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Sample records for high-purity ceramic powders

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

    NASA Technical Reports Server (NTRS)

    Hoyer, Jesse L.

    1993-01-01

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

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

    DOEpatents

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

    2002-01-01

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

  3. Unusual ferromagnetism in high purity ZnO sintered ceramics

    SciTech Connect

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

    2011-01-15

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

  4. Combustion synthesis process for the rapid preparation of high-purity SrO powders

    NASA Astrophysics Data System (ADS)

    Granados-Correa, Francisco; Bonifacio-Martínez, Juan

    2014-12-01

    A rapid, safe and simple technique for the production of high purity strontium oxide powders via a chemical combustion process is reported. The combustion reactions were performed to optimize the fuel to oxidizer ratios in the reaction mixtures required to obtain pure SrO powders by varying the molar ratio of chemical precursors and the temperature. The synthesized powders were characterized by X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectrometry, infrared spectroscopy, differential scanning calorimetry, thermogravimetric analysis, and N2-physisorption measurements. The results indicate that crystalline SrO was obtained using a 1:1 strontium nitrate: urea molar ratio at 1000 °C after 5 minutes. In addition, high-purity, homogeneous and crystalline SrO powders were easily produced in a short time via a chemical combustion process.

  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. Ceramic powder compaction

    SciTech Connect

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

    1995-12-31

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

  8. Effects of grain, grain boundary, and dc electric field on giant dielectric response in high purity CuO ceramics

    NASA Astrophysics Data System (ADS)

    Thongbai, Prasit; Maensiri, Santi; Yamwong, Teerapon

    2008-08-01

    Giant dielectric constant ɛ' of ˜(2.8-3.7)×104 was observed in high purity CuO (99.999%) ceramics with grain sizes of 4.57±1.71 and 9.57±3.01 μm. The ɛ' and Ea increase with an increase in grain size due to the different electrical properties in the grains. The high dielectric response observed in the CuO ceramics can be described by the internal barrier layer capacitance model. The resistance of grain boundaries (Rgb) and the dielectric constant of the CuO samples decrease with increasing dc bias due to the decrease in grain boundaries capacitance, whereas the resistance of grains (Rg) remains constant.

  9. 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.

  10. 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.

  11. 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.

  12. Electrically conductive ceramic powders

    NASA Astrophysics Data System (ADS)

    Lu, Yanxia

    1999-11-01

    Electrically conductive ceramic powders were investigated in this project. There are three ways to produce those materials. The first is doping alkali metal into the titanium dioxides in an inert or reducing atmosphere. The second is reducing un-doped titanium dioxide, forming a non-stoichiometric composition in a hydrogen atmosphere. The third is to coat a conductive layer, reduced titanium dioxide, on an insulating core such as alumina. Highly conductive powders have been produced by all these processes. The conductivity of powder compacts ranged between 10-2 and 10° S/cm. A novel doping process was developed. All samples were doped by a solid-vapor reaction instead of a solid state reaction. Titanium dioxide was doped with alkali metals such as Na or Li in this study. The alkali metal atom contributes an electron to the host material (TiO2), which then creates Ti 3+ ion. The conductivity was enhanced by creating the donor level due to the presence of these Ti3+ ions. The conductivity of those alkali doped titanium oxides was dependent on the doping level and charge mobility. Non-stoichiometric titanium oxides were produced by reduction of titanium dioxide in a hydrogen atmosphere at 800°C to 1000°C for 2 to 6 hours. The reduced titanium oxides showed better stability with respect to conductivity at ambient condition when compared with the Na or Li doped samples. Conductive coatings were prepared by coating titanium precursors on insulating core materials like SiO2, Al2O3 or mica. The titania coating was made by hydrolysis of titanyl sulfate (TiOSO 4) followed by a reduction procedure to form reduced titanium oxide. The reduced titanium oxides are highly conductive. A uniform coating of titanium oxides on alumina cores was successfully produced. The conductivity of coated powder composites was a function of coating quantity and hydrolysis reaction temperature. The conductivity of the powder as a function of structure, composition, temperature, frequency and

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. 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.

