H., Jr.

    2003-05-01

    High-purity, semi-insulating (HPSI) 4H-SiC crystals with diameters up to 75 mm have been grown by the seeded sublimation technique without the intentional introduction of elemental deep-level dopants, such as vanadium. Wafers cut from these crystals exhibit homogeneous activation energies near mid gap and thermally stable semi-insulating (SI) behavior (>109 ohm-cm) throughout device processing. Secondary ion mass spectroscopy, deep-level transient spectroscopy, optical admittance spectroscopy, and electron paramagnetic resonance data suggest that the SI behavior originates from several deep levels associated with intrinsic point defects. Micropipe densities in HPSI substrates have been demonstrated to be as low as 10 cm-2 in 2-in. substrates, and the room-temperature thermal conductivity of this material is near the theoretical maximum of 5 W/cm·K for 4H-SiC. Devices fabricated on these HPSI wafers do not exhibit any substrate related back-gating effects and have power densities as high as 5.2 W/mm with 63% power added efficiency.

  10. Characterization of high purity lycopene from tomato wastes using a new pressurized extraction approach.

    PubMed

    Naviglio, Daniele; Caruso, Tonino; Iannece, Patrizia; Aragòn, Alejandro; Santini, Antonello

    2008-08-13

    In this paper, a method for the extraction of high purity lycopene from tomato wastes is presented. The method is based on a pressurized extraction that uses the Extractor Naviglio, and it is performed in the 0.7-0.9 MPa range. Tomato skin, the byproduct deriving from manufacturing of tomato, in a water dispersion, are used as starting material. Lycopene is transferred, for the effect of the high pressure used, in the form of molecular aggregates into the water as a dispersion, while apolar compounds remain in the matrix. The aggregates are easily purified in a single subsequent step by using methanol, thus, obtaining lycopene at 98% chromatographic purity or higher. A new stationary phase, phenyl-hexyl silicone, and a simple water/acetonitrile gradient were used for HPLC analysis of lycopene. The extract was characterized by UV-Vis spectrophotometry, (1)H NMR, (13)C NMR, and electrospray ionization mass spectrometry. An average recovery of 2.8 mg lycopene/kg tomato waste can be obtained after 4 hours of extraction and using tap water as the extracting liquid. The recovery percentage was of about 10%. The exhausted tomato byproduct can be easily dried and used in agriculture or as feeding for animals.

  11. 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

  12. 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.

  13. 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

  14. 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.

  15. Evaluation of Prebiotic Effects of High-Purity Galactooligosaccharides in vitro and in vivo

    PubMed Central

    Hong, Ki Bae; Kim, Jae Hwan; Kwon, Hyuk Kon; Han, Sung Hee

    2016-01-01

    Summary Galactooligosaccharides (GOS) are an important class of dietary prebiotics that exert beneficial effects on intestinal microbiota and gut barrier function. In this study, high-purity GOS (HP-GOS) were investigated in vitro and in vivo and confirmed as prebiotic ingredients in rat diet. HP-GOS were successfully produced using a two-step process, enzymatic hydrolysis and fermentation by yeast. They were found to serve as a good substrate and carbon source for supporting the growth of probiotic bacteria more effectively than other commercial GOS. Following administration of 1% (by mass) of HP-GOS to rats, the growth of Bifidobacterium bifidum and B. longum in the gut increased most rapidly up to 12 h, and thereafter the increase was slow. Therefore, 1% HP-GOS was found to be acceptable for the growth of probiotic bacteria. Groups of animals that were orally administered HP-GOS and bifidobacteria during the study, and the group administered HP-GOS during the 2nd (days 13–15) and 4th (days 28–30) period of the study had significantly (p<0.05) higher numbers of bifidobacteria in faeces than groups receiving a single dose of bifidobacteria. HP-GOS affected the expression of genes encoding glucagon-like peptide-1 (GLP-1) and peptide YY (PYY). There was a significant upregulation of GLP-1 and PYY mRNA with HP-GOS and bifidobacteria intake. We propose that the prebiotic properties of HP-GOS are potentially valuable for the production of functional foods for human consumption. PMID:27904405

  16. Raman and photoelectron spectroscopic investigation of high-purity niobium materials: Oxides, hydrides, and hydrocarbons

    NASA Astrophysics Data System (ADS)

    Singh, Nageshwar; Deo, M. N.; Nand, Mangla; Jha, S. N.; Roy, S. B.

    2016-09-01

    We present investigations of the presence of oxides, hydrides, and hydrocarbons in high-purity (residual resistivity ratio, ˜300) niobium (Nb) materials used in fabrication of superconducting radio frequency (SRF) cavities for particle accelerators. Raman spectroscopy of Nb materials (as-received from the vendor as well as after surface chemical- and thermal processing) revealed numerous peaks, which evidently show the presence of oxides (550 cm-1), hydrides (1277 and 1385 cm-1: ˜80 K temperature), and groups of hydrocarbons (1096, 2330, 2710, 2830, 2868, and 3080 cm-1). The present work provides direct spectroscopic evidence of hydrides in the electropolished Nb materials typically used in SRF cavities. Raman spectroscopy thus can provide vital information about the near-surface chemical species in niobium materials and will help in identifying the cause for the performance degradation of SRF cavities. Furthermore, photoelectron spectroscopy was performed on the Nb samples to complement the Raman spectroscopy study. This study reveals the presence of C and O in the Nb samples. Core level spectra of Nb (doublet 3d5/2 and 3d3/2) show peaks near 206.6 and 209.4 eV, which can be attributed to the Nb5+ oxidation state. The core level spectra of C 1 s of the samples are dominated by graphitic carbon (binding energy, 284.6 eV), while the spectra of O 1 s are asymmetrically peaked near binding energy of ˜529 eV, and that indicates the presence of metal-oxide Nb2O5. The valence-band spectra of the Nb samples are dominated by a broad peak similar to O 2p states, but after sputtering (for 10 min) a peak appears at ˜1 eV, which is a feature of the elemental Nb atom.

  17. 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.

  18. 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.

  19. 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.

  20. 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.

  1. Uranium-233 purification and conversion to stabilized ceramic grade urania for LWBR fuel fabrication (LWBR Development Program)

    SciTech Connect

    Lloyd, R.

    1980-10-01

    High purity ceramic grade urania (/sup 233/UO/sub 2/) used in manufacturing the fuel for the Light Water Breeder Reactor (LWBR) core was made from uranium-233 that was obtained by irradiating thoria under special conditions to result in not more than 10 ppM of uranium-232 in the recovered uranium-233 product. A developmental study established the operating parameters of the conversion process for transforming the uranium-233 into urania powder with the appropriate chemical and physical attributes for use in fabricating the LWBR core fuel. This developmental study included the following: (a) design of an ion exchange purification process for removing the gamma-emitting alpha-decay daughters of uranium-232, to reduce the gamma-radiation field of the uranium-233 during LWBR fuel manufacture; (b) definition of the parameters for precipitating the uranium-233 as ammonium uranate (ADU) and for reducing the ADU with hydrogen to yield a urania conversion product of the proper particle size, surface area and sinterability for use in manufacturing the LWBR fuel; (c) establishment of parameters and design of equipment for stabilizing the urania conversion product to prevent it from undergoing excessive oxidation on exposure to the air during LWBR fuel manufacturing operations; and (d) development of a procedure and a facility to reprocess the unirradiated thoria-urania fuel scrap from the LWBR core manufacturing operations to recover the uranium-233 and convert it into high purity ceramic grade urania for LWBR core fabrication.

  2. 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

  3. 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

  4. 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

  5. Fabrication and properties of YBa2Cu3O7- x ceramics at different sintering temperatures

    NASA Astrophysics Data System (ADS)

    Prayoonphokkharat, Poom; Jiansirisomboon, Sukanda; Watcharapasorn, Anucha

    2013-07-01

    The influence of sintering temperatures on the fabrication of YBCO ceramics under normal air atmosphere was investigated in this study. YBCO ceramics were prepared by mixing starting compounds of Y2O3, BaCO3 and CuO powders, which were calcined at 850°C for 12 h. The powder was pelletized and sintered at different temperatures, from 930°C-1050°C, for 12 h. Phase identification was carried out by x-ray diffraction (XRD) technique. Scanning electron microscopy (SEM) with energy dispersive x-ray analysis (EDS) was used to study microstructure and chemical composition. In addition, density, Vickers hardness properties, the change of resistance and dielectric properties with temperature above T c were investigated. It was found that, at 950°C-1000°C, high-purity YBCO ceramic could be obtained. Outside this temperature range, either impurity phases were present or melting occurred. SEM images showed that grain size, which ranged from 1.5-2.5 µm, and hardness were related to density and liquid phase present in the sample. Furthermore, the sintering temperature affected oxygen content which, in turn, determined the conductive or semi-conductive behavior observed by electrical property measurement.

  6. 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.

  7. Matrix elimination ion chromatography method for the determination of trace levels of anionic impurities in high purity cesium iodide.

    PubMed

    Ayushi; Kumar, Sangita D; Reddy, A V R

    2012-01-01

    In the present study an ion chromatographic method based on matrix elimination has been developed for the determination of anionic impurities in high purity cesium iodide crystals. The presence of impurities has a detrimental effect on the characteristics of detectors based on cesium iodide crystals. In particular, oxygen-containing anions inhibit the resolving power of scintillators and decrease the optical absorption. The quantitative determination of anions (fluoride, chloride, bromide, nitrate, phosphate, and sulphate) simultaneously in the high-purity cesium iodide crystals has not been carried out before. The large concentration of iodide poses a challenge in the determination of anions (especially phosphate and sulphate); hence, matrix elimination is accomplished by adopting a sample pretreatment technique. The method is validated for linearity, accuracy, and precision. The limit of detection for different anions is in the range of 0.3-3 µg/g, and the relative standard deviation is in the range of 4-6% for the overall method.

  8. A facile route to preparation of high purity nanoporous silica from acid-leached residue of serpentine.

    PubMed

    Bai, Penn; Sharratt, Paul; Yeo, Tze Yuen; Bu, Jie

    2014-09-01

    As the current cost of mineral carbonation is too high for an economically viable industrial process, it is desirable to produce value-added products from CO2 mineralization process. In this work, a facile and cost-effective process was developed for the production of high purity SiO2 from acid-leached serpentine residue. The Si extraction rate is fast even under ambient conditions due to the highly defective structure of the residue. The reaction kinetics were studied and it was found that the Si extraction rate was under a combination of chemical reaction control and film diffusion control. The SiO2 sample prepared has high purity with a nanoporous structure, which renders it a potential candidate for applications such as an adsorbent and a catalyst support.

  9. 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.

  10. 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.

  11. 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

  12. 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.

  13. Investigation of possibility to fabricate Si3N4-TiN ceramic nanocomposite powder by azide SHS method

    NASA Astrophysics Data System (ADS)

    Kondratieva, L. A.; Kerson, I. A.; Illarionov, A. Yu; Amosov, A. P.; Bichurov, G. V.

    2016-11-01

    The process of self-propagating high-temperature synthesis with use of a powder of sodium azide NaN3 as a nitriding agent (the SHS-Az method) was applied to fabricate a nanocomposite powder Si3N4-TiN. Combustion of the initial mixtures of NaN3 only with precursors that are halides of silicon and titanium: Na2SiF6, (NH4)2SiF6, Na2TiF6, (NH4)2TiF6 did not allow us to synthesize the composite powder of Si3N4-TiN, as the phases of silicon nitride Si3N4 were not formed. After water washing, the ultrafine powdered product of combustion consisted of one target phase of titanium nitride only and a large amount of impurity of side phases. Replacement of the halide salt of one of the elements (Si or Ti) by the powder of this element in the initial mixture of SHS-Az system resulted in formation of silicon nitride together with the titanium nitride and impurities. The least amount of impurities was obtained by burning the initial mixtures of xSi + y(NH4)2TiF6 + zNaN3 system. Only the initial mixture of 9Si + (NH4)2TiF6 + 6NaN3 allowed us to obtain as a result of the SHS-Az process the nanostructured composite powder of Si3N4-TiN without impurities.

  14. 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.

  15. 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.

  16. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2014-06-01

    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.

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

    PubMed

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

    2014-06-01

    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.

  19. 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.

  20. 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.

  1. 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.

  2. High-purity hydrogen generation by ultraviolet illumination with the membrane composed of titanium dioxide nanotube array and Pd layer

    NASA Astrophysics Data System (ADS)

    Hattori, Masashi; Noda, Kei; Matsushige, Kazumi

    2011-09-01

    High-purity hydrogen generation was observed by using a membrane composed of a bilayer of an anodized titanium dioxide nanotube array (TNA) and a hydrogen permeable metal. This membrane was fabricated by transferring a TNA embedded in a titanium foil onto a sputtered 10-μm-thick palladium film. Alcohols are reformed photocatalytically and concurrently generated hydrogen is purified through the Pd layer. H2 with a purity of more than 99% was obtained from liquid alcohols under ultraviolet illumination onto the membrane. Thus, we demonstrated the integration of photocatalytic hydrogen production and purification within a single membrane.

  3. Rapid Single-Stage Separation of Micrometer-Long and High-Purity Semiconducting Carbon Nanotubes by Gel Filtration

    NASA Astrophysics Data System (ADS)

    Thendie, Boanerges; Miyata, Yasumitsu; Kitaura, Ryo; Miyauchi, Yuhei; Matsuda, Kazunari; Shinohara, Hisanori

    2013-06-01

    We demonstrate the separation of high-purity, long semiconducting single-wall carbon nanotubes (s-SWCNTs) by single-stage gel filtration. Semiconducting SWCNTs are preferentially adsorbed on an allyl dextran-based gel column and then eluted with surfactant solution at a rate that depends on nanotube length as well as electronic type of nanotubes. These differences allow the separation of length-sorted and purity-enhanced s-SWCNTs by fractionated collection of the eluate, which provides the desired nanotubes for electronic device applications.

  4. Processing and properties of high-purity, fine-grain-size depleted-uranium, deep-drawn shapes

    SciTech Connect

    Jackson, R J; Lundberg, M R; Bruchey, W L

    1980-10-01

    Unalloyed uranium is a candidate material for shaped charge liners used in conventional ordinance applications. For test purposes, it was decided that a high-grade uranium material with good toughness should be used. This report describes a process for producing a high-purity (less than 500 ppM total impurities) wrought material consisting of a recrystallized, equiaxed grain structure with a 10 micron (ASTM-8) average grain size. The fabrication process is discussed in detail. In all, six material conditions having a wide range of mechanical and structural properties were investigated. The tensile, hardness, and microstructural properties of these six material conditions are reported in detail.

  5. 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.

  6. The effect of a novel crystallised bioactive glass-ceramic powder on dentine hypersensitivity: a long-term clinical study.

    PubMed

    Tirapelli, C; Panzeri, H; Lara, E H G; Soares, R G; Peitl, O; Zanotto, E D

    2011-04-01

    The aim of this comparative clinical study was to evaluate a novel bioactive glass-ceramic (Biosilicate® 1-20 μm particles) to treat dentine hypersensitivity (DH). Volunteers (n = 120 patients/ 230 teeth) received the following treatments: G1-Sensodyne® , G2-SensiKill®, G3-Biosilicate® incorporated in a 1% water-free-gel and G4-Biosilicate® mixed with distilled water at 1:10 ratio. G1 and G3 were applied at home, daily for 30 days; G2 and G4 were applied once a week by a dentist (four applications). A visual analogue scale (VAS) was employed to evaluate pain for each quadrant in one sensitive tooth at baseline, weekly during treatment and during a 6-month follow-up period. Dentine hypersensitivity values (G1/n= 52), (G2/n =62), (G3/n = 59) and (G4/n = 59) were analysed with Kruskal-Wallis/Dunn tests. All the products were efficient in reducing DH after 4 weeks. Among the four materials tested, G4 demonstrated the best clinical performance and provided the fastest treatment to reduce DH pain. Distilled water proved to be an adequate vehicle to disperse Biosilicate®. Low DH scores were maintained during the 6-month follow-up period. The hypothesis that the novel bioactive glass-ceramic may be an efficient treatment for DH was confirmed.

  7. Clay minerals for advanced ceramics

    SciTech Connect

    Murray, H.H. )

    1989-11-01

    The author describes new and improved beneficiation techniques available to allow the production of clay minerals of exceptionally high purity. This is particularly true for kaolins and smectites. Wet processing techniques include particle size separation, high intensity magnetic separation, chemical leaching, flotation, and selective flocculation. The blending of clay minerals with other minerals provides opportunities to make special ceramic materials such as cordierite and other minerals that have very special ceramic properties including low heat expansion, high fired strength, low absorption, and other desired qualities.

  8. Compaction of spray-dried ceramic powders: An experimental study of the factors that control green density

    SciTech Connect

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

    1995-11-01

    The pressure-compaction response of a spray-dried, 94% alumina powder containing several percent of a polymeric binder was investigated as a function of die diameter and compact aspect ratio. The results show that the die fill density decreases markedly with decreasing die diameter and aspect ratio, while the final green density (at 120 MPa) decreases only slightly under the same conditions. These results suggest that the ratio of the initial compact dimensions to the size of the granules may be much more important than previously considered.

  9. [Determination of trace impurities in high purity titanium dioxide by high resolution inductively coupled plasma mass spectrometry].

    PubMed

    He, Xiao-Mei; Xie, Hua-Lin; Nie, Xi-Du; Tang, You-Gen

    2007-06-01

    An analytical method using high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for the rapid simultaneous determination of twenty six elements (Be, Na, Mg, Al, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, As, Mo, Cd, Sn, Sb, Ba, Ce, Nd, Sm, Pt, Pb and Bi) in high purity titanium dioxide was described. Samples were decomposed by (NH4)2SO4 and H2SO4. Most of the spectral interferences could be avoided by measuring in the high-resolution mode. The matrix effects due to the presence of excess sulfuric acid and Ti were evaluated. The optimum conditions for the determination were tested and discussed. The standard addition method was employed for quantitative analysis. The detection limits are 0.004-0.63 microg x g(-1), the recovery ratio is 87.6%-106.4%, and the RSD is less than 3.5%. The method is accurate, quick and convenient. It has been applied to the determination of trace impurities in high purity titanium dioxide with satisfactory results.

  10. High purity recombinant human Growth Hormone (rhGH) expression in Escherichia coli under phoA promoter.

    PubMed

    Song, Hao; Jiang, Jingxin; Wang, Xuedong; Zhang, Jianguo

    2016-07-26

    ABSTACT Recombinant human Growth Hormone (rhGH) is an important protein for human growth and is in high demand in clinics. Hence, it is necessary to develop an efficient fermentation process to produce highly pure rhGH. In this study, rhGH was expressed in Escherichia coli under alkaline phosphatase (phoA) promoter. The cultivation conditions for high expression level and purity of rhGH were investigated. The best initial phosphate concentration for rhGH expression, out of the 4 levels of initial phosphate concentration tests performed, was 12.6 mmol/L. Subsequently, 2 fed-batch cultivations under low dissolved oxygen (DO) (0% - 10%) and high DO (20% - 30%) conditions were carried out. High purity rhGH (92%) was obtained from 20% - 30% DO-stat cultivation, although the biomass did not show any significant difference. In summary, this research provided an efficient fermentation process for high purity rhGH production from E. coli under phoA promoter, which can lower the production and purification costs for large-scale production of rhGH.

  11. 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.

  12. 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.

  13. Qualification and initial characterization of a high-purity 233U spike for use in uranium analyses

    DOE PAGES

    Mathew, K. J.; Canaan, R. D.; Hexel, C.; ...

    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

  14. Matrix Elimination Ion Chromatography Method for the Determination of Trace Levels of Anionic Impurities in High Purity Cesium Iodide

    PubMed Central

    Ayushi; Kumar, Sangita D.; Reddy, A.V.R.

    2012-01-01

    In the present study an ion chromatographic method based on matrix elimination has been developed for the determination of anionic impurities in high purity cesium iodide crystals. The presence of impurities has a detrimental effect on the characteristics of detectors based on cesium iodide crystals. In particular, oxygen-containing anions inhibit the resolving power of scintillators and decrease the optical absorption. The quantitative determination of anions (fluoride, chloride, bromide, nitrate, phosphate, and sulphate) simultaneously in the high-purity cesium iodide crystals has not been carried out before. The large concentration of iodide poses a challenge in the determination of anions (especially phosphate and sulphate); hence, matrix elimination is accomplished by adopting a sample pretreatment technique. The method is validated for linearity, accuracy, and precision. The limit of detection for different anions is in the range of 0.3–3 µg/g, and the relative standard deviation is in the range of 4–6% for the overall method. PMID:22291061

  15. Determination of uranium, thorium, and 18 other elements in high-purity molybdenum by radiochemical neutron activation analysis

    SciTech Connect

    Theimer, K.H.; Krivan, V. )

    1990-12-15

    A radiochemical neutron activation analysis technique for the determination of uranium and thorium in high-purity molybdenum via the indicator radionuclides {sup 239}Np for U and {sup 233}Pa for Th has been developed. Simultaneously, the elements Ag, Co, Cr, Cs, Cu, Fe, Ga, In, Ir, K, Mn, Na, Ni, Rb, Ru, Sc, Se, and Zn can be determined, too. The elements Hf, Sb, Ta, Sn, and W were determined by instrumental neutron activation analysis. The radiochemical separation is performed by anion exchange on a Dowex 1 {times} 8 column from a 20 M HF/3% H{sub 2}O{sub 2} medium. A limit of detection of 4 ng/g for uranium and 40 pg/g for thorium can be achieved. For the other elements, the limits of detection are between 1 pg/g and 100 ng/g. A modified more selective separation of the indicator radionuclide of Th, {sup 233}Pa, allows improvement of the limit of detection for Th by a factor up to 5. This technique was applied to the analysis of high-purity molybdenum, and the results of a number of elements were compared with those of other techniques.

  16. 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

  17. 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.

  18. Microstructures and superconducting properties of high performance MgB2 thin films deposited from a high-purity, dense Mg-B target

    PubMed Central

    Li, G.Z.; Susner, M.A.; Bohnenstiehl, S.D.; Sumption, M.D.; Collings, E.W.

    2015-01-01

    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. PMID:26417117

  19. 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

  20. Microstructures and superconducting properties of high performance MgB2 thin films deposited from a high-purity, dense Mg-B target.

    PubMed

    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 10(5) A/cm(2) at 7.8 T; at 20 K, 10(5) A/cm(2) 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.

  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. Separation of analyte and matrix for the direct analysis of high-purity molybdenum-based materials by electrothermal atomic spectrometry methods—I. Radiotracer investigation of thermal extraction of impurities in a graphite cup

    NASA Astrophysics Data System (ADS)

    Dočekal, Bohumil; Krivan, Viliam; Franek, Martin

    1994-06-01

    By means of radiotracers, thermal vaporization of a number of detrimental trace elements (alkali, alkali earth and heavy metals) from metallic molybdenum powder has been studied. For this purpose, molybdenum samples labelled with appropriate radiotracers of the trace elements were prepared from a slurry of molybdenum oxide, ammonium molybdate solution and a radiotracer solution. Vaporization yields were measured after electrothermal treatment of the samples at temperatures between 1900 and 3000°C. Alkali and alkali earth elements, copper and zinc were vaporized with yields higher than 98%. Possible application of the electrothermal vaporization technique to the direct analysis of high-purity molybdenumbased materials by atomic absorption and atomic emission spectrometry is discussed.

  3. Nano-alumina powders/ceramics derived from aluminum foil waste at low temperature for various industrial applications.

    PubMed

    El-Amir, Ahmed A M; Ewais, Emad M M; Abdel-Aziem, Ahmed R; Ahmed, Adel; El-Anadouli, Bahgat E H

    2016-12-01

    In this work, nanoscale single crystalline γ- and α-alumina powders have been successfully prepared from aluminum foil waste precursor via co-precipitation method using NH4OH as a precipitant. The obtained gel after co-precipitation treatment, was calcined at different temperatures (500,700, 900, 1050, 1100, 1300 and 1500 °C) and the products were characterized by XRD, FTIR and HRTEM. The results revealed that nano-γ-Al2O3 was fully transformed to nanometer-sized α-Al2O3 (36-200 nm) after annealing at temperatures as low as 1100 °C.The thermally preheated powder at 500 °C was further pressed under 95 MPa by the uniaxial press and the obtained bodies were found to have98.82% of the theoretical density, 1.18% porosity and 708 MPa compressive strength, when sintered at temperatures as low as 1600 °C without using any sintering aid. These excellent results proved that this work will contribute to finding a commercial source for preparing sub 100 nm α-alumina through the secondary resources management and even more so to synthesizing strong α-Al2O3 bodies which are promising in terms of their structure and compression. The α-Al2O3 bodies synthesized by the present work could be used as a feedstock for fabrication of various kinds of functional and structural materials that are extensively used in high tech.

  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. 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.

  6. 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.

  7. 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.

  8. Engineering of high purity ultra-long optical needle field through reversing the electric dipole array radiation.

    PubMed

    Wang, Jiming; Chen, Weibin; Zhan, Qiwen

    2010-10-11

    We report a new method to create high purity longitudinally polarized field with extremely long depth of focus in the focal volume of a high numerical aperture (NA) objective lens. Through reversing the radiated field from an electric dipole array situated near the focus of the high-NA lens, the required incident field distribution in the pupil plane for the creation of an ultra-long optical needle field can be found. Numerical examples demonstrate that an optical needle field with a depth of focus up to 8λ is obtainable. Throughout the depth of focus, this engineered focal field maintains a diffraction limited transverse spot size (<0.43λ) with high longitudinal polarization purity. From the calculated pupil plane distribution, a simplified discrete complex pupil filter can be designed and significant improvements over the previously reported complex filters are clearly demonstrated.

  9. Industrial-scale separation of high-purity single-chirality single-wall carbon nanotubes for biological imaging.

    PubMed

    Yomogida, Yohei; Tanaka, Takeshi; Zhang, Minfang; Yudasaka, Masako; Wei, Xiaojun; Kataura, Hiromichi

    2016-06-28

    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.

  10. 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.

  11. 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.

  12. 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.

  13. Microfluidic Pipette Tip for High-Purity and High-Throughput Blood Plasma Separation from Whole Blood.

    PubMed

    Kim, Byeongyeon; Oh, Sein; You, Dongwon; Choi, Sungyoung

    2017-02-07

    Blood plasma separation from whole blood is often limited by numerous blood cells which can compromise separation processes and thus deteriorate separation performance such as purity and throughput. To address this challenge, we present a microfluidic pipet tip composed of slant array ridges that enable autonomous blood cell focusing without significant deviation as well as facilitating a high degree of parallelization without compromising separation purity. With these advantages, we achieved high-purity (99.88%) and high-throughput (904.3 μL min(-1)) plasma separation from whole blood. In combination with a smart pipet, we successfully demonstrated rapid, inexpensive, and equipment-free blood plasma preparation for pretransfusion testing.

  14. 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.

  15. 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.

  16. 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.

  17. 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.

  18. 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.

  19. 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.

  20. 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.

  1. Effect of low-temperature (77 K) quasihydrostatic extrusion on the properties of high-purity titanium: The role of initial structural state

    NASA Astrophysics Data System (ADS)

    Tikhonovsky, M. A.; Khaimovich, P. A.; Kutniy, K. V.; Kislyak, I. F.; Okovit, V. S.; Rudycheva, T. Yu.

    2013-11-01

    This is a study of the effect of quasihydrostatic extrusion at liquid nitrogen and room temperatures on the evolution of the structure and mechanical properties of high-purity titanium produced by severe plastic deformation in a swaging-extrusion-drawing regime and with subsequent annealing at temperatures of 350-550 °C. It is shown that a combination of severe plastic deformation and cryogenic quasihydrostatic extrusion makes it possible to create high-purity nanocrystalline titanium with high strength and plasticity.

  2. 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.

  3. The formation of high-purity isocyanurate through proazaphosphatrane-catalysed isocyanate cyclo-trimerisation: computational insights.

    PubMed

    Gibb, Jack N; Goodman, Jonathan M

    2013-01-07

    Polyurethane foams are widely used materials and control of their physical properties is a significant challenge. Management of cyclo-trimerisation during the polymerisation process is vital when tailoring the mechanical properties of the foam. Proazaphosphatranes are known to efficiently catalyse the cyclo-trimerisation of organic isocyanates, giving high purity isocyanurate with little uretdione by-product. The mechanism of this catalysis was previously unknown, although some zwitterionic intermediates have been identified spectroscopically. We have investigated a nucleophilic-catalysis reaction pathway involving sequential addition of methyl isocyanate to activated zwitterionic intermediates using density functional theory calculations. Evidence for significant transannulation by the proazaphosphatrane nitrogen was found for all intermediates, offering stabilisation of the phosphonium cation. Steric crowding at the proazaphosphatrane nucleophilic phosphorus gives rise to a preference for direct isocyanurate formation rather than via the uretdione, in sharp contrast to the uncatalysed system which has been found to preferentially proceed via the kinetic uretdione product. The investigations suggest the mechanism of proazaphosphatrane catalysed cyclo-oligomerisation does not proceed via the uretdione product, and hence why little of this impurity is observed experimentally.

  4. Influence of Grain Boundaries and their Composition on the Deformation Strength of High-purity, Synthetic Forsterite

    NASA Astrophysics Data System (ADS)

    Dillman, Amanda Marie

    Grain boundaries are an important feature of the mantle. With recent studies suggesting the majority of the upper mantle deforms by grain boundary sliding (Hirth and Kohlstedt, 2003; Hansen et al., 2013), understanding the role grain boundaries play is key. As grain boundary sliding always requires an accommodation mechanism, directly determining the contribution of grain boundary sliding to total strain on a sample is important for modeling deformation in the mantle. Altering grain boundary composition can change the structure and viscosity of the boundary. Understanding the effects of grain boundary composition is necessary for comparing data sets of different olivine as well as for accurately extrapolating experimental data to represent the mantle. In Chapter 2, uniaxial deformation experiments on high-purity synthetic forsterite at high temperature and ambient pressure are used to characterize the contribution of grain boundary sliding to strain in diffusion creep. Experiments were conducted in a one-atmosphere deformation rig, which allowed the polished surfaces of the samples to be analyzed with atomic force microscopy. The high temperature necessary for deformation enabled a great deal of thermal grooving, which can dramatically alter the topography of an initially polished surface. A methodology was developed to correct for the effect of thermal grooving and determine the amount of grain boundary sliding as a function of grain size and stress. A comparison is also made between two popular methods for determining grain size: the line intercept method and the equivalent area circle method. The line intercept method consistently produces larger grain sizes than the equivalent area circle method. In Chapter 3, triaxial compression experiments on forsterite are used to determine the effect of grain boundary chemistry on deformation strength. High-purity synthetic forsterite was doped with either Ca or Pr and then deformed at high temperature and a confining

  5. CO{sub 2} looping cycle performance of a high-purity limestone after thermal activation/doping

    SciTech Connect

    Vasilije Manovic; Edward J. Anthony; Gemma Grasa; J. Carlos Abanades

    2008-09-15

    The influence of thermal pretreatment on the performance of a high-purity limestone (La Blanca) during CO{sub 2} capture cycles is investigated in this paper. This limestone was chosen for more detailed investigation because, in earlier research, it failed to show any favorable effect as a result of thermal pretreatment. Here, the original sample, with a particle size of 0.4-0.6 mm, and ground samples were thermally pretreated at 1000-1200{sup o}C, for 6-24 h, and then subjected to several carbonation/calcination cycles in a thermogravimetric analyzer (TGA). This work shows that thermal pretreatment failed to produce a significant self-reactivation effect during CO{sub 2} cycles, despite the use of a wide range of conditions during pretreatment (grinding, temperature, and pretreatment duration) as well as during cycling (CO{sub 2} concentration and duration of the carbonation stage). Additional doping experiments showed that both high Na content and lack of Al in La Blanca limestone cause poor self-reactivation performance after thermal pretreatment. Scanning electron microscope-energy-dispersive X-ray (SEM-EDX) analyses also confirmed more pronounced sintering and loss of activity, which we believe are caused by the relatively high Na content. However, stabilization of sorbent particle morphology by Al can allow this limestone to show self-reactivation performance and higher conversions over a longer series of CO{sub 2} cycles. 35 refs., 12 figs., 2 tabs.

  6. Plastic deformation of high-purity a-titanium: model development and validation using the Taylor cylinder impact test

    NASA Astrophysics Data System (ADS)

    Chandola, Nitin; Revil-Baudard, Benoit; Cazacu, Oana

    2016-08-01

    Results of an experimental study on the quasi-static and high-rate plastic deformation due to impact of a high-purity, polycrystalline, a-titanium material are presented. To quantify the plastic anisotropy and tension-compression asymmetry of the material, first monotonic uniaxial compression and tension tests were carried out at room temperature under quasi-static conditions. It was found that the material is transversely isotropic and displays strong strength differential effects. To characterize the material's strain rate sensitivity, Split Hopkinson Pressure Bar tests in tension and compression were also conducted. Taylor impact tests were performed for impact velocity of 196 m/s. Plastic deformation extended to 64% of the length of the deformed specimen, with little radial spreading. To model simultaneously the observed anisotropy, strain-rate sensitivity, and tension-compression asymmetry of the material, a three-dimensional constitutive model was developed. Key in the formulation is a macroscopic yield function [1] that incorporates the specificities of the plastic flow, namely the combined effects of anisotropy and tension-compression asymmetry. Comparison between model predictions and data show the capabilities of the model to describe with accuracy the plastic behavior of the a-Ti material for both quasi-static and dynamic loadings, in particular, a very good agreement was obtained between the simulated and experimental post-test Taylor specimen geometries.

  7. 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

  8. Determination of indium in high purity antimony by electrothermal atomic absorption spectrometry (ETAAS) using boric acid as a modifier.

    PubMed

    Dash, K; Thangavel, S; Chaurasia, S C; Arunachalam, J

    2006-10-15

    The use of boric acid as a modifier for the determination of trace amount of indium in high purity antimony by electrothermal atomic absorption is described. It was found that the negative influence of the hydrofluoric acid, used for the digestion could not be eliminated by using stabilized temperature platform furnace (STPF) alone. Due to the high dissociation energy (D(0)=506kJmol(-1)) of indium fluoride, it is difficult to dissociate in the gas phase and hence is lost. In presence of HF (used for the dissolution of antimony), the universal Pd-Mg modifier does not work satisfactorily. Additionally, rising corrosion and reduced tube lifetime were observed when the acid digested (HF-HNO(3)) antimony solution was injected in to the platform. Improvement in platform life and elimination of interferences were achieved by the addition of boric acid as a chemical modifier together with ruthenium coating of the platform. Corrosive changes of the transversely heated graphite atomizer (THGA) platform surface were examined by scanning electron microscopy. The standard addition method was applied. A characteristic mass of 36pg was obtained. The detection limit of the proposed method is around 0.04mugg(-1). The developed method was applied to the determination of indium in real samples. The data obtained by this method were in good agreement with those obtained by ICP-MS.

  9. 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.

  10. Towards a single step process to create high purity gold structures by electron beam induced deposition at room temperature

    NASA Astrophysics Data System (ADS)

    Mansilla, C.; Mehendale, S.; Mulders, J. J. L.; Trompenaars, P. H. F.

    2016-10-01

    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.

  11. Development of High-purity Certified Reference Materials for 17 Proteinogenic Amino Acids by Traceable Titration Methods.

    PubMed

    Kato, Megumi; Yamazaki, Taichi; Kato, Hisashi; Eyama, Sakae; Goto, Mari; Yoshioka, Mariko; Takatsu, Akiko

    2015-01-01

    To ensure the reliability of amino acid analyses, the National Metrology Institute of Japan of the National Institute of Advanced Industrial Science and Technology (NMIJ/AIST) has developed high-purity certified reference materials (CRMs) for 17 proteinogenic amino acids. These CRMs are intended for use as primary reference materials to enable the traceable quantification of amino acids. The purity of the present CRMs was determined based on two traceable methods: nonaqueous acidimetric titration and nitrogen determination by the Kjeldahl method. Since neither method could distinguish compounds with similar structures, such as amino acid-related impurities, impurities were thoroughly quantified by combining several HPLC methods, and subtracted from the obtained purity of each method. The property value of each amino acid was calculated as a weighted mean of the corrected purities by the two methods. The uncertainty of the property value was obtained by combining measurement uncertainties of the two methods, a difference between the two methods, the uncertainty from the contribution of impurities, and the uncertainty derived from inhomogeneity. The uncertainty derived from instability was considered to be negligible based on stability monitoring of some CRMs. The certified value of each amino acid, property value with uncertainty, was given for both with or without enantiomeric separation.