  18. 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.

  19. 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.

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

    DOEpatents

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

    2011-04-12

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

  1. 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.

  2. 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.

  3. 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.

  4. 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.

  5. Dynamic consolidation of ceramic powders: practicalities, problems, and prospects

    SciTech Connect

    Gourdin, W.H.

    1983-11-10

    I present an assessment of the technological potential of shock wave consolidation of ceramic powders as a technique for producing well-bonded, uniform, crack-free monoliths. Current compaction methods are briefly reviewed and the characteristics of the consolidated material are presented. The shock and release histories experienced by powder compacts in simple compaction assemblies are complex and I conclude that such simple assemblies are unlikely to yield structurally sound bodies. Control of the stress history over the entire loading cycle is necessary if the tensile stresses which develop during release are to be reduced to acceptable levels. Such exacting control is difficult to achieve, and becomes increasingly difficult as the peak stresses are increased. The powder must therefore be sufficiently plastic at moderate stresses to permit densification and bonding of the compact without destruction of the compact during release. Not all ceramic powders will satisfy this criterion. Local microstructural modification, including interfacial melting, is limited by the fine particle sizes and large surface areas of many ceramic powders. Production of cohesive, crack-free bodies thus depends upon a complex interplay between shock history, material properties, and powder characteristics which is poorly understood. I conclude that the technology of dynamic consolidation of ceramic powders will be difficult to develop and will have limited applications. 37 references, 8 figures.

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

    DOEpatents

    Moorhead, A.J.; Kim, H.

    1999-08-10

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

  7. 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.

  8. 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.

  9. 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.

  10. Dense silica coatings on ceramic powder particles

    SciTech Connect

    Opitz, J.F.A.; Mayr, W.

    1995-09-01

    Dense silica coatings on the surface of inorganic powders particles are prepared by the hydrolysis of tetraethoxysilane (TEOS) in alcoholic suspensions. In a first reaction step, the TEOS is pre-hydrolysed in acidic solution and afterwards, a suspension of powder particles in this reaction solution is treated with ammonia which results in a dense silica coating of typically 10 - 100 nm thickness. Different luminescent powders which are used in the manufacture of cathode-ray tubes or fluorescent lamps have been coated by this procedure. The silica coating forms a transparent layer and the suspension properties of the coated powders are determined by the silica layer. The silica coating also protects sulfidic luminescent powders from being attacked by oxidizing agents like dichromate ions which are used in the suspension formulations for TV tube fabrication.

  11. 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

  12. 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

  13. 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

  14. Applied mechanics modeling of granulated ceramic powder compaction

    SciTech Connect

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

    1995-08-01

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

  15. 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.

  16. 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.

  17. Manufacturing of transparent ZnS ceramics by powders sintering

    NASA Astrophysics Data System (ADS)

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

    2016-05-01

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

  18. Synthesis of ceramic oxide powders in a microwave plasma device

    SciTech Connect

    Vollath, D.; Sickafus, K.E.

    1993-05-01

    Synthesizing oxide ceramic powders by application of a microwave plasma is of great advantage. The microwave plasma can be used two ways: To act as a source of heat for the pyrolysis of solutions and to excite gas phase reactions to obtain nanosized powders. Both applications are superior to standard methods. A microwave cavity well suited for these experiments and its operating characteristics are described. Using a microwave plasma as a source of heat for pyrolytic decomposition of nitrates in aqueous solutions leads to a fine grained product with particle sizes from 100 to 1000 nm. Crystallite sizes in those particles are in most cases less than 10 nm. This is demonstrated with zirconia-based ceramics, such as ZrO{sub 2} -- 3m% Y{sub 2}O{sub 3} -- 20m% Al{sub 2}O{sub 3}, Depending on conditions during pyrolysis, it is possible to obtain a product in which alumina is either dissolved in zirconia or the onset of the phase separation is observed. Energy efficiency for this process is better than 80%. If the reactants are gaseous e.g., ZrCl{sub 4} it is possible to produce powders with mean crystallite sizes of about 4 nm. In the case of zirconia these particles are nanocrystalline with a cubic structure. This structure is not in equilibrium under the experimental conditions.