  12. Evaluation of a new contact technology for a planar high-purity germanium double-sided strip detector

    NASA Astrophysics Data System (ADS)

    Jackson, Emily

    This thesis is an evaluation of a new electrode technology for segmented germanium gamma-ray detectors. The detector assessed herein is a planar high-purity germanium wafer (a LEPS or low-energy photon spectrometer) with 16 photolithographic-deposited, amorphous-germanium contacts on either side. This new contact material is shown to be an improvement over the current standard, lithium and boron electrodes, in both ease-of-manufacture and in performance. The symmetry gained with the use of one material for all the contacts is shown to greatly reduce the difference in energy collected by strips on either side. The stability of the amorphous germanium allows for finer electrode segmentation, reducing the gap between each strip. This smaller gap leads to a more uniform electric field in the active volume and ultimately less charge loss between strips. These improvements are quantified with the analysis of the energy difference and distribution of one- and two-hit interactions in the crystal by mono-energetic gamma rays from a 137Cs source. The detector is shown to be a major step forward in the development of contact technologies necessary for the application of position-sensitive gamma-detection outside of fundamental research, such as in nuclear medicine, astrophysics, and homeland security.

  13. Recovery of silicon from sewage sludge for production of high-purity nano-SiO(2).

    PubMed

    Zou, Jinlong; Dai, Ying; Pan, Kai; Jiang, Baojiang; Tian, Chungui; Tian, Guohui; Zhou, Wei; Wang, Lei; Wang, Xue; Fu, Honggang

    2013-02-01

    Generation of excess sewage sludge has already caused many environmental problems. A novel investigation for recovery of Si from the carbonized raw sewage sludge (RS) has been conducted in this study. Results show that early rupture (by OH(-)) of Si-O-Si bond in the networks of SiO(4)(4-) tetrahedron is the key step for formation of RS-derived sodium silicate (Na(2)O·(SiO(2))(x)·(H(2)O)(y)). SiO(2) gel is formed through the silica colloidal-particles cohesion, which is partly affected by the bridging role of the hydrated Na(+) (1070.7eV). O1s peaks of the SiO(2) can be decomposed into two components, i.e. Si-O bridging oxygen atoms (532.4 eV) and hydroxyl groups (O-H, 533.0 eV). Intensity of the O-H stretching vibration bands around 3450 cm(-1) (residual Si-OH), which is inversely related to the condensation degree, decreases as sol pH increases. Properties of this high purity RS-SiO(2) enable it to have the potential for numerous technological (environmental and biotechnology) applications. Reutilization of RS for production of SiO(2) may provide an environmental benefits to communities by protecting water, soil and air.

  14. 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.

  15. 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)

  16. 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.

  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.

    1999-07-13

    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.

  19. 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.

  20. Synthesis of mullite powders by acrylamide polymerization.

    SciTech Connect

    Sin, A.; Picciolo, J. J.; Lee, R. H.; Gutierrez-Mora, F.; Goretta, K. C.; Energy Technology; INPG-CNRS

    2001-09-01

    Mullite (3Al{sub 2}O{sub 3} {center_dot} 2SiO{sub 2}) ceramics and composites are widely used. Synthesis of mullite powders, especially those that can be readily sintered, remains a focus of much current research. In support of recent efforts to fabricate mullite fibrous monoliths and to use superplastic flow to join ceramics, we have looked to synthesize reactive mullite powders. Recent advances in application of acrylamide polymers to ceramic synthesis offer promise of obtaining large quantities of high-quality powder at relatively low cost. We report here on synthesis from acrylamide monomers of mullite powders of two interesting particle sizes.

  1. Effects of ultrasonication and conventional mechanical homogenization processes on the structures and dielectric properties of BaTiO3 ceramics.

    PubMed

    Akbas, Hatice Zehra; Aydin, Zeki; Yilmaz, Onur; Turgut, Selvin

    2017-01-01

    The effects of the homogenization process on the structures and dielectric properties of pure and Nb-doped BaTiO3 ceramics have been investigated using an ultrasonic homogenization and conventional mechanical methods. The reagents were homogenized using an ultrasonic processor with high-intensity ultrasonic waves and using a compact mixer-shaker. The components and crystal types of the powders were determined by Fourier-transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD) analyses. The complex permittivity (ε('), ε″) and AC conductivity (σ') of the samples were analyzed in a wide frequency range of 20Hz to 2MHz at room temperature. The structures and dielectric properties of pure and Nb-doped BaTiO3 ceramics strongly depend on the homogenization process in a solid-state reaction method. Using an ultrasonic processor with high-intensity ultrasonic waves based on acoustic cavitation phenomena can make a significant improvement in producing high-purity BaTiO3 ceramics without carbonate impurities with a small dielectric loss.

  2. Los Alamos National Laboratory final report

    SciTech Connect

    Lopez, W.H. . Center for Micro-Engineered Ceramics)

    1993-01-01

    Five subtasks are reported on: laser ablation synthesis of nanophase ceramic powders (alumina, AlN), preparation of high-purity submicron MoSi[sub 2], microwave sintering of ceramics, synthesis of high-purity mullite, and scale-up of aerosol decomposition for ceramic powder production.

  3. Los Alamos National Laboratory final report

    SciTech Connect

    Lopez, W.H.

    1993-01-01

    Five subtasks are reported on: laser ablation synthesis of nanophase ceramic powders (alumina, AlN), preparation of high-purity submicron MoSi{sub 2}, microwave sintering of ceramics, synthesis of high-purity mullite, and scale-up of aerosol decomposition for ceramic powder production.

  4. Unique low-molecular-weight lignin with high purity extracted from wood by deep eutectic solvents (DES): a source of lignin for valorization

    SciTech Connect

    Alvarez-Vasco, Carlos; Ma, Ruoshui; Quintero, Melissa; Guo, Mond; Geleynse, Scott; Ramasamy, Karthikeyan K.; Wolcott, Michael; Zhang, Xiao

    2016-01-01

    This paper reports a new method of applying Deep Eutectic Solvents (DES) for extracting lignin from woody biomass with high yield and high purity. DES mixtures prepared from Choline Chloride (ChCl) and four hydrogen-bond donors–acetic acid, lactic acid, levulinic acid and glycerol–were evaluated for treatment of hardwood (poplar) and softwood (D. fir). It was found that these DES treatments can selectively extract a significant amount of lignin from wood with high yields: 78% from poplar and 58% from D. fir. The extracted lignin has high purity (95%) with unique structural properties. We discover that DES can selectively cleave ether linkages in wood lignin and facilitate lignin removal from wood. The mechanism of DES cleavage of ether bonds between phenylpropane units was investigated. The results from this study demonstrate that DES is a promising solvent for wood delignification and the production of a new source of lignin with promising potential applications.

  5. 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.

  6. 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.

  7. Ionic liquid-based extraction followed by graphite-furnace atomic absorption spectrometry for the determination of trace heavy metals in high-purity iron metal.

    PubMed

    Matsumiya, Hiroaki; Kato, Tatsuya; Hiraide, Masataka

    2014-02-01

    The analysis of high-purity materials for trace impurities is an important and challenging task. The present paper describes a facile and sensitive method for the determination of trace heavy metals in high-purity iron metal. Trace heavy metals in an iron sample solution were rapidly and selectively preconcentrated by the extraction into a tiny volume of an ionic liquid [1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide] for the determination by graphite-furnace atomic absorption spectrometry (GFAAS). A nitrogen-donating neutral ligand, 2,4,6-tris(2-pyridyl)-1,3,5-triazine (TPTZ), was found to be effective in the ionic liquid-based selective extraction, allowing the nearly complete (~99.8%) elimination of the iron matrix. The combination with the optimized GFAAS was successful. The detectability reached sub-μg g(-1) levels in iron metal. The novel use of TPTZ in ionic liquid-based extraction followed by GFAAS was successfully applied to the determination of traces of Co, Ni, Cu, Cd, and Pb in certified reference materials for high-purity iron metal.

  8. 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

  9. Improved compaction of ZnO nano-powder triggered by the presence of acetate and its effect on sintering

    PubMed Central

    Gonzalez-Julian, Jesus; Guillon, Olivier

    2015-01-01

    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. PMID:27877777

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. 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.

  18. Fine-grained multiferroic BaTiO{sub 3}/(Ni{sub 0.5}Zn{sub 0.5})Fe{sub 2}O{sub 4} composite ceramics synthesized by novel powder-in-sol precursor hybrid processing route

    SciTech Connect

    Zhang Hongfang; Or, Siu Wing; Chan, Helen Lai Wa

    2009-06-03

    Dense, homogeneous, and fine-grained multiferroic BaTiO{sub 3}/(Ni{sub 0.5}Zn{sub 0.5})Fe{sub 2}O{sub 4} composite ceramics are synthesized by a novel powder-in-sol precursor hybrid processing route. This route includes the dispersion of nanosized BaTiO{sub 3} ferroelectric powders prepared via conventional sold-state ceramic process into (Ni{sub 0.5}Zn{sub 0.5})Fe{sub 2}O{sub 4} ferromagnetic sol-gel precursor prepared via sol-gel wet chemistry process. Uniformly distributed slurry is obtained after ball milling and used in the fabrication of the ceramics with low sintering temperatures. The ceramics show coexistence of ferromagnetic and ferroelectric phases with obvious ferromagnetic and ferroelectric hysteresis loops at room temperature, besides exhibiting excellent magnetic and dielectric properties in a wide range of frequency. The combination of high permeability and permittivity with low losses in the ceramics enables significant miniaturization of electronic devices based on the ceramics.

  19. 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.

  20. 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

  1. 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.

  2. 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.

  3. Magnetic Behavior of High-Density Powder Metallurgy Bodies

    DTIC Science & Technology

    1976-03-01

    rupture and impact resistance. Square bars were prepared from a single type of high-purity iron powder with minimal carbon content, so as to...of theoret- ical. Available dies guided the selection of sample geometry for compatibility with mechanical ( Charpy , transverse rupture) and magnetic...sturdier die was used for 96% specimens measur- ing 2.95 x 0.39 x 0.39 inches (as for Charpy tests). For comparison of the dies, additional 86% and

  4. Effect of low-energy alpha-particles irradiation on surface structure and physical-mechanical properties of high-purity tungsten

    NASA Astrophysics Data System (ADS)

    Aldabergenova, T. M.; Kislitsin, S. B.; Larionov, A. S.; Yar-Mukhamedova, G. S.

    2016-11-01

    Effect of radiation by low-energy alpha-particles on the surface structure and physical-mechanical properties of high-purity tungsten was studied. Samples of tungsten were irradiated by 4He+2 ions with the energy of 45 keV at low-energy channel of accelerator DC-60 in Astana branch of Institute Nuclear Physics. Irradiation fluence was 1.5 × 1018 cm-2, irradiation temperature was 150°C. Experimentally found that irradiation with low-energy alpha particles results in formation of helium filled bubbles in the straggling region.

  5. Influence of the chloride ion concentration on the corrosion of high-purity Mg, ZE41 and AZ91 in buffered Hank's solution.

    PubMed

    Taltavull, C; Shi, Z; Torres, B; Rams, J; Atrens, A

    2014-02-01

    This research studied the influence of the chloride ion concentration on the corrosion behaviour of high-purity magnesium (Mg) and two Mg alloys in Hank's solution, using hydrogen evolution and weight loss. A buffer based on CO2 and NaHCO3 was used to maintain the pH constant. The corrosion behaviour was governed by a partially protective surface film, and film breakdown by the chloride ions. The carbonated calcium phosphate layer that formed in Hank's solution was important in determining the protective properties of the surface film.

  6. 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.

  7. Determination of rare earth elements in high purity rare earth oxides by liquid chromatography, thermionic mass spectrometry and combined liquid chromatography/thermionic mass spectrometry

    NASA Astrophysics Data System (ADS)

    Stijfhoorn, D. E.; Stray, H.; Hjelmseth, H.

    1993-03-01

    A high-performance liquid Chromatographie (HPLC) method for the determination of rare earth elements in rocks has been modified and used for the determination of rare earth elements (REE) in high purity rare earth oxides. The detection limit was 1-1.5 ng or 2-3 mg/kg when a solution corresponding to 0.5 mg of the rare earth oxide was injected. The REE determination was also carried out by adding a mixture of selected REE isotopes to the sample and analysing the collected HPLC-fractions by mass spectrometry (MS) using a thermionic source. Since the matrix element was not collected, interference from this element during the mass spectrometric analysis was avoided. Detection limits as low as 0.5 mg/kg could then be obtained. Detection limits as low as 0.05 mg/kg were possible by MS without HPLC-pre-separation, but this approach could only be used for those elements that were not affected by the matrix. Commercial samples of high purity Nd 2O 3, Gd 2O 3 and Dy 2O 3 were analysed in this study, and a comparison of results obtained by HPLC, combined HPLC/MS and direct MS are presented.

  8. Determination of traces of rubidium in high purity cesium chloride by electrothermal atomic absorption spectrometry (ETAAS) using boric acid as a modifier.

    PubMed

    Dash, K; Thangavel, S; Chaurasia, S C; Arunachalam, J

    2007-02-12

    The use of boric acid as a modifier for the determination of trace amount of rubidium in high purity cesium chloride matrix by electrothermal atomic absorption is described. It was found that the negative influence of the chloride matrix could not be eliminated using stabilized temperature platform (STPF) alone. Due to the high dissociation energy (D(0)=427 kJ mol(-1)) of rubidium chloride, it was difficult to dissociate in the gas phase and hence is lost. Elimination of interferences was achieved by the addition of boric acid as a chemical modifier. Diluted cesium chloride samples (5%, m/v) were analyzed applying the standard addition method. The characteristic mass of 24 pg was obtained. The detection limit of the proposed method is around 26 ng g(-1). The developed method was applied to the determination of traces of rubidium in high purity cesium chloride samples. The data obtained by this method were in good agreement with those obtained by other independent method like FAAS.

  9. 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.

  10. Pre-degenerated peripheral nerves co-cultured with bone marrow-derived cells: a new technique for harvesting high-purity Schwann cells

    PubMed Central

    Wang, Xiao-pan; Wu, Min; Guan, Jian-zhong; Wang, Zhao-dong; Gao, Xu-bin; Liu, Yang-yang

    2016-01-01

    Schwann cells play an important role in the peripheral nervous system, especially in nerve repair following injury, so artificial nerve regeneration requires an effective technique for obtaining purified Schwann cells. In vivo and in vitro pre-degeneration of peripheral nerves have been shown to obtain high-purity Schwann cells. We believed that in vitro pre-degeneration was simple and controllable, and available for the clinic. Thus, we co-cultured the crushed sciatic nerves with bone marrow-derived cells in vitro. Results demonstrated that, 3 hours after injury, a large number of mononuclear cells moved to the crushed nerves and a large number of bone marrow-derived cells infiltrated the nerve segments. These changes promoted the degradation of the nerve segments, and the dedifferentiation and proliferation of Schwann cells. Neural cell adhesion molecule and glial fibrillary acidic protein expression were detected in the crushed nerves. Schwann cell yield was 9.08 ± 2.01 × 104/mg. The purity of primary cultured Schwann cells was 88.4 ± 5.79%. These indicate a successful new method for obtaining Schwann cells of high purity and yield from adult crushed sciatic nerve using bone marrow-derived cells. PMID:27904498

  11. 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…

  12. Structural and electrical properties of NASICON type solid electrolyte nanoscaled glass-ceramic powder by mechanical milling for thin film batteries.

    PubMed

    Patil, Vaishali; Patil, Arun; Yoon, Seok-Jin; Choi, Ji-Won

    2013-05-01

    During last two decades, lithium-based glasses have been studied extensively as electrolytes for solid-state secondary batteries. For practical use, solid electrolyte must have high ionic conductivity as well as chemical, thermal and electrochemical stability. Recent progresses have focused on glass electrolytes due to advantages over crystalline solid. Glass electrolytes are generally classified into two types oxide glass and sulfide glass. Oxide glasses do not react with electrode materials and this chemical inertness is advantageous for cycle performances of battery. In this study, major effort has been focused on the improvement of the ion conductivity of nanosized LiAlTi(PO4)3 oxide electrolyte prepared by mechanical milling (MM) method. After heating at 1000 degrees C the material shows good crystallinity and ionic conductivity with low electronic conductivity. In LiTi2(PO4)3, Ti4+ ions are partially substituted by Al3+ ions by heat-treatment of Li20-Al2O3-TiO2-P2O5 glasses at 1000 degrees C for 10 h. The conductivity of this material is 1.09 x 10(-3) S/cm at room temp. The glass-ceramics show fast ion conduction and low E(a) value. It is suggested that high conductivity, easy fabrication and low cost make this glass-ceramics promising to be used as inorganic solid electrolyte for all-solid-state Li rechargeable batteries.

  13. 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

  14. 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.

  15. 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.

  16. 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.

  17. In vitro and in vivo characterization of a high-purity, solvent/detergent-treated factor VIII concentrate: evidence for its therapeutic efficacy in von Willebrand's disease.

    PubMed

    Mazurier, C; De Romeuf, C; Parquet-Gernez, A; Goudemand, M

    1989-07-01

    A factor VIII (FVIII) concentrate, virus-inactivated by the solvent/detergent procedure, was studied in vitro. In contrast with most high-purity, virus-inactivated FVIII concentrates, it contains not only high levels of von Willebrand factor (vWF) antigen and ristocetin cofactor activity but also high molecular weight forms of von Willebrand factor. Furthermore, it is able to promote platelet adhesion on collagen in a perfusion system. In vivo studies performed in patients with different types of von Willebrand's disease provided evidence that this concentrate corrects Duke's bleeding time and prevents or stops haemorrhages. Thus, the particular advantages of this FVIII/vWF preparation are safety, low content of contamination proteins, and efficacy in von Willebrand's disease.

  18. Characteristics of signals originating near the lithium-diffused N+ contact of high purity germanium p-type point contact detectors

    DOE PAGES

    Aguayo, E.; Amman, M.; Avignone, F. T.; ...

    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

  19. RADIOCHEMICAL PURITY OF MO AND TC SOLUTION OBTAINED AFTER IRRADIATION AND DISSOLUTION OF MO-100-ENRICHED AND ULTRA-HIGH-PURITY NATURAL MO DISKS

    SciTech Connect

    Tkac, Peter; Gromov, Roman; Chemerisov, Sergey D.; Rotsch, David A.; Vandegrift, George F.

    2016-09-01

    Four irradiations of ultra-high-purity natural Mo targets and one irradiation using 97.4% Mo-100-enriched material were performed. The purpose of these irradiations was to determine whether the presence of Sn stabilizer in the H2O2 used for the dissolution of sintered Mo disks can affect the radiochemical purity of the final K2MoO4 in 5M KOH solution. Results from radiochemical purity tests performed using thin-layer paper chromatography show that even 2– 3× excess of Sn-stabilized H2O2 typically used for dissolution of sintered Mo disks did not affect the radiochemical purity of the final product.

  20. 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.

  1. Thermal evolution of high-purity and boron-doped sub-microcrystalline Ni{sub 3}Al produced by severe plastic deformation

    SciTech Connect

    Korznikov, A.V.; Korznikova, G.F.; Idrisova, S.R.; Dimitrov, O.; Dallas, J.P.; Faudot, F.; Valiev, R.Z.

    1999-09-08

    The influence of boron on the structural stability of sub-microcrystalline Ni{sub 3}Al intermetallic compounds was investigated by comparing a high-purity material with a boron-doped (0.1 wt%) compound. The nanocrystalline structure was obtained by severe shear deformation under quasi-hydrostatic pressure. Residual electrical resistivity, Vickers microhardness, X-ray diffraction and transmission electron microscopy were used to characterize the material evolution during thermal treatments in the temperature range 293--1,313 K. After severe deformation the materials were disordered, with a small crystallite size of about 20 nm, similar in both materials. During isochronal anneals, the evolution of the microstructure, the long-range ordering and the recovery of the investigated properties took place at higher temperatures in the boron-doped compound, i.e. the thermal stability of the cold-worked structure was higher.

  2. 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.

  3. 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.

  4. Determination of trace impurities in high-purity zirconium dioxide by inductively coupled plasma atomic emission spectrometry using microwave-assisted digestion and wavelet transform-based correction procedure.

    PubMed

    Ma, Xiaoguo; Li, Yibing

    2006-10-02

    This paper describes a rapid, accurate and precise method for the determination of trace Fe, Hf, Mn, Na, Si and Ti in high-purity zirconium dioxide (ZrO2) powders by inductively coupled plasma atomic emission spectrometry (ICP-AES). The samples were dissolved by a microwave-assisted digestion system. Four different digestion programs with various reagents were tested. It was found that using a mixture of sulfuric acid (H2SO4) and ammonium sulfate ((NH4)2SO4), the total sample dissolution time was 30 min, much shorter than that required for conventional digestion in an opening system. The determination of almost all of the target analytes suffered from spectral interferences, since Zr shows a line-rich atomic emission spectrometry. The wavelet transform (WT), a recently developed mathematical technique was applied to the correction of spectral interference, and more accurate and precise results were obtained, compared with traditional off-peak background correction procedure. Experimental work revealed that a high Zr concentration would result in a significant decrease in peak height of the analyte lines, which was corrected by standard addition method. The performance of the developed method was evaluated by using synthetic samples. The recoveries were in the range of 87-112% and relative standard deviation was within 1.1-3.4%. The detection limits (3sigma) for Fe, Hf, Mn, Na, Si and Ti were found to be 1.2, 13.3, 1.0, 4.5, 5.8 and 2.0 microg g(-1), respectively. The results showed that with the microwave-assisted digestion and the WT correction, the detection limits have improved by a factor of about 5 for Fe, 4 for Mn and Ti, 3 for Si, and 2 for Hf and Na, respectively, in comparison with conventional open-system digestion and off-peak correction. The proposed technique was applied to the analysis of trace elements above-mentioned in three types of ZrO2 powders.

  5. 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.

  6. Monte Carlo simulation of gamma-ray interactions in an over-square high-purity germanium detector for in-vivo measurements

    NASA Astrophysics Data System (ADS)

    Saizu, Mirela Angela

    2016-09-01

    The developments of high-purity germanium detectors match very well the requirements of the in-vivo human body measurements regarding the gamma energy ranges of the radionuclides intended to be measured, the shape of the extended radioactive sources, and the measurement geometries. The Whole Body Counter (WBC) from IFIN-HH is based on an “over-square” high-purity germanium detector (HPGe) to perform accurate measurements of the incorporated radionuclides emitting X and gamma rays in the energy range of 10 keV-1500 keV, under conditions of good shielding, suitable collimation, and calibration. As an alternative to the experimental efficiency calibration method consisting of using reference calibration sources with gamma energy lines that cover all the considered energy range, it is proposed to use the Monte Carlo method for the efficiency calibration of the WBC using the radiation transport code MCNP5. The HPGe detector was modelled and the gamma energy lines of 241Am, 57Co, 133Ba, 137Cs, 60Co, and 152Eu were simulated in order to obtain the virtual efficiency calibration curve of the WBC. The Monte Carlo method was validated by comparing the simulated results with the experimental measurements using point-like sources. For their optimum matching, the impact of the variation of the front dead layer thickness and of the detector photon absorbing layers materials on the HPGe detector efficiency was studied, and the detector’s model was refined. In order to perform the WBC efficiency calibration for realistic people monitoring, more numerical calculations were generated simulating extended sources of specific shape according to the standard man characteristics.

  7. A combined arc-melting and tilt-casting furnace for the manufacture of high-purity bulk metallic glass materials.

    PubMed

    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 Zr(55)Cu(30)Al(10)Ni(5) 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.

  8. A hybrid enrichment process combining conjugated polymer extraction and silica gel adsorption for high purity semiconducting single-walled carbon nanotubes (SWCNT)

    NASA Astrophysics Data System (ADS)

    Ding, Jianfu; Li, Zhao; Lefebvre, Jacques; Cheng, Fuyong; Dunford, Jeffrey L.; Malenfant, Patrick R. L.; Humes, Jefford; Kroeger, Jens

    2015-09-01

    A novel purification process for the enrichment of sc-SWCNTs that combines selective conjugated polymer extraction (CPE) with selective adsorption using silica gel, termed hybrid-CPE (h-CPE), has been developed, providing a high purity sc-SWCNT material with a significant improvement in process efficiency and yield. Using the h-CPE protocol, a greater than 5 fold improvement in yield can be obtained compared to traditional CPE while obtaining sc-SWCNT with a purity >99.9% as assessed by absorption spectroscopy and Raman mapping. Thin film transistor devices using the h-CPE derived sc-SWCNTs as the semiconductor possess mobility values ranging from 10-30 cm2 V-1 s-1 and current ON/OFF ratio of 104-105 for channel lengths between 2.5 and 20 μm.A novel purification process for the enrichment of sc-SWCNTs that combines selective conjugated polymer extraction (CPE) with selective adsorption using silica gel, termed hybrid-CPE (h-CPE), has been developed, providing a high purity sc-SWCNT material with a significant improvement in process efficiency and yield. Using the h-CPE protocol, a greater than 5 fold improvement in yield can be obtained compared to traditional CPE while obtaining sc-SWCNT with a purity >99.9% as assessed by absorption spectroscopy and Raman mapping. Thin film transistor devices using the h-CPE derived sc-SWCNTs as the semiconductor possess mobility values ranging from 10-30 cm2 V-1 s-1 and current ON/OFF ratio of 104-105 for channel lengths between 2.5 and 20 μm. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr04851f

  9. 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.

  10. 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

  11. 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.

  12. 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.

  13. Multi-Scale Porous Ultra High Temperature Ceramics

    DTIC Science & Technology

    2015-01-08

    flights. 15. SUBJECT TERMS Ultra High Temperature Ceramics, Colloidal Powder Processing, Multi-scale Porous Materials, Lattice Monte...flights. 15. SUBJECT TERMS Ultra High Temperature Ceramics, Colloidal Powder Processing, Multi-scale Porous Materials, Lattice Monte Carlo Method 16...for better control of the heat transfer. The routes proposed to manufacture such materials rely on the combination of colloidal processing

  14. 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.

  15. 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

    2016-02-02

    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.

  16. 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.

  17. 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.

  18. 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.

  19. Structural ceramics

    SciTech Connect

    Wachtman, J.B. Jr.

    1989-01-01

    The present work discusses opportunities for application of structural ceramics in heat engines, industrial-wear parts, prosthetics and bearings; conceptual and detailed design principles for structural ceramics; the processing, consolidation, and properties of members of the SiC family of structural ceramics; and the silicon nitride and sialon families of hot-pressed, sintered, and reaction-bonded, structural ceramics. Also discussed are partially-stabilized zirconia and zirconia-toughened ceramics for structural applications, the processing methods and mechanisms of fiber-reinforcement in ceramic-matrix fiber-reinforced composites, and the tribological properties of structural ceramics.

  20. 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.

  1. Method of manufacturing ceramic shaped articles

    NASA Astrophysics Data System (ADS)

    Inoue, K.

    1983-05-01

    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.

  2. 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.

  3. 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.

  4. 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.

  5. 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

  6. 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.

  7. Er-doped and Er, Yb co-doped oxyfluoride glasses and glass-ceramics, structural and optical properties

    NASA Astrophysics Data System (ADS)

    Lisiecki, Radosław; Augustyn, Elżbieta; Ryba-Romanowski, Witold; Żelechower, Michał

    2011-09-01

    The selected glasses and glass-ceramics pertinent to following chemical composition in mol%:48%SiO 2-11%Al 2O 3-7%Na 2O-10%CaO-10%PbO-11%PbF 2-3%ErF 3 and 48%SiO 2-11%Al 2O 3-7%Na 2O-10%CaO-10%PbO-10%PbF 2-1%ErF 3-3%YbF 3 have been manufactured from high purity components (Aldrich) at 1450 °C in normal atmosphere. Glass optical fibers were successfully drawn. Subsequently they were subject to the heat-treatment at 700 °C in various time periods. The preceding differential thermal analysis (DTA) studies allowed estimating both the fiber drawing temperature and the controlled crystallization temperature of glass fibers. It has been observed that the controlled heat-treatment of oxyfluoride glass fibers results in the creation of Pb 5Al 3F 19, Er 4F 2O 11Si 3 and Er 3FO 10Si 3 crystalline phases. The identified phases were characterized by X-ray powder diffraction (XRD) and confirmed by selected area electron diffraction (SAED). The fibers consist of mixed amorphous-crystalline microstructure with nano-crystals of size even below 10 nm distributed in the glassy host. Their morphology was investigated applying high-resolution transmission electron microscopy. Optical properties and excited state relaxation dynamics of optically active ions (Er 3+, Yb 3+) in glass and glass-ceramics have been studied. Based on absorption spectra the Judd-Ofelt analysis was carried out. The main attention was directed to NIR luminescence at. 1.6 μm related to 4I 13/2 → 4I 15/2 Er 3+ and less effective emission associated with 4I 11/2 → 4I 15/2 Er 3+ and 2F 5/2 → 2F 7/2 Yb 3+ transitions. The dissimilar spectroscopic properties have been revealed for glasses and glass-ceramic samples, respectively. The reduction of emission linewidth at 1.6 and 1.0 μm combined with substantial increase of 4I 13/2 lifetimes of erbium in glass-ceramics appear to be evidences that Er 3+ ions are accommodated in crystalline phases. The structural and optical characteristics of oxyfluoride glass-ceramic

  8. Purification of high-purity glycyrrhizin from licorice using hydrophilic interaction solid phase extraction coupled with preparative reversed-phase liquid chromatography.

    PubMed

    Yu, Wenyi; Jin, Hongli; Shen, Aijin; Deng, Liang; Shi, Jianlian; Xue, Xingya; Guo, Yadong; Liu, Yanfang; Liang, Xinmiao

    2017-01-01

    Glycyrrhizin (GA), a major bioactive compound in licorice, has been extensively used throughout the world as a medicine to treat chronic viral hepatitis and allergic dermatitis. In this study, a new method based on hydrophilic interaction solid phase extraction (HILIC-SPE) and preparative reversed-phase liquid chromatography (prep-RPLC) was developed to purify GA with high purity from the complex licorice extract. Via evaluation of retention behavior of GA and flavonoids in different commercially available columns, a hydrophilic column--Click XIon was finally chosen for the purification due to its excellent resolution toward GA and flavonoids under HILIC mode. To optimize the SPE elution conditions, relative factors including water content, pH and ionic strength had been investigated in chromatographic condition. The result indicated that the most appropriate water content was 30% and pH at 4.00, as well as salt concentration should be controlled at 5mM. In addition, the optimization revealed that GA experiences both hydrophilic interaction and ion-exchange interaction on the Click XIon material. According to the chromatographic evaluation, the optimized conditions were applied to HILIC-SPE to enrich GA from licorice, which leads to an increased content of GA from 13.67% to 64.22%. Finally, prep-RPLC was performed to obtain GA with purity higher than 99.00%,which demonstrating great prospect in large-scale preparation of GA.

  9. A method for high purity intestinal epithelial cell culture from adult human and murine tissues for the investigation of innate immune function.

    PubMed

    Graves, Christina L; Harden, Scott W; LaPato, Melissa; Nelson, Michael; Amador, Byron; Sorenson, Heather; Frazier, Charles J; Wallet, Shannon M

    2014-12-01

    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.

  10. Microfluidic device with integrated microfilter of conical-shaped holes for high efficiency and high purity capture of circulating tumor cells.

    PubMed

    Tang, Yadong; Shi, Jian; Li, Sisi; Wang, Li; Cayre, Yvon E; Chen, Yong

    2014-08-13

    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.

  11. 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.

  12. Influence of impurity elements on the nucleation and growth of Si in high purity melt-spun Al-Si-based alloys

    NASA Astrophysics Data System (ADS)

    Li, J. H.; Zarif, M. Z.; Dehm, G.; Schumacher, P.

    2012-11-01

    The nucleation and growth of Si has been investigated by TEM in a series of high purity melt spun Al-5Si (wt%)-based alloys with a trace addition of Fe and Sr. In the as-melt-spun condition, some twinned Si particles were found to form directly from the liquid along the grain boundary. The addition of Sr into Al-5Si-based alloys promotes the twinning of Si particles on the grain boundary and the formation of Si precipitates in the α-Al matrix. The majority of plate-shaped and truncated pyramid-shaped Si precipitates were also found to nucleate and grow along {111}α-Al planes from supersaturated solid solution in the α-Al matrix. In contrast, controlled slow cooling decreased the amount of Si precipitates, while the size of the Si precipitates increased. The orientation relationship between these Si precipitates and the α-Al matrix still remained cube to cube. The β-Al5FeSi intermetallic was also observed, depending on subsequent controlled cooling.

  13. 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.

  14. 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.

  15. Separation of high-purity syringol and acetosyringone from rice straw-derived bio-oil by combining the basification-acidification process and column chromatography.

    PubMed

    Hao, Shilai; Chen, Kaifei; Cao, Leichang; Zhu, Xiangdong; Luo, Gang; Zhang, Shicheng; Chen, Jianmin

    2016-10-01

    Numerous technologies have been used to reclaim valuable chemicals from bio-oil. In this study, a combination of the basification-acidification process and column chromatography was employed for the separation of high-purity syringol and acetosyringone from rice straw-derived bio-oil. The optimal conditions for the basification-acidification process and the possible precipitation mechanism of the basification were explored. The results showed the following as the optimal conditions for the basification process: mass ratio of calcium hydroxide (Ca(OH)2 ) to bio-oil, 2.0; reaction temperature, 70°C; and reaction time, 30 min. The results also showed that 1.6 mol of hydrochloric acid (HCl) per gram of bio-oil was optimal for the acidification. The precipitation was found to proceed via a possible mechanism involving the reaction of the phenolic compounds in the bio-oil with Ca(OH)2 to produce a precipitate. After further separation by column chromatography, purities of 91.4 and 96.2% (from gas chromatography-mass spectrometry) were obtained for syringol and acetosyringone, respectively. Their recoveries for the whole process were 73.0 and 39.3%, respectively.

  16. 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.

  17. Mechanical Properties of Zirconium Ceramics with Hierarchical Porous Structure

    NASA Astrophysics Data System (ADS)

    Kulkov, S.; Shutilova, E.; Buyakova, S.

    2016-07-01

    The work studies porous ceramics produced from ultra-fine powders. The porosity of ceramic samples was from 15 to 80%. The ceramic materials had 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 cellular elements in a ceramic frame.

  18. 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.

  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. 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.

  1. Ceramic Material.

    DTIC Science & Technology

    1990-05-02

    A ceramic material which is (1) ceramics based on monoclinic BaO.Al2O3.2SiO2; (2) ceramics based on monoclinic SrO.Al2O3.2SiO2; or (3) ceramics based on monoclinic solid solution of BaO.Al2O3.2SiO2 and SrO.Al2O3.2SiO2.

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. 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.

  9. Green nanochemistry: metal oxide nanoparticles and porous thin films from bare metal powders.

    PubMed

    Redel, Engelbert; Petrov, Srebri; Dag, Omer; Moir, Jonathon; Huai, Chen; Mirtchev, Peter; Ozin, Geoffrey A

    2012-01-09

    A universal, simple, robust, widely applicable and cost-effective aqueous process is described for a controlled oxidative dissolution process of micrometer-sized metal powders to form high-purity aqueous dispersions of colloidally stable 3-8 nm metal oxide nanoparticles. Their utilization for making single and multilayer optically transparent high-surface-area nanoporous films is demonstrated. This facile synthesis is anticipated to find numerous applications in materials science, engineering, and nanomedicine.

  10. 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.

  11. Neutron Damage in Mechanically-Cooled High-Purity Germanium Detectors for Field-Portable Prompt Gamma Neutron Activation Analysis (PGNAA) Systems

    SciTech Connect

    E.H. Seabury; C.J. Wharton; A.J. Caffrey; J.B. McCabe; C. DeW. Van Siclen

    2013-10-01

    Prompt Gamma Neutron Activation (PGNAA) systems require the use of a gamma-ray spectrometer to record the gamma-ray spectrum of an object under test and allow the determination of the object’s composition. Field-portable systems, such as Idaho National Laboratory’s PINS system, have used standard liquid-nitrogen-cooled high-purity germanium (HPGe) detectors to perform this function. These detectors have performed very well in the past, but the requirement of liquid-nitrogen cooling limits their use to areas where liquid nitrogen is readily available or produced on-site. Also, having a relatively large volume of liquid nitrogen close to the detector can impact some assessments, possibly leading to a false detection of explosives or other nitrogen-containing chemical. Use of a mechanically-cooled HPGe detector is therefore very attractive for PGNAA applications where nitrogen detection is critical or where liquid-nitrogen logistics are problematic. Mechanically-cooled HPGe detectors constructed from p-type germanium, such as Ortec’s trans-SPEC, have been commercially available for several years. In order to assess whether these detectors would be suitable for use in a fielded PGNAA system, Idaho National Laboratory (INL) has been performing a number of tests of the resistance of mechanically-cooled HPGe detectors to neutron damage. These detectors have been standard commercially-available p-type HPGe detectors as well as prototype n-type HPGe detectors. These tests compare the performance of these different detector types as a function of crystal temperature and incident neutron fluence on the crystal.

  12. High temperature annealing effects on deep-level defects in a high purity semi-insulating 4H-SiC substrate

    NASA Astrophysics Data System (ADS)

    Iwamoto, Naoya; Azarov, Alexander; Ohshima, Takeshi; Moe, Anne Marie M.; Svensson, Bengt G.

    2015-07-01

    Effects of high-temperature annealing on deep-level defects in a high-purity semi-insulating 4H silicon carbide substrate have been studied by employing current-voltage, capacitance-voltage, junction spectroscopy, and chemical impurity analysis measurements. Secondary ion mass spectrometry data reveal that the substrate contains boron with concentration in the mid 1015 cm-3 range, while other impurities including nitrogen, aluminum, titanium, vanadium and chromium are below their detection limits (typically ˜1014 cm-3). Schottky barrier diodes fabricated on substrates annealed at 1400-1700 °C exhibit metal/p-type semiconductor behavior with a current rectification of up to 8 orders of magnitude at bias voltages of ±3 V. With increasing annealing temperature, the series resistance of the Schottky barrier diodes decreases, and the net acceptor concentration in the substrates increases approaching the chemical boron content. Admittance spectroscopy results unveil the presence of shallow boron acceptors and deep-level defects with levels in lower half of the bandgap. After the 1400 °C annealing, the boron acceptor still remains strongly compensated at room temperature by deep donor-like levels located close to mid-gap. However, the latter decrease in concentration with increasing annealing temperature and after 1700 °C, the boron acceptor is essentially uncompensated. Hence, the deep donors are decisive for the semi-insulating properties of the substrates, and their thermal evolution limits the thermal budget for device processing. The origin of the deep donors is not well-established, but substantial evidence supporting an assignment to carbon vacancies is presented.

  13. High temperature annealing effects on deep-level defects in a high purity semi-insulating 4H-SiC substrate

    SciTech Connect

    Iwamoto, Naoya Azarov, Alexander; Svensson, Bengt G.; Ohshima, Takeshi; Moe, Anne Marie M.

    2015-07-28

    Effects of high-temperature annealing on deep-level defects in a high-purity semi-insulating 4H silicon carbide substrate have been studied by employing current-voltage, capacitance-voltage, junction spectroscopy, and chemical impurity analysis measurements. Secondary ion mass spectrometry data reveal that the substrate contains boron with concentration in the mid 10{sup 15 }cm{sup −3} range, while other impurities including nitrogen, aluminum, titanium, vanadium and chromium are below their detection limits (typically ∼10{sup 14 }cm{sup −3}). Schottky barrier diodes fabricated on substrates annealed at 1400–1700 °C exhibit metal/p-type semiconductor behavior with a current rectification of up to 8 orders of magnitude at bias voltages of ±3 V. With increasing annealing temperature, the series resistance of the Schottky barrier diodes decreases, and the net acceptor concentration in the substrates increases approaching the chemical boron content. Admittance spectroscopy results unveil the presence of shallow boron acceptors and deep-level defects with levels in lower half of the bandgap. After the 1400 °C annealing, the boron acceptor still remains strongly compensated at room temperature by deep donor-like levels located close to mid-gap. However, the latter decrease in concentration with increasing annealing temperature and after 1700 °C, the boron acceptor is essentially uncompensated. Hence, the deep donors are decisive for the semi-insulating properties of the substrates, and their thermal evolution limits the thermal budget for device processing. The origin of the deep donors is not well-established, but substantial evidence supporting an assignment to carbon vacancies is presented.

  14. Diagnostics method for the rapid quantitative detection and identification of low-level contamination of high-purity water with pathogenic bacteria.

    PubMed

    Minogue, Elizabeth; Reddington, Kate; Dorai-Raj, Siobhan; Tuite, Nina; Clancy, Eoin; Barry, Thomas

    2013-09-01

    High-purity water (HPW) can be contaminated with pathogenic microorganisms, which may result in human infection. Current culture-based techniques for the detection of microorganisms from HPW can be slow and laborious. The aim of this study was to develop a rapid method for the quantitative detection and identification of pathogenic bacteria causing low-level contamination of HPW. A novel internally controlled multiplex real-time PCR diagnostics assay was designed and optimized to specifically detect and identify Pseudomonas aeruginosa and the Burkholderia genus. Sterile HPW, spiked with a bacterial load ranging from 10 to 10(3) cfu/100 ml, was filtered and the bacterial cells were removed from the filters by sonication. Total genomic DNA was then purified from these bacteria and subjected to testing with the developed novel multiplex real-time PCR diagnostics assay. The specific P. aeruginosa and Burkholderia genus assays have an analytical sensitivity of 3.5 genome equivalents (GE) and 3.7 GE, respectively. This analysis demonstrated that it was possible to detect a spiked bacterial load of 1.06 × 10(2) cfu/100 ml for P. aeruginosa and 2.66 × 10(2) cfu/100 ml for B. cepacia from a 200-ml filtered HPW sample. The rapid diagnostics method described can reliably detect, identify, and quantify low-level contamination of HPW with P. aeruginosa and the Burkholderia genus in <4 h. We propose that this rapid diagnostics method could be applied to the pharmaceutical and clinical sectors to assure the safety and quality of HPW, medical devices, and patient-care equipment.

  15. 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.

  16. Titanium diboride ceramic fiber composites for Hall-Heroult cells

    DOEpatents

    Besmann, Theodore M.; Lowden, Richard A.

    1990-01-01

    An improved cathode structure 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 deg. C can be used.

  17. Photovoltaic and photostrictive effects in lanthanum-modified lead zirconate titanate ceramics

    NASA Astrophysics Data System (ADS)

    Poosanaas, Patcharin

    Photostriction is the light induced strain in a material, arising from the combination of photovoltaic and converse-piezoelectric effects. The possibility of directly producing strain by light illumination, without any electrical lead wire connection, makes the photostrictive materials very attractive for potential usage in future generation wireless remote controlled micro-actuator and micro-sensor. However, for the fabrication of these devices, materials exhibiting higher photovoltaic effect and higher response speed must be developed. This research was aimed towards investigating the mechanism of photovoltaic effect, developing photostrictive materials with enhanced performance, and exploring the limits of the photostriction. A new model based on the optical nonlinearity in ferroelectrics having noncentric symmetry has been proposed to explain the mechanism of photovoltaic effect. This model provides a better understanding of photostrictive phenomenon and agrees well with the experimental measurements carried out on PLZT ceramics. Among the various processing routes attempted, coprecipitation route was found to be most suitable for the fabrication of PLZT ceramics. High purity homogeneous powders with stoichiometric compositions obtained from this method yielded compacts with high density, fine grain size and uniformly distributed dopants. These desirable properties resulted in enhancement of photostrictive response. Photovoltaic and photoinduced strain were found to increase with decreasing grain size and increasing relative density. The composition, especially near the morphotropic phase boundary (MPB) of PLZT ceramics, was optimized for photovoltaic characteristics. The maximum photocurrent was observed in tetragonal phase 4/48/52 PLZT, while the maximum photovoltage was observed in 5/54/46 PLZT, which is around the MPB of the PLZT phase diagram. The photostriction was found to be strongly influenced by the surface characteristics (namely, sample thickness

  18. Evaluation of occupational exposure to naturally occurring radioactive materials in the Iranian ceramics industry.

    PubMed

    Fathabadi, N; Farahani, M V; Amani, S; Moradi, M; Haddadi, B

    2011-06-01

    Zircon contains small amounts of uranium, thorium and radium in its crystalline structure. The ceramic industry is one of the major consumers of zirconium compounds that are used as an ingredient at ∼10-20 % by weight in glaze. In this study, seven different ceramic factories have been investigated regarding the presence of radioactive elements with focus on natural radioactivity. The overall objective of this investigation is to provide information regarding the radiation exposure to workers in the ceramic industry due to naturally occurring radioactive materials. This objective is met by collecting existing radiological data specific to glaze production and generating new data from sampling activities. The sampling effort involves the whole process of glaze production. External exposures are monitored using a portable gamma-ray spectrometer and environmental thermoluminescence dosimeters, by placing them for 6 months in some workplaces. Internal routes of exposure (mainly inhalation) are studied using air sampling, and gross alpha and beta counting. Measurement of radon gas and its progeny is performed by continuous radon gas monitors that use pulse ionisation chambers. Natural radioactivity due to the presence of ²³⁸U, ²³²Th and ⁴⁰K in zirconium compounds, glazes and other samples is measured by a gamma-ray spectrometry system with a high-purity germanium detector. The average concentrations of ²³⁸U and ²³²Th observed in the zirconium compounds are >3300 and >550 Bq kg⁻¹, respectively. The specific activities of other samples are much lower than in zirconium compounds. The annual effective dose from external radiation had a mean value of ∼0.13 mSv y⁻¹. Dust sampling revealed the greatest values in the process at the powdering site and hand weighing places. In these plants, the annual average effective dose from inhalation of long-lived airborne radionuclides was 0.226 mSv. ²²²Rn gas concentrations in the glaze production plant and

  19. Sub-band gap photo-enhanced secondary electron emission from high-purity single-crystal chemical-vapor-deposited diamond

    NASA Astrophysics Data System (ADS)

    Yater, J. E.; Shaw, J. L.; Pate, B. B.; Feygelson, T. I.

    2016-02-01

    Secondary-electron-emission (SEE) current measured from high-purity, single-crystal (100) chemical-vapor-deposited diamond is found to increase when sub-band gap (3.06 eV) photons are incident on the hydrogenated surface. Although the light does not produce photoemission directly, the SEE current increases by more than a factor of 2 before saturating with increasing laser power. In energy distribution curves (EDCs), the emission peak shows a corresponding increase in intensity with increasing laser power. However, the emission-onset energy in the EDCs remains constant, indicating that the bands are pinned at the surface. On the other hand, changes are observed on the high-energy side of the distribution as the laser power increases, with a well-defined shoulder becoming more pronounced. From an analysis of this feature in the EDCs, it is deduced that upward band bending is present in the near-surface region during the SEE measurements and this band bending suppresses the SEE yield. However, sub-band gap photon illumination reduces the band bending and thereby increases the SEE current. Because the bands are pinned at the surface, we conclude that the changes in the band levels occur below the surface in the electron transport region. Sample heating produces similar effects as observed with sub-band gap photon illumination, namely, an increase in SEE current and a reduction in band bending. However, the upward band bending is not fully removed by either increasing laser power or temperature, and a minimum band bending of ˜0.8 eV is established in both cases. The sub-band gap photo-excitation mechanism is under further investigation, although it appears likely at present that defect or gap states play a role in the photo-enhanced SEE process. In the meantime, the study demonstrates the ability of visible light to modify the electronic properties of diamond and enhance the emission capabilities, which may have potential impact for diamond-based vacuum electron

  20. Couples Magnetic and Structural Transitions in High-Purity Dy and Gd5SbxGe4-x

    SciTech Connect

    Chernyshov, Alexander S.

    2006-01-01

    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 ~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 Gd5SbxGe4-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

  1. The effect of environment on the creep deformation of ultra-high purity nickel-chromium-iron alloys at 360 degrees Celcius

    NASA Astrophysics Data System (ADS)

    Paraventi, Denise Jean

    2000-10-01

    Steam generators in pressurized water nuclear power plants have experienced significant problems with intergranular stress corrosion cracking (IGSCC) on the inner diameter of steam generator tubing for over 25 years. In the course of research to understand IGSCC, it has been shown that creep deformation may play a significant role in the cracking of commercial Alloy 600 (Ni-16Cr-9Fe-0.03C). The primary water environment can cause decreases in creep resistance (i.e., faster creep rates, shorter time to failure, and higher creep strains). During corrosion under the conditions of interest, both hydrogen reduction and metal dissolution occur. One or both may contribute to the enhancement of creep. The purpose of this work was to isolate the mechanism by which the water environment causes the creep deformation to increase. Activation area and activation enthalpy for glide were measured in argon and primary water on high purity Ni-16Cr-9Fe alloys. The results indicated that the activation area was reduced by primary water, consistent with a hydrogen enhanced plasticity mechanism for enhanced creep. The stress dependence of creep was also examined in argon and primary water. The results indicated that the internal stress of the alloy is reduced by the primary water environment. Lower internal stress is consistent with both a hydrogen model as well as a vacancy-aided climb model for enhanced creep. To isolate the effect of hydrogen on the creep of the alloy, experiments were conducted in a dissociated hydrogen environment. The results indicated that hydrogen would only increase the steady state creep rate if present before loading of the samples. However, if the sample was already in steady state creep and hydrogen introduced, a transient in the creep strain was observed. The creep rate returned to the original steady state rate in a short time. The results indicate that while hydrogen does affect the steady state creep to an extent, hydrogen cannot completely account for

  2. Sub-band gap photo-enhanced secondary electron emission from high-purity single-crystal chemical-vapor-deposited diamond

    SciTech Connect

    Yater, J. E. Shaw, J. L.; Pate, B. B.; Feygelson, T. I.

    2016-02-07

    Secondary-electron-emission (SEE) current measured from high-purity, single-crystal (100) chemical-vapor-deposited diamond is found to increase when sub-band gap (3.06 eV) photons are incident on the hydrogenated surface. Although the light does not produce photoemission directly, the SEE current increases by more than a factor of 2 before saturating with increasing laser power. In energy distribution curves (EDCs), the emission peak shows a corresponding increase in intensity with increasing laser power. However, the emission-onset energy in the EDCs remains constant, indicating that the bands are pinned at the surface. On the other hand, changes are observed on the high-energy side of the distribution as the laser power increases, with a well-defined shoulder becoming more pronounced. From an analysis of this feature in the EDCs, it is deduced that upward band bending is present in the near-surface region during the SEE measurements and this band bending suppresses the SEE yield. However, sub-band gap photon illumination reduces the band bending and thereby increases the SEE current. Because the bands are pinned at the surface, we conclude that the changes in the band levels occur below the surface in the electron transport region. Sample heating produces similar effects as observed with sub-band gap photon illumination, namely, an increase in SEE current and a reduction in band bending. However, the upward band bending is not fully removed by either increasing laser power or temperature, and a minimum band bending of ∼0.8 eV is established in both cases. The sub-band gap photo-excitation mechanism is under further investigation, although it appears likely at present that defect or gap states play a role in the photo-enhanced SEE process. In the meantime, the study demonstrates the ability of visible light to modify the electronic properties of diamond and enhance the emission capabilities, which may have potential impact for diamond-based vacuum electron

  3. Dynamic Compaction of Metal and Ceramic Powders

    DTIC Science & Technology

    1983-03-01

    Electric Company; Derek Raybould , Institute Cerac, Ecublens, Switzerland; Robert A. Graham, Sandia Laboratories; Gordon A. Bruggeman, U.S. Army...not extensive for porous or distended materials although some constitutive models have been developed (Herman 1969, Raybould 1981, Roman and...between 100 and 2000 m/sec ( Raybould 1980). With special techniques, velocities as low as 20 m/sec have been routinely achieved (Graham 1977

  4. Ceramic joining

    SciTech Connect

    Loehman, R.E.

    1996-04-01

    This paper describes the relation between reactions at ceramic-metal interfaces and the development of strong interfacial bonds in ceramic joining. Studies on a number of systems are described, including silicon nitrides, aluminium nitrides, mullite, and aluminium oxides. Joints can be weakened by stresses such as thermal expansion mismatch. Ceramic joining is used in a variety of applications such as solid oxide fuel cells.

  5. Ceramic Processing

    SciTech Connect

    EWSUK,KEVIN G.

    1999-11-24

    Ceramics represent a unique class of materials that are distinguished from common metals and plastics by their: (1) high hardness, stiffness, and good wear properties (i.e., abrasion resistance); (2) ability to withstand high temperatures (i.e., refractoriness); (3) chemical durability; and (4) electrical properties that allow them to be electrical insulators, semiconductors, or ionic conductors. Ceramics can be broken down into two general categories, traditional and advanced ceramics. Traditional ceramics include common household products such as clay pots, tiles, pipe, and bricks, porcelain china, sinks, and electrical insulators, and thermally insulating refractory bricks for ovens and fireplaces. Advanced ceramics, also referred to as ''high-tech'' ceramics, include products such as spark plug bodies, piston rings, catalyst supports, and water pump seals for automobiles, thermally insulating tiles for the space shuttle, sodium vapor lamp tubes in streetlights, and the capacitors, resistors, transducers, and varistors in the solid-state electronics we use daily. The major differences between traditional and advanced ceramics are in the processing tolerances and cost. Traditional ceramics are manufactured with inexpensive raw materials, are relatively tolerant of minor process deviations, and are relatively inexpensive. Advanced ceramics are typically made with more refined raw materials and processing to optimize a given property or combination of properties (e.g., mechanical, electrical, dielectric, optical, thermal, physical, and/or magnetic) for a given application. Advanced ceramics generally have improved performance and reliability over traditional ceramics, but are typically more expensive. Additionally, advanced ceramics are typically more sensitive to the chemical and physical defects present in the starting raw materials, or those that are introduced during manufacturing.

  6. Ceramic filters

    SciTech Connect

    Holmes, B.L.; Janney, M.A.

    1995-12-31

    Filters were formed from ceramic fibers, organic fibers, and a ceramic bond phase using a papermaking technique. The distribution of particulate ceramic bond phase was determined using a model silicon carbide system. As the ceramic fiber increased in length and diameter the distance between particles decreased. The calculated number of particles per area showed good agreement with the observed value. After firing, the papers were characterized using a biaxial load test. The strength of papers was proportional to the amount of bond phase included in the paper. All samples exhibited strain-tolerant behavior.

  7. Joining of ceramics for advanced heavy-duty diesels

    SciTech Connect

    Moorhead, A.J.; Keating, H.

    1986-03-01

    The wettability and adherence in vacuum of a series of metal alloys on several oxide ceramics were investigated with the goal of identifying those compositions suitable as filler metals for direct brazing of ceramics in uncooled diesel engine applications. Wetting behavior was determined by the sessile-drop technique. Adherence was measured by several tests including sessile-drop shear, flexure strength of ceramics brazed in a butt-joint configuration, fracture toughness using a composite double cantilever beam specimen, and, in the case of ceramic-metal brazements, by a bar/pad shear test. Compositions were identified in both the Cu-Ag-Ti and Cu-Au-Ti ternary systems that wet and strongly adhered to high-purity aluminas, partially stabilized zirconia ceramics, and alumina reinforced with SiC whiskers. Excellent flexural strengths, at temperatures up to 600/sup 0/C, of brazements containing these filler metals indicate that these materials are good candidates for use in advanced heavy-duty diesel engines. They have the advantage over competing systems of not requiring that the ceramic be metallized before brazing.

  8. Ceramics containing dispersants for improved fracture toughness

    DOEpatents

    Nevitt, Michael V.; Aldred, Anthony T.; Chan, Sai-Kit

    1987-01-01

    The invention is a ceramic composition containing a new class of dispersant for hindering crack propagation by means of one or more energy-dissipative mechanisms. The composition is composed of a ceramic matrix with dispersed particles of a transformation-prone rare-earth niobate, tantalate or mixtures of these with each other and/or with a rare-earth vanadate. The dispersants, having a generic composition tRMO.sub.4, where R is a rare-earth element, B is Nb or Ta and O is oxygen, are mixed in powder form with a powder of the matrix ceramic and sintered to produce a ceramic form or body. The crack-hindering mechanisms operates to provide improved performance over a wide range of temperature and operating conditions.

  9. Ceramics containing dispersants for improved fracture toughness

    DOEpatents

    Nevitt, Michael V.; Aldred, Anthony T.; Chan, Sai-Kit

    1987-07-07

    The invention is a ceramic composition containing a new class of dispersant for hindering crack propagation by means of one or more energy-dissipative mechanisms. The composition is composed of a ceramic matrix with dispersed particles of a transformation-prone rare-earth niobate, tantalate or mixtures of these with each other and/or with a rare-earth vanadate. The dispersants, having a generic composition tRMO.sub.4, where R is a rare-earth element, B is Nb or Ta and O is oxygen, are mixed in powder form with a powder of the matrix ceramic and sintered to produce a ceramic form or body. The crack-hindering mechanisms operates to provide improved performance over a wide range of temperature and operating conditions.

  10. Method of making contamination-free ceramic bodies

    NASA Technical Reports Server (NTRS)

    Philipp, Warren H. (Inventor)

    1991-01-01

    Ceramic structures having high strength at temperatures above 1000 C after sintering are made by mixing ceramic powders with binder deflocculants such as guanidine salts of polymeric acids, guanidine salts of aliphatic organic carboxylic acids or guanidine alkylsulfates with the foregoing guanidine salts. The novelty of the invention appears to lie in the substitution of guanidine salts for the alkalai metal salt components or organic fatty acids of the prior art binder-deflocculant, ceramic processing aids whereby no undesirable metal contaminants are present in the final ceramic structure. Guanidine alkylsulfates also replace the Na or K alkylsulfates commonly used with binder-deflocculants in making high temperature ceramic structures.

  11. Dispersed metal-toughened ceramics and ceramic brazing

    SciTech Connect

    Moorhead, A.J.; Tiegs, T.N.; Lauf, R.J.

    1983-01-01

    An alumina (Al/sub 2/O/sub 3/) based material that contains approximately 1 vol % finely dispersed platinum or chromium was developed for use in high temperature thermal-shock resistant electrical insulators. The work at ORNL is divided into two areas: (1) development of DMT ceramics; and (2) development of brazing filler metals suitable for making ceramic-to-ceramic and ceramic-to-metal brazements. The DMT ceramics and brazements are intended for service at elevated temperatures and at high stress levels in the dirty environments of advanced heat engines. The development and characterization of DMT ceramics includes processing (powder preparation, densification and heat treatment) and detailed measurement of mechanical and physical properties (strength, fracture toughness, and thermal conductivity). The brazing work includes: (1) the formulation and melting of small quantities of experimental brazing filler metals; (2) evaluation of the wetting and bonding behavior of these filler metals on Al/sub 2/O/sub 3/, partially stabilized zirconia and ..cap alpha..-SiC in a sessile drop apparatus; and (3) determine the short-term strength and fracture toughness of brazements.

  12. Sol-Gel Synthesis Of Aluminoborosilicate Powders

    NASA Technical Reports Server (NTRS)

    Bull, Jeffrey; Leiser, Daniel; Selvaduray, Guna

    1992-01-01

    Application of sol-gel process to synthesis of aluminoborosilicate powders shows potential for control of microstructures of materials. Development of materials having enhanced processing characteristics prove advantageous in extending high-temperature endurance of fibrous refractory composite insulation made from ceramic fibers.

  13. Analysis of Rare Earth Elements (REE) in vein quartz and quartz-sandstone host rock in the Zhelannoe high purity quartz deposit, Russia

    NASA Astrophysics Data System (ADS)

    Zemskova, Marina; Prokofiev, Vsevolod; Bychkov, Andrey

    2015-04-01

    The Zhelannoe high purity quartz deposit is located on the western slope of the Polar Urals. It is one of the largest deposits of vein quartz and rock crystal in Russia. Most of the mineralization is hosted within a single horizon of very firm quartz-sandstone, where plastic deformation did not occur almost entirely. All tectonic stress was released by the development of numerous thrust faults of different scales. Cavities formed during this process were later filled with quartz and rock crystal. In order to obtain more details on conditions under which mineralization took place, analysis of trace element contents in vein quartz and host rocks, and the micro-thermometric study of fluid inclusions in quartz have been carried out. The trace element composition of vein quartz and of the host rock has been determined by ICP-MS. The results have shown that concentrations of most of the 46 studied elements in quartz are two orders of magnitude lower than in chondrite, and more than three orders of magnitude lower than in the upper crust. Even though Pb and Li have the highest concentrations in quartz samples, levels are only nearly comparable in chondrite, and substantially lower in the upper crust. At the same time, negative anomalies of Pb and Li concentrations in the host rock may indicate the removal of these elements during vein quartz formation. Contents of most REEs are two orders of magnitude lower than in chondrite, and three orders of magnitude lower than in the host rock. Generally, the patterns of REE distribution in vein quartz and the host rock express a clear correlation; confirming the genetic link between vein quartz and quartz-sandstone host rock. However, the process of quartz recrystallization led to an intense decrease of REEs content, and of all other impurities, which consequently influenced industrial value of the Zhelannoe deposit. As a result of the micro-thermometric study of fluid inclusions in quartz, the following physical

  14. [Separation with ion exchange fiber column and determination of La, Nd, Eu and Gd in high purity ytterbium oxide by ICP-AES].

    PubMed

    Gong, Qi; Chen, Jie; Ji, Ri-Wen; Pan, Xue-Zhen; Wu, Juan

    2010-02-01

    In the present paper, trace La, Nd, Eu and Gd were separated and enriched with strong acid ion exchange fiber column from high purity Yb2 O3, and then determined by Optima 5 300 DV ICP-AES. The ion exchange fiber's breakthrough capacity for Yb was 134 mg x g(-1). The separation condition using 4.0 g fiber column was that after the test solution (pH = 3.0) was fed into the ion exchange fiber column at 1.0 mL x min(-1), the column was pre--leached by dilute nitric acid (pH = 3.00) of 80 mL at 1.5 mL x min(-1) at first, and then was eluted by 0.01 mol x L(-1) ammonium EDTA (pH = 5.00) at the same flow rate. The results showed that 10 mg Yb could reach the baseline separation with 0.100 microg of the four rare earth impurities, and after 100 mg Yb in feed solution had been separated, only 0.017 1 microg x mL(-1) Yb remained in the impurities enriched effluent. When the concentration of Yb2 O3 is less than 100 microg x mL(-1) (87.8 microg x mL(-1) Yb), the matrix interference from Yb on with determination of La, Nd, Eu and Gd can be neglected. The enrichment factors were 3.68 x 10(5) for La2 O3, 4.20 x 10(5) for Nds O3, 3.82 x 10(5) for Eu2 O3, and 4.01 x 10(5) for Gd2 O3, and the detection limits of the method were 0.005 0, 0.014, 0.001 8 and 0.008 2 pg x mL(-1) for La2 O3, Nd2 O3, Eu2 O3 and Gd2 O3 respectively. The proposed method was applied to the analysis of 99.99% Yb2 O3 with RSD (%, n = 5) of 6.2, 5.9, 7.3 and 2.5 for La2 O3, Nd2 O3, Eu2 O3 and Gd2 O3 respectively, and the average recoveries of standard addition were 94.2%, 107%, 97.8% and 102% for La2 O3, Nd2 O3, Eu2 O3 and Gd2 O3 respectively. The calibration curve did not need matrix matching with Yb, and the analysis period was within 4 hour.

  15. Fabrication of transparent ceramics using nanoparticles

    DOEpatents

    Cherepy, Nerine J; Tillotson, Thomas M; Kuntz, Joshua D; Payne, Stephen A

    2012-09-18

    A method of fabrication of a transparent ceramic using nanoparticles synthesized via organic acid complexation-combustion includes providing metal salts, dissolving said metal salts to produce an aqueous salt solution, adding an organic chelating agent to produce a complexed-metal sol, heating said complexed-metal sol to produce a gel, drying said gel to produce a powder, combusting said powder to produce nano-particles, calcining said nano-particles to produce oxide nano-particles, forming said oxide nano-particles into a green body, and sintering said green body to produce the transparent ceramic.

  16. Ceramic fiber reinforced glass-ceramic matrix composite

    NASA Technical Reports Server (NTRS)

    Bansal, Narottam P. (Inventor)

    1993-01-01

    A slurry of BSAS glass powders is cast into tapes which are cut to predetermined sizes. Mats of continuous chemical vapor deposition (CVD)-SiC fibers are alternately stacked with these matrix tapes. This tape-mat stack is warm-pressed to produce a 'green' composite which is heated to burn out organic constituents. The remaining interim material is then hot-pressed to form a BSAS glass-ceramic fiber-reinforced composite.

  17. Nanostructured Ceramics Obtained Under Extreme Conditions of Pressure and Temperature

    DTIC Science & Technology

    2011-11-20

    nanostructured organic-inorganic ceramic materials using the sol - gel method combined with high-pressure technique to produce ceramics with multifnctional...by the midle of 2012. several works were already published on this matter and some were presented in International Meetings. alumina, sol - gel ... sol - gel synthesis to produced nanocomposites powders of both ceramics: alumina and zirconia. In order to do that, several surfactants were

  18. Method of making multilayered titanium ceramic composites

    DOEpatents

    Fisher, II, George T.; Hansen, Jeffrey S.; Oden, Laurance L.; Turner, Paul C.; Ochs, Thomas L.

    1998-01-01

    A method making a titanium ceramic composite involves forming a hot pressed powder body having a microstructure comprising at least one titanium metal or alloy layer and at least one ceramic particulate reinforced titanium metal or alloy layer and hot forging the hot pressed body follwed by hot rolling to substantially reduce a thickness dimension and substantially increase a lateral dimension thereof to form a composite plate or sheet that retains in the microstructure at least one titanium based layer and at least one ceramic reinforced titanium based layer in the thickness direction of the composite plate or sheet.

  19. Method of making multilayered titanium ceramic composites

    DOEpatents

    Fisher, G.T. II; Hansen, J.S.; Oden, L.L.; Turner, P.C.; Ochs, T.L.

    1998-08-25

    A method making a titanium ceramic composite involves forming a hot pressed powder body having a microstructure comprising at least one titanium metal or alloy layer and at least one ceramic particulate reinforced titanium metal or alloy layer and hot forging the hot pressed body followed by hot rolling to substantially reduce a thickness dimension and substantially increase a lateral dimension thereof to form a composite plate or sheet that retains in the microstructure at least one titanium based layer and at least one ceramic reinforced titanium based layer in the thickness direction of the composite plate or sheet. 3 figs.

  20. Method of making multilayered titanium ceramic composites

    DOEpatents

    Fisher, George T., II; Hansen; Jeffrey S.; Oden; Laurance L.; Turner; Paul C.; Ochs; Thomas L.

    1998-08-25

    A method making a titanium ceramic composite involves forming a hot pressed powder body having a microstructure comprising at least one titanium metal or alloy layer and at least one ceramic particulate reinforced titanium metal or alloy layer and hot forging the hot pressed body follwed by hot rolling to substantially reduce a thickness dimension and substantially increase a lateral dimension thereof to form a composite plate or sheet that retains in the microstructure at least one titanium based layer and at least one ceramic reinforced titanium based layer in the thickness direction of the composite plate or sheet.

  1. [Preparation of porous ceramics based on waste ceramics and its Ni2+ adsorption characteristics].

    PubMed

    Zhang, Yong-Li; Wang, Cheng-Zhi; Shi, Ce; Shang, Ling-Ling; Ma, Rui; Dong, Wan-Li

    2013-07-01

    The preparation conditions of porous ceramics were determined by SEM, XRD and FT-IR characterizations as well as the nickel removal ability of porous ceramics to be: the mass fraction w of sesbania powder doped was 4%, and the calcination temperature was 800 degrees C. SEM and pore structure characterization illustrated that calcination caused changes in the structure and morphology of waste ceramics. With the increase of calcination temperature, the specific surface area and pore volume decreased, while the aperture increased. EDS analyses showed that the main elements of both the original waste porcelain powder and the porous ceramics were Si, Al and O. The SEM, XRD and FT-IR characterization of porous ceramics illustrated that the structure of porous ceramics was stable before and after adsorption. The series of experiments of Ni2+ adsorption using these porous ceramics showed that when the dosage of porous ceramics was 10 g x L(-1), the adsorption time was 60 min, the pH value was 6.32, and the concentration of nickel-containing wastewater was below 100 mg x L(-1), the Ni2+ removal of wastewater reached 89.7%. Besides, the porous ceramics showed higher removal efficiency on nickel in the wastewater. The Ni(2+)-containing wastewater was processed by the porous ceramics prepared, and the adsorption dynamics and adsorption isotherms of Ni2+ in wastewater by porous ceramics were investigated. The research results showed that the Ni2+ adsorption process of porous ceramics was in accordance with the quasi second-order kinetic model (R2 = 0.999 9), with Q(e) of 9.09 mg x g(-1). The adsorption process can be described by the Freundlich equation and Langmuir equation, and when the temperature increased from 20 degrees C to 40 degrees C, the maximum adsorption capacity Q(m) increased from 14.49 mg x g(-1) to 15.38 mg x g(-1).

  2. Dynamic Behavior and Optimization of Advanced Armor Ceramics: January-December 2012 Annual Report

    DTIC Science & Technology

    2015-03-01

    properties. Since the rapid heating process avoids many of the negative attributes of traditional B4C synthesis , such as the presence of unreacted C...References Weimer A, Moore W, Roach R, Hitt J, Dixit R, Pratsinis S. Kinetics of carbothermal reduction synthesis of boron carbide. J Am Ceram Soc. 1992;75...9):2509. Knudsen A. Laser-driven synthesis and densification of ultrafine boron carbide powders. Advances in Ceramics: Ceramic Powder Science

  3. Thermal shock resistance ceramic insulator

    DOEpatents

    Morgan, Chester S.; Johnson, William R.

    1980-01-01

    Thermal shock resistant cermet insulators containing 0.1-20 volume % metal present as a dispersed phase. The insulators are prepared by a process comprising the steps of (a) providing a first solid phase mixture of a ceramic powder and a metal precursor; (b) heating the first solid phase mixture above the minimum decomposition temperature of the metal precursor for no longer than 30 minutes and to a temperature sufficiently above the decomposition temperature to cause the selective decomposition of the metal precursor to the metal to provide a second solid phase mixture comprising particles of ceramic having discrete metal particles adhering to their surfaces, said metal particles having a mean diameter no more than 1/2 the mean diameter of the ceramic particles, and (c) densifying the second solid phase mixture to provide a cermet insulator having 0.1-20 volume % metal present as a dispersed phase.

  4. Process for making ceramic insulation

    DOEpatents

    Akash, Akash; Balakrishnan, G. Nair

    2009-12-08

    A method is provided for producing insulation materials and insulation for high temperature applications using novel castable and powder-based ceramics. The ceramic components produced using the proposed process offers (i) a fine porosity (from nano-to micro scale); (ii) a superior strength-to-weight ratio; and (iii) flexibility in designing multilayered features offering multifunctionality which will increase the service lifetime of insulation and refractory components used in the solid oxide fuel cell, direct carbon fuel cell, furnace, metal melting, glass, chemical, paper/pulp, automobile, industrial heating, coal, and power generation industries. Further, the ceramic components made using this method may have net-shape and/or net-size advantages with minimum post machining requirements.

  5. Recent developments in glass-ceramic materials

    SciTech Connect

    Beall, G.H.

    1993-12-31

    Glass-ceramic materials can be made by sintering and crystallization of fine glass powders or by internal nucleation and crystallization of formed glass articles. In both cases, the final properties are controlled by phase assemblage and microstructure. Transparent glass-ceramics based upon ultra-fine grained {beta}-quartz solid solution have been developed with near-zero thermal expansion coefficient for a variety of consumer and technical products: cookware, stove-tops, telescope mirrors, optical gyroscopes. Fluormica glass-ceramics with a {open_quotes}house-of-cards{close_quotes} microstructure are easily machined and have found wide application in vacuum systems, precision dielectric components, insulators, and medical and dental prostheses. Acicular chain silicate glass-ceramics are strong and tough, and have recently been developed as high performance tableware and magnetic memory disk substrates. Sintered glass-ceramics based on magnesium aluminosilicate frits are the basis of copper-cordierite packaging for advanced IC packaging.

  6. Towards Development of a Super Ceramic Composite - Initial Investigation into Improvement of Strength and Toughness of Polycrystalline Ceramics

    DTIC Science & Technology

    2012-08-01

    airplanes, ships, trains, gear sets, turbines, etc. Table 1. Material properties of ceramics compared with steel and aluminum. Material Young’s...polycrystalline ceramic. The as-received powders were characterized for particle size and density. After planetary milling for various durations, the

  7. Laser synthesis of nanostructured ceramics from liquid precursors

    NASA Astrophysics Data System (ADS)

    Wilden, Johannes; Fischer, Georg

    2007-12-01

    The free-form net shape laser synthesis of nanostructured ceramics from liquid precursors enables a residual stress-free production of high temperature resistant ceramic units and components for the use in microsystem engineering. Due to the use of molecular compounded liquid, ceramic precursors the resulting ceramic components show outstanding properties, for example high purity and a nanostructured material design. The use of pulsed lasers enables a defined input of energy required to pyrolyse the precursor material into a crystalline ceramic, so the active volume can be reduced significantly compared to other processes, for example pyrolysis by furnace. In this paper several methods for a further minimization of the active volume are presented. The investigations determined different factors affecting the process. Realizing selective experiments allows a determination of their influencing level and the definition of a working area to produce three-dimensional components with high aspect ratio. By several studies, e.g., scanning electron microscopy, transmission electron microscopy as well as X-ray diffraction analysis, the atomic structure and composition of the created components were analyzed and valued, so the different reaction processes can be described extensively.

  8. Structural ceramics

    NASA Technical Reports Server (NTRS)

    Craig, Douglas F.

    1992-01-01

    This presentation gives a brief history of the field of materials sciences and goes on to expound the advantages of the fastest growing area in that field, namely ceramics. Since ceramics are moving to fill the demand for lighter, stronger, more corrosion resistant materials, advancements will rely more on processing and modeling from the atomic scale up which is made possible by advanced analytical, computer, and processing techniques. All information is presented in viewgraph format.

  9. Effects of TiCl4 Purity on the Sinterability of Armstrong-Processed Ti Powder

    SciTech Connect

    Weil, K. Scott; Hovanski, Yuri; Lavender, Curt A.

    2009-04-03

    A series of high purity and low purity powders were synthesized from TiCl4 by the Armstrong process. While both powders displayed swelling when consolidated and sintered, the lower purity powder exhibited this phenomenon in significantly lower degree. The improvement is attributed to the increase in the onset of sintering temperature, which mitigates the entrapment of volatile impurities that would otherwise lead to pore formation and growth. The net effect is that the use of a lower purity TiCl4 may beneficial in two ways: (1) it is a potentially lower cost precursor to Ti powder production and (2) the trace impurities allow higher density components to be fabricated via a typical low-cost press and sinter approach.

  10. OXYGEN TRANSPORT CERAMIC MEMBRANES

    SciTech Connect

    Dr. Sukumar Bandopadhyay; Dr. Nagendra Nagabhushana

    2001-12-01

    Conversion of natural gas to liquid fuels and chemicals is a major goal for the Nation as it enters the 21st Century. Technically robust and economically viable processes are needed to capture the value of the vast reserves of natural gas on Alaska's North Slope, and wean the Nation from dependence on foreign petroleum sources. Technologies that are emerging to fulfill this need are all based syngas as an intermediate. Syngas (a mixture of hydrogen and carbon monoxide) is a fundamental building block from which chemicals and fuels can be derived. Lower cost syngas translates directly into more cost-competitive fuels and chemicals. The currently practiced commercial technology for making syngas is either steam methane reforming (SMR) or a two-step process involving cryogenic oxygen separation followed by natural gas partial oxidation (POX). These high-energy, capital-intensive processes do not always produce syngas at a cost that makes its derivatives competitive with current petroleum-based fuels and chemicals. This project has the following 6 main 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. Task 6--Measure kinetics of oxygen uptake and transport in ceramic membrane materials under commercially relevant conditions using isotope labeling techniques.

  11. Structural Ceramics Database

    National Institute of Standards and Technology Data Gateway

    SRD 30 NIST Structural Ceramics Database (Web, free access)   The NIST Structural Ceramics Database (WebSCD) provides evaluated materials property data for a wide range of advanced ceramics known variously as structural ceramics, engineering ceramics, and fine ceramics.

  12. Ceramic/metal nanocomposites by lyophilization: Processing and HRTEM study

    SciTech Connect

    Gutierrez-Gonzalez, C.F.; Agouram, S.; Torrecillas, R.; Moya, J.S.; Lopez-Esteban, S.

    2012-02-15

    Highlights: Black-Right-Pointing-Pointer A cryogenic route has been used to obtain ceramic/metal nanostructured powders. Black-Right-Pointing-Pointer The powders present good homogeneity and dispersion of metal. Black-Right-Pointing-Pointer The metal nanoparticle size distributions are centred in 17-35 nm. Black-Right-Pointing-Pointer Both phases, ceramic and metal, present a high degree of crystallinity. Black-Right-Pointing-Pointer Good metal/ceramic interfaces due to epitaxial growth, studied by HRTEM. -- Abstract: This work describes a wet-processing route based on spray-freezing and subsequent lyophilization designed to obtain nanostructured ceramic/metal powders. Starting from the ceramic powder and the corresponding metal salt, a water-based suspension is sprayed on liquid nitrogen. The frozen powders are subsequently freeze-dried, calcined and reduced. The material was analyzed using X-ray diffraction analysis at all stages. High resolution transmission electron microscopy studies showed a uniform distribution of metal nanoparticles on the ceramic grain surfaces, good interfaces and high crystallinity, with an average metal particle size in the nanometric range.

  13. Phase Equilibria and Crystallography of Ceramic Oxides

    PubMed Central

    Wong-Ng, W.; Roth, R. S.; Vanderah, T. A.; McMurdie, H. F.

    2001-01-01

    Research in phase equilibria and crystallography has been a tradition in the Ceramics Division at National Bureau of Standards/National Institute of Standatrds and Technology (NBS/NIST) since the early thirties. In the early years, effort was concentrated in areas of Portland cement, ceramic glazes and glasses, instrument bearings, and battery materials. In the past 40 years, a large portion of the work was related to electronic materials, including ferroelectrics, piezoelectrics, ionic conductors, dielectrics, microwave dielectrics, and high-temperature superconductors. As a result of the phase equilibria studies, many new compounds have been discovered. Some of these discoveries have had a significant impact on US industry. Structure determinations of these new phases have often been carried out as a joint effort among NBS/NIST colleagues and also with outside collaborators using both single crystal and neutron and x-ray powder diffraction techniques. All phase equilibria diagrams were included in Phase Diagrams for Ceramists, which are collaborative publications between The American Ceramic Society (ACerS) and NBS/NIST. All x-ray powder diffraction patterns have been included in the Powder Diffraction File (PDF). This article gives a brief account of the history of the development of the phase equilibria and crystallographic research on ceramic oxides in the Ceramics Division. Represented systems, particularly electronic materials, are highlighted. PMID:27500068

  14. Phase Equilibria and Crystallography of Ceramic Oxides.

    PubMed

    Wong-Ng, W; Roth, R S; Vanderah, T A; McMurdie, H F

    2001-01-01

    Research in phase equilibria and crystallography has been a tradition in the Ceramics Division at National Bureau of Standards/National Institute of Standatrds and Technology (NBS/NIST) since the early thirties. In the early years, effort was concentrated in areas of Portland cement, ceramic glazes and glasses, instrument bearings, and battery materials. In the past 40 years, a large portion of the work was related to electronic materials, including ferroelectrics, piezoelectrics, ionic conductors, dielectrics, microwave dielectrics, and high-temperature superconductors. As a result of the phase equilibria studies, many new compounds have been discovered. Some of these discoveries have had a significant impact on US industry. Structure determinations of these new phases have often been carried out as a joint effort among NBS/NIST colleagues and also with outside collaborators using both single crystal and neutron and x-ray powder diffraction techniques. All phase equilibria diagrams were included in Phase Diagrams for Ceramists, which are collaborative publications between The American Ceramic Society (ACerS) and NBS/NIST. All x-ray powder diffraction patterns have been included in the Powder Diffraction File (PDF). This article gives a brief account of the history of the development of the phase equilibria and crystallographic research on ceramic oxides in the Ceramics Division. Represented systems, particularly electronic materials, are highlighted.

  15. Tailored ceramics for laser applications

    NASA Astrophysics Data System (ADS)

    Hollingsworth, Joel Philip

    Transparent ceramics have many features that recommend them over single crystals for use as laser amplifiers. Some features, such as greater mechanical toughness and an absence of extended crystalline defects, are intrinsic to polycrystalline materials. Other advantages accrue from ceramic processing: ceramics sinter more rapidly than crystals grow from a melt, at lower temperatures. Ceramic processes are more readily scaled than Czochralski growth, facilitating larger apertures. Unlike a uniform melt, a ceramic green structure can have controlled concentration gradients, resulting in a multifunctional device upon sintering. Identifying diffusion mechanisms in a suitable host material and quantifying diffusion for a dopant with appropriate energy levels are key steps toward tailoring laser ceramics to the specifications of device designers. Toward that end, this study was the first to identify the mechanism and rate of Nd diffusion in YAG. Grain boundary diffusion was shown to dominate Nd transport under conditions relevant to laser ceramics fabrication. Based on a definition of grain boundary width as 1 A, this process occurs at a rate of DGB = 6.4 x 105 +/- 2.0 x 105 exp(-491 +/- 64 kJ/(mol K))m 2/s. Mechanism identification and the first published kinetics measurement were made possible by the introduction of a heat treatment method that isolates microstructural change from dopant diffusion: the concentration of grain boundaries was kept great enough to allow rapid diffusion, but low enough to limit the driving force for coarsening. Sintering of fine-grained and phase-pure precursor powder for 4 min at 1700 °C produced 0.8 mum grains; subsequent diffusion heat treatments at up to 1650 °C for up to 64 h caused negligible coarsening, while achieving diffusion distances of up to 23 mum.

  16. Analyses of the modulatory effects of antibacterial silver doped calcium phosphate-based ceramic nano-powder on proliferation, survival, and angiogenic capacity of different mammalian cells in vitro.

    PubMed

    Bostancıoğlu, R Beklem; Peksen, Ceren; Genc, Hatice; Gürbüz, Mevlüt; Karel, Filiz Bayrakçı; Koparal, A Savas; Dogan, Aydin; Kose, Nusret; Koparal, A Tansu

    2015-08-26

    In this study, the antibacterial, cytotoxic, and angiogenic activities of silver doped calcium phosphate-based inorganic powder (ABT or PAG) were systematically investigated. ABT powders containing varying silver content were fabricated using a wet chemical manufacturing method. Antibacterial efficiencies of the ABT powders were investigated using a standard test with indicator bacteria and yeast. The cytotoxic effects of ABT on three different fibroblast cells and human umbilical vein endothelial cells (HUVECs) were assessed using MTT assay. ABT powder exhibits concentration-related cytotoxicity characteristics. Apoptotic activity, attachment capability, and wound healing effects were examined on fibroblasts. The angiogenic activity of ABT was investigated by tube formation assay in HUVECs; 10 μg ml(-1) and 100 μg ml(-1) concentrations of the highest metal ion content of ABT did not disrupt the tube formation of HUVECs. All these tests showed that ABT does not compromise the survival of the cells and might impose regeneration ability to various cell types. These results indicate that silver doped calcium phosphate-based inorganic powder with an optimal silver content has good potential for developing new biomaterials for implant applications.

  17. Development of Ceramic Systems for High temperature Coatings

    NASA Technical Reports Server (NTRS)

    Eslamloo-Grami, Maryame

    2003-01-01

    Professor Eslamloo-Grami will synthesize ceramic powders of various compositions based on pyrochlore, perovskite, and magnetoplumbite structures by doping with various oxides. Sol-gel and combustion synthesis routes will be used for powder syntheses. The powders will be characterized for particle size, surface area, microstructure, sintering etc. Thermal conductivity of the hot pressed specimens will also be measured at various temperatures. At the end, a project report will be prepared describing in details the experimental methods, results, discussion, and future research.

  18. Fundamental studies of ceramic/metal interfacial reactions at elevated temperatures.

    SciTech Connect

    McDeavitt, S. M.; Billings, G. W.; Indacochea, J. E.

    2000-12-14

    This work characterizes the interfaces resulting from exposing oxide and non-oxide ceramic substrates to zirconium metal and stainless steel-zirconium containing alloys. The ceramic/metal systems together were preheated at about 600 C and then the temperatures were increased to the test maximum temperature, which exceeded 1800 C, in an atmosphere of high purity argon. Metal samples were placed onto ceramic substrates, and the system was heated to elevated temperatures past the melting point of the metallic specimen. After a short stay at the peak temperature, the system was cooled to room temperature and examined. The chemical changes across the interface and other microstructural developments were analyzed with energy dispersive spectroscopy (EDS). This paper reports on the condition of the interfaces in the different systems studied and describes possible mechanisms influencing the microstructure.

  19. Influence of nanocrystalline boron precursor powder on superconductivity in MgB2 bulk.

    PubMed

    Zhang, Yun; Lu, Cheng; Zhou, Sihai; Joo, Jinho

    2009-12-01

    In this report, high-purity nanocrystalline boron powders processed by ball-milling were used as the precursor powders to fabricate MgB2 superconductor. The transport properties and the critical current density in the samples made from ball-milled boron powders and as-supplied boron powders were investigated. It was found that the ball-milled boron powders led to a significant enhancement of the critical current density in MgB2 sintered at 650 degrees C. The reason can be attributed to the small MgB2 grain size caused by the ball-milled boron precursor powders. The resistivity of the samples made from the ball-milled boron powder was lower than that of the sample from as-supplied boron powder. As the sintering temperature increased, both resistivity and upper critical field decreased in the samples using the ball-milled boron powders as a precursor. Poor connectivity and large strain are responsible for the high resistivity.

  20. Sol-Gel Synthesis of High-Purity Actinide Oxide ThO2 and Its Solid Solutions with Technologically Important Tin and Zinc Ions.

    PubMed

    Tripathi, Vikash Kumar; Nagarajan, Rajamani

    2016-12-19

    The applicability of epoxide-based sol-gel synthesis for actinide oxide (thoria) starting from air-stable salt, Th(NO3)4, has been examined. The homogeneous gel formed from Th(NO3)4 when calcined at 400 °C yielded nanostructured thoria, and with increasing tempeartures (600, 700, and 800 °C), the average crystallite size increased. Successful Rietveld refinement of the powder X-ray diffraction pattern of ThO2 in Fm3̅m space group was carried out with a = 5.6030(35) Å. The fingerprint vibrational mode of the fluorite structure of ThO2 was noticed as a sharp band in the Raman spectrum at 457 cm(-1). In the SEM image, a near spherical morphology of thoria was noticed. Samples showed blue emission on exciting with λ = 380 nm in the photoluminescence spectrum indicative of the presence of defects. Following this approach, 50 mol % of Sn(4+) could be substituted for Th(4+), retaining the fluorite structure as evidenced by the PXRD, Raman spectroscopy, electron microscopy, EDAX, and XPS measurements. Randomization of the lattice was observed for the tin-substituted samples. A significant blue shift in the absorption threshold along with a persistent blue emission in the photoluminesence spectra were evident for the tin-substituted samples. The concentration of Zn(2+) ion in thoria was limited to 15 mol % as revealed by PXRD and XPS measurements. The Raman peak shifted to higher values for Zn(2+)-substituted samples. A change in the optical absorbance characteristics was observed for the zinc-substituted thoria. A 50 mol % Sn(4+)-substituted thoria degraded aqueous Rhodamine 6G dye solutions in the presence of UV-vis radiation following pseudo-first-order kinetics.

  1. Structural changes during milling of aluminum oxide powders

    NASA Technical Reports Server (NTRS)

    Ziepler, G.

    1984-01-01

    The mechanical activation of four fused corundum powders and a calcined Al2O3 powder was studied. The milled powders were characterized by their structural properties, crystallite size, and lattice distortions. Structural changes during milling, detected by X-ray line broadening analysis, gave information about the enhanced activity of the powders caused by the lattice distortions and by the decreasing crystallite size during milling. The structural changes during milling, under the same milling conditions, can be quite different for the same ceramic material, but with different characteristics in the as received state.

  2. Energetic powder

    DOEpatents

    Jorgensen, Betty S.; Danen, Wayne C.

    2003-12-23

    Fluoroalkylsilane-coated metal particles. The particles have a central metal core, a buffer layer surrounding the core, and a fluoroalkylsilane layer attached to the buffer layer. The particles may be prepared by combining a chemically reactive fluoroalkylsilane compound with an oxide coated metal particle having a hydroxylated surface. The resulting fluoroalkylsilane layer that coats the particles provides them with excellent resistance to aging. The particles can be blended with oxidant particles to form energetic powder that releases chemical energy when the buffer layer is physically disrupted so that the reductant metal core can react with the oxidant.

  3. Interaction phenomena at reactive metal/ceramic interfaces.

    SciTech Connect

    McDeavitt, S. M.; Billings, G. W.; Indacochea, J. E.

    2000-11-03

    The objective of this study was to understand the interface chemical reactions between stable ceramics and reactive liquid metals, and developing microstructure. Experiments were conducted at elevated temperatures where small metal samples of Zr and Zr-alloy were placed on top of selected oxide and non-oxide ceramic substrates (Y{sub 2}O{sub 3}, ZrN, ZrC, and HfC). The sample stage was heated in high-purity argon to about 2000 C, held in most cases for five minutes at the peak temperature, and then cooled to room temperature at {approximately}20 c/min. An external video camera was used to monitor the in-situ wetting and interface reactions. Post-test examinations of the systems were conducted by scanning electron microscopy and energy dispersive spectroscopy. It was determined that the Zr and the Zr-alloy are very active in the wetting of stable ceramics at elevated temperatures. In addition, in some systems, such as Zr/ZrN, a reactive transition phase formed between the ceramic and the metal. In other systems, such as Zr/Y{sub 2}O{sub 3}, Zr/ZrC and Zr/HfC, no reaction products formed, but a continuous and strong joint developed under these circumstances also.

  4. Mixed oxygen ion/electron-conducting ceramics for oxygen separation

    SciTech Connect

    Stevenson, J.W.; Armstrong, T.R.; Armstrong, B.L.

    1996-08-01

    Mixed oxygen ion and electron-conducting ceramics are unique materials that can passively separate high purity oxygen from air. Oxygen ions move through a fully dense ceramic in response to an oxygen concentration gradient, charge-compensated by an electron flux in the opposite direction. Compositions in the system La{sub 1{minus}x}M{sub x}Co{sub 1{minus}y{minus}z}Fe{sub y}N{sub z}O{sub 3{minus}{delta}}, perovskites where M=Sr, Ca, and Ba, and N=Mn, Ni, Cu, Ti, and Al, have been prepared and their electrical, oxygen permeation, oxygen vacancy equilibria, and catalytic properties evaluated. Tubular forms, disks, and asymmetric membrane structures, a thin dense layer on a porous support of the same composition, have been fabricated for testing purposes. In an oxygen partial gradient, the passive oxygen flux through fully dense structures was highly dependent on composition. An increase in oxygen permeation with increased temperature is attributed to both enhanced oxygen vacancy mobility and higher vacancy populations. Highly acceptor-doped compositions resulted in oxygen ion mobilities more than an order of magnitude higher than yttria-stabilized zirconia. The mixed conducting ceramics have been utilized in a membrane reactor configuration to upgrade methane to ethane and ethylene. Conditions were established to balance selectivity and throughput in a catalytic membrane reactor constructed from mixed conducting ceramics.

  5. Method for bonding thin film thermocouples to ceramics

    DOEpatents

    Kreider, Kenneth G.

    1993-01-01

    A method is provided for adhering a thin film metal thermocouple to a ceramic substrate used in an environment up to 700 degrees Centigrade, such as at a cylinder of an internal combustion engine. The method includes the steps of: depositing a thin layer of a reactive metal on a clean ceramic substrate; and depositing thin layers of platinum and a platinum-10% rhodium alloy forming the respective legs of the thermocouple on the reactive metal layer. The reactive metal layer serves as a bond coat between the thin noble metal thermocouple layers and the ceramic substrate. The thin layers of noble metal are in the range of 1-4 micrometers thick. Preferably, the ceramic substrate is selected from the group consisting of alumina and partially stabilized zirconia. Preferably, the thin layer of reactive metal is in the range of 0.015-0.030 micrometers (15-30 nanometers) thick. The preferred reactive metal is chromium. Other reactive metals may be titanium or zirconium. The thin layer of reactive metal may be deposited by sputtering in ultra high purity argon in a vacuum of approximately 2 milliTorr (0.3 Pascals).

  6. NDE of structural ceramics

    NASA Technical Reports Server (NTRS)

    Klima, S. J.; Vary, A.

    1986-01-01

    Radiographic, ultrasonic, scanning laser acoustic microscopy (SLAM), and thermo-acoustic microscopy techniques were used to characterize silicon nitride and silicon carbide modulus-of-rupture test specimens in various stages of fabrication. Conventional and microfocus X-ray techniques were found capable of detecting minute high density inclusions in as-received powders, green compacts, and fully densified specimens. Significant density gradients in sintered bars were observed by radiography, ultrasonic velocity, and SLAM. Ultrasonic attenuation was found sensitive to microstructural variations due to grain and void morphology and distribution. SLAM was also capable of detecting voids, inclusions and cracks in finished test bars. Consideration is given to the potential for applying thermo-acoustic microscopy techniques to green and densified ceramics. The detection probability statistics and some limitations of radiography and SLAM also are discussed.

  7. Ceramic Sintering

    DTIC Science & Technology

    1974-10-01

    Prepared for: Office of Naval Research Advanced Research Projects Agency October 1974 DISTRIBUTED BY: National Technical InformatiM Service U. S... Cristobalite . This was also the crystalline form of the oxide on the powder on which the samples lay. Figure 5 showj oxidation data obtained at 1550oC...diameter were prepared by firing isostatically pressed silicon carbide powder containing boron and carbon for h hour at 2100oC in an argon-nitrogen

  8. High Temperature Tolerant Ceramic Composites Having Porous Interphases

    DOEpatents

    Kriven, Waltraud M.; Lee, Sang-Jin

    2005-05-03

    In general, this invention relates to a ceramic composite exhibiting enhanced toughness and decreased brittleness, and to a process of preparing the ceramic composite. The ceramic composite comprises a first matrix that includes a first ceramic material, preferably selected from the group including alumina (Al2O3), mullite (3Al2O3.2SiO2), yttrium aluminate garnet (YAG), yttria stabilized zirconia (YSZ), celsian (BaAl2Si2O8) and nickel aluminate (NiAl2O4). The ceramic composite also includes a porous interphase region that includes a substantially non-sinterable material. The non-sinterable material can be selected to include, for example, alumina platelets. The platelets lie in random 3-D orientation and provide a debonding mechanism, which is independent of temperature in chemically compatible matrices. The non-sinterable material induces constrained sintering of a ceramic powder resulting in permanent porosity in the interphase region. For high temperature properties, addition of a sinterable ceramic powder to the non-sinterable material provides sufficiently weak debonding interphases. The ceramic composite can be provided in a variety of forms including a laminate, a fibrous monolith, and a fiber-reinforced ceramic matrix. In the laminated systems, intimate mixing of strong versus tough microstructures were tailored by alternating various matrix-to-interphase thickness ratios to provide the bimodal laminate.

  9. Removing Undesired Fine Powder From Silicon Reactor

    NASA Technical Reports Server (NTRS)

    Flagella, Robert N.

    1992-01-01

    Fluidized-bed reactor produces highly pure polycrystalline silicon particles with diameters approximately greater than 400 micrometers. Operates by pyrolysis of silane in reaction zone, which is bed of silicon seed particles fluidized by flow of silane and carrier gas. Above reaction zone, gas mixture flows rapidly enough to entrain silicon powders, but not larger seed and product particles. Entrained particles swept out of reactor. Applicable to other processes such as production of fine metal and ceramic powders where control of sizes of product needed.

  10. Ceramic Seal.

    SciTech Connect

    Smartt, Heidi A.; Romero, Juan A.; Custer, Joyce Olsen; Hymel, Ross W.; Krementz, Dan; Gobin, Derek; Harpring, Larry; Martinez-Rodriguez, Michael; Varble, Don; DiMaio, Jeff; Hudson, Stephen

    2016-11-01

    Containment/Surveillance (C/S) measures are critical to any verification regime in order to maintain Continuity of Knowledge (CoK). The Ceramic Seal project is research into the next generation technologies to advance C/S, in particular improving security and efficiency. The Ceramic Seal is a small form factor loop seal with improved tamper-indication including a frangible seal body, tamper planes, external coatings, and electronic monitoring of the seal body integrity. It improves efficiency through a self-securing wire and in-situ verification with a handheld reader. Sandia National Laboratories (SNL) and Savannah River National Laboratory (SRNL), under sponsorship from the U.S. National Nuclear Security Administration (NNSA) Office of Defense Nuclear Nonproliferation Research and Development (DNN R&D), have previously designed and have now fabricated and tested Ceramic Seals. Tests have occurred at both SNL and SRNL, with different types of tests occurring at each facility. This interim report will describe the Ceramic Seal prototype, the design and development of a handheld standalone reader and an interface to a data acquisition system, fabrication of the seals, and results of initial testing.

  11. High temperature (1200 C) ceramic-to-metal seal development

    NASA Technical Reports Server (NTRS)

    Mckisson, R. L.; Ervin, G., Jr.

    1972-01-01

    Two phases have been completed, of a program whose ultimate objective is the development of an alkali metal resistant, thermal shock resistant, leak-tight, and neutron radiation resistant ceramic-to-metal seal capable of operation at 1200 C for three to five years. The first phase involved the screening of platinum-base, vanadium-base and vanadium-niobium base brazes for the joining of Cb-1Zr or T-111 alloys to high purity alumina. The second phase involved studies of the performance of sealed capsule samples during 5000-hour aging tests at 800, 1000, and 1200 C in high vacuum. Sealed capsules which were made using pure vanadium braze, and were brazed at 1850 C for one minute, survived 64 thermal cycles to 1200 C at the heating/cooling rate of 100 C/minute. Vanadium braze samples survived 5000-hour aging tests at 800, 1000, and 1200 C. One thermally cycled sample survived a subsequent 5000-hour aging period at 1000 C, but another, at 1200 C, did not survive. It was concluded that a pure vanadium braze used to bond high purity alumina to Cb-1Zr alloy is the best of the systems studied, but that additional studies must be performed to establish its service temperature limitations for the desired three to five years' service.

  12. Additive Manufacturing of SiC Based Ceramics and Ceramic Matrix Composites

    NASA Technical Reports Server (NTRS)

    Halbig, Michael Charles; Singh, Mrityunjay

    2015-01-01

    Silicon carbide (SiC) ceramics and SiC fiber reinforcedSiC ceramic matrix composites (SiCSiC CMCs) offer high payoff as replacements for metals in turbine engine applications due to their lighter weight, higher temperature capability, and lower cooling requirements. Additive manufacturing approaches can offer game changing technologies for the quick and low cost fabrication of parts with much greater design freedom and geometric complexity. Four approaches for developing these materials are presented. The first two utilize low cost 3D printers. The first uses pre-ceramic pastes developed as feed materials which are converted to SiC after firing. The second uses wood containing filament to print a carbonaceous preform which is infiltrated with a pre-ceramic polymer and converted to SiC. The other two approaches pursue the AM of CMCs. The first is binder jet SiC powder processing in collaboration with rp+m (Rapid Prototyping+Manufacturing). Processing optimization was pursued through SiC powder blending, infiltration with and without SiC nano powder loading, and integration of nanofibers into the powder bed. The second approach was laminated object manufacturing (LOM) in which fiber prepregs and laminates are cut to shape by a laser and stacked to form the desired part. Scanning electron microscopy was conducted on materials from all approaches with select approaches also characterized with XRD, TGA, and bend testing.

  13. Polymer quenched prealloyed metal powder

    DOEpatents

    Hajaligol, Mohammad R.; Fleischhauer, Grier; German, Randall M.

    2001-01-01

    A powder metallurgical process of preparing a sheet from a powder having an intermetallic alloy composition such as an iron, nickel or titanium aluminide. The sheet can be manufactured into electrical resistance heating elements having improved room temperature ductility, electrical resistivity, cyclic fatigue resistance, high temperature oxidation resistance, low and high temperature strength, and/or resistance to high temperature sagging. The iron aluminide has an entirely ferritic microstructure which is free of austenite and can include, in weight %, 4 to 32% Al, and optional additions such as .ltoreq.1% Cr, .gtoreq.0.05% Zr .ltoreq.2% Ti, .ltoreq.2% Mo, .ltoreq.1% Ni, .ltoreq.0.75% C, .ltoreq.0.1% B, .ltoreq.1% submicron oxide particles and/or electrically insulating or electrically conductive covalent ceramic particles, .ltoreq.1% rare earth metal, and/or .ltoreq.3 % Cu. The process includes forming a non-densified metal sheet by consolidating a powder having an intermetallic alloy composition such as by roll compaction, tape casting or plasma spraying, forming a cold rolled sheet by cold rolling the non-densified metal sheet so as to increase the density and reduce the thickness thereof and annealing the cold rolled sheet. The powder can be a water, polymer or gas atomized powder which is subjecting to sieving and/or blending with a binder prior to the consolidation step. After the consolidation step, the sheet can be partially sintered. The cold rolling and/or annealing steps can be repeated to achieve the desired sheet thickness and properties. The annealing can be carried out in a vacuum furnace with a vacuum or inert atmosphere. During final annealing, the cold rolled sheet recrystallizes to an average grain size of about 10 to 30 .mu.m. Final stress relief annealing can be carried out in the B2 phase temperature range.

  14. Measurements of gamma (γ)-emitting radionuclides with a high-purity germanium detector: the methods and reliability of our environmental assessments on the Fukushima 1 Nuclear Power Plant accident.

    PubMed

    Mimura, Tetsuro; Mimura, Mari; Komiyama, Chiyo; Miyamoto, Masaaki; Kitamura, Akira

    2014-01-01

    The severe accident of Fukushima 1 Nuclear Power Plant due to the Tohoku Region Pacific Coast Earthquake in 11 March 2011 caused wide contamination and pollution by radionuclides in Fukushima and surrounding prefectures. In the current JPR symposium, a group of plant scientists attempted to examine the impact of the radioactive contamination on wild and cultivated plants. Measurements of gamma (γ) radiation from radionuclides in "Fukushima samples", which we called and collected from natural and agricultural areas in Fukushima prefecture were mostly done with a high-purity Ge detector in the Graduate School of Maritime Sciences, Kobe University. In this technical note, we describe the methods of sample preparation and measurements of radioactivity of the samples and discuss the reliability of our data in regards to the International Atomic Energy Agency (IAEA) Interlaboratory comparisons and proficiency test (IAEA proficiency test).

  15. 1,1-dimethylhydrazine as a high purity nitrogen source for MOVPE-water reduction and quantification using nuclear magnetic resonance, gas chromatography-atomic emission detection spectroscopy and cryogenic-mass spectroscopy analytical techniques

    SciTech Connect

    Odedra, R.; Smith, L.M.; Rushworth, S.A.

    2000-01-01

    Hydrazine derivatives are attractive low temperature nitrogen sources for use in MOVPE due to their low thermal stability. However their purification and subsequent analysis has not previously been investigated in depth for this application. A detailed study on 1,1-dimethylhydrazine {l{underscore}brace}(CH{sub 3}){sub 2}N-NH{sub 2}{r{underscore}brace} purified by eight different methods and the subsequent quantitative measurements of water present in the samples obtained is reported here. A correlation between {sup 1}H nuclear magnetic resonance spectroscopy (NMR), gas chromatography-atomic emission detection (GC-AED) and cryogenic mass spectroscopy (Cryogenic-MS) has been performed. All three analysis techniques can be used to measure water in the samples and with the best purification the water content can be lowered well below 100 ppm. The high purity of this material has been demonstrated by growth results and the state-of-the-art performance of laser diodes.

  16. Microwave processing of ceramics

    SciTech Connect

    Katz, J.D.

    1989-01-01

    This paper discusses the following topics on microwave processing of ceramics: Microwave-material interactions; anticipated advantage of microwave sintering; ceramic sintering; and ceramic joining. 24 refs., 4 figs. (LSP)

  17. SUPPORTED DENSE CERAMIC MEMBRANES FOR OXYGEN SEPARATION

    SciTech Connect

    Timothy L. Ward

    2003-03-01

    This project addresses the need for reliable fabrication methods of supported thin/thick dense ceramic membranes for oxygen separation. Some ceramic materials that possess mixed conductivity (electronic and ionic) at high temperature have the potential to permeate oxygen with perfect selectivity, making them very attractive for oxygen separation and membrane reactor applications. In order to maximize permeation rates at the lowest possible temperatures, it is desirable to minimize diffusional limitations within the ceramic by reducing the thickness of the ceramic membrane, preferably to thicknesses of 10 {micro}m or thinner. It has proven to be very challenging to reliably fabricate dense, defect-free ceramic membrane layers of such thickness. In this project we are investigating the use of ultrafine SrCo{sub 0.5}FeO{sub x} (SCFO) powders produced by aerosol pyrolysis to fabricate such supported membranes. SrCo{sub 0.5}FeO{sub x} is a ceramic composition that has been shown to have desirable oxygen permeability, as well as good chemical stability in the reducing environments that are encountered in some important applications. Our approach is to use a doctor blade procedure to deposit pastes prepared from the aerosol-derived SCFO powders onto porous SCFO supports. We have previously shown that membrane layers deposited from the aerosol powders can be sintered to high density without densification of the underlying support. However, these membrane layers contained large-scale cracks and open areas, making them unacceptable for membrane purposes. In the past year, we have refined the paste formulations based on guidance from the ceramic tape casting literature. We have identified a multicomponent organic formulation utilizing castor oil as dispersant in a solvent of mineral spirits and isopropanol. Other additives were polyvinylbutyral as binder and dibutylphthalate as plasticizer. The nonaqueous formulation has superior wetting properties with the powder, and

  18. NDE for heat engine ceramics

    NASA Technical Reports Server (NTRS)

    Klima, S. J.

    1984-01-01

    Radiographic, ultrasonic, and scanning laser acoustic microscopy (SLAM) techniques were used to characterize silicon nitride and silicon carbide MOR bars in various stages of fabrication. Conventional and microfocus x-ray techniques were found capable of detecting minute high density inclusions in as-received powders, green compacts, and fully densified specimens. Significant density gradients in sintered bars were observed by radiography, ultrasonic velocity, and SLAM. Ultrasonic attenuation was found sensitive to microstructural variations due to grain and void morphology and distribution. SLAM was also capable of detecting voids, inclusions, and cracks in finished test bars. It was determined that thermoacoustic microscopy techniques have promise for application to green and densified ceramics.

  19. Incipient flocculation molding: A new ceramic-forming technique

    NASA Astrophysics Data System (ADS)

    Arrasmith, Steven Reade

    Incipient Flocculation Molding (IFM) was conceived as a new near-net-shape forming technique for ceramic components. It was hypothesized that the development of a temperature-dependent deflocculant would result in a forming technique that is flexible, efficient, and capable of producing a superior microstructure with improved mechanical properties from highly reactive, submicron ceramic powders. IFM utilizes a concentrated, nonaqueous, sterically stabilized ceramic powder and/or colloidal suspension which is injected into a non-porous mold. The suspension is then flocculated by destabilizing the suspension by lowering the temperature. Flocculation is both rapid and reversible. Cooling to -20°C produces a green body with sufficient strength for removal from the mold. The solvent is removed from the green body by evaporation. The dried green body is subsequently sintered to form a dense ceramic monolith. This is the first ceramic forming method based upon the manipulation of a sterically-stabilized suspension. To demonstrate IFM, the process of grafting polyethylene glycol (PEG), with molecular weights from 600 to 8000, to alumina powders was investigated. The maximum grafted amounts were achieved by the technique of dispersing the alumina powders in molten polymer at 195°C. The ungrafted PEG was then removed by repeated centrifuging and redispersion in fresh distilled water. The rheological behavior of suspensions of the PEG-grafted powders in water, 2-propanol and 2-butanol were characterized. All of the aqueous suspensions were shear thinning. The PEG 4600-grafted alumina powder aqueous suspensions were the most fluid. Sample rods and bars were molded from 52 vol% PEG-grafted alumina suspensions in 2-butanol. The best results were obtained with a preheated aluminum mold lubricated with a fluorinated oil mold-release. The samples were dried, sintered, and their microstructure and density were compared with sintered samples dry pressed from the same alumina powder

  20. Ceramic components manufacturing by selective laser sintering

    NASA Astrophysics Data System (ADS)

    Bertrand, Ph.; Bayle, F.; Combe, C.; Goeuriot, P.; Smurov, I.

    2007-12-01

    In the present paper, technology of selective laser sintering/melting is applied to manufacture net shaped objects from pure yttria-zirconia powders. Experiments are carried out on Phenix Systems PM100 machine with 50 W fibre laser. Powder is spread by a roller over the surface of 100 mm diameter alumina cylinder. Design of experiments is applied to identify influent process parameters (powder characteristics, powder layering and laser manufacturing strategy) to obtain high-quality ceramic components (density and micro-structure). The influence of the yttria-zirconia particle size and morphology onto powder layering process is analysed. The influence of the powder layer thickness on laser sintering/melting is studied for different laser beam velocity V ( V = 1250-2000 mm/s), defocalisation (-6 to 12 mm), distance between two neighbour melted lines (so-called "vectors") (20-40 μm), vector length and temperature in the furnace. The powder bed density before laser sintering/melting also has significant influence on the manufactured samples density. Different manufacturing strategies are applied and compared: (a) different laser beam scanning paths to fill the sliced surfaces of the manufactured object, (b) variation of vector length (c) different strategies of powder layering, (d) temperature in the furnace and (e) post heat treatment in conventional furnace. Performance and limitations of different strategies are analysed applying the following criteria: geometrical accuracy of the manufactured samples, porosity. The process stability is proved by fabrication of 1 cm 3 volume cube.