  19. 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.

  20. Absorption of microwaves in metal-ceramic powder materials

    NASA Astrophysics Data System (ADS)

    Egorov, S. V.; Eremeev, A. G.; Plotnikov, I. V.; Rybakov, K. I.; Kholoptsev, V. V.; Bykov, Yu. V.

    2010-11-01

    Sintering of metal-ceramic composites by microwave heating is a promising method for creation of functionally graded materials. In this paper, we study the absorption of microwaves in compacted mixtures of metal and dielectric powders. The coefficient of microwave absorption is calculated within the framework of the effective-medium approximation as a function of the mass fraction, dimensions, and temperature of metal particles. The experimental method for determination of the microwave absorption coefficient is proposed, which is based on measuring the temperature of the samples during their heating by microwaves in an oversized working chamber. The coefficients of microwave absorption in powder composites Al2O3-Ni, which were measured by the proposed method, are presented. An agreement between the theoretical and experimental results is demonstrated.

  1. 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.

  2. 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.

  3. High-purity thermoacoustic isotope enrichment.

    PubMed

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

    2014-08-01

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

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. Biaxial deformation in high purity aluminum

    DOE PAGES

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

    2015-09-25

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

  9. 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.

  10. Techniques for the determination of the static and dynamics internal friction of coefficients of ceramic powder

    SciTech Connect

    Martinez, M.A.; Cortes, R.; Sanchez-Galvez, V.; Navarro, C. . Dept. of Materials Science)

    1993-11-01

    This paper discusses different techniques for the experimental estimation of the static and dynamic internal friction coefficients of fragmented ceramics. These were applied to the powders of two ballistic ceramics, SiC and Al[sub 2]O[sub 3]. The relationship between the fragment size and the internal friction coefficients of the powders was determined. The results obtained with the different techniques are compared.

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

    NASA Astrophysics Data System (ADS)

    Kulovaná, Tereza; Pavlík, Zbyšek

    2016-06-01

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

  12. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2016-04-01

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

  14. 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.

  15. 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.

  16. 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.

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

    SciTech Connect

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

    2006-01-27

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

  18. 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.

  19. 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

  20. 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.

  1. 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.

  2. 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%.

  3. 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.

  4. 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.

  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. 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%.

  7. Improved Protection Properties by Using Nanostructured Ceramic Powders for HVOF Coatings

    NASA Astrophysics Data System (ADS)

    Varis, T.; Knuuttila, J.; Turunen, E.; Leivo, J.; Silvonen, J.; Oksa, M.

    2007-12-01

    The potential of the high-velocity oxy-fuel (HVOF) thermal spray process for reduced porosity in coatings compared to those produced by other ambient thermal spray processes is well known. The ability to produce high-density ceramic coatings offers potential in high-performance applications in the field of wear, corrosion resistance, and dielectric coatings. However, due to operational limit of the HVOF process to effectively melt the ceramic particles, the process—structure relationship must be well optimized. It has been also demonstrated that benefits from HVOF ceramic coatings can be obtained only if particles are melted enough and good lamella adhesion is produced. One strategy to improve melting of ceramic particles in relative low-flame temperatures of HVOF process is to modify particle crystal structure and composition. In this paper the effect of the powder manufacturing method and the composition on deposition efficiency of spray process as well as on the mechanical properties of the HVOF sprayed are studied. Effect of fuel gas, hydrogen vs. propane, was also demonstrated. Studied materials were alumina-, chromia-, and titania-based agglomerated powders. Coating properties such as microstructure, hardness, abrasive wear resistance, and relative fracture toughness were compared to the coating manufactured by using conventional fused and crushed powders. It can be concluded that powder size distribution and microstructure should be optimized to fulfill process requirements very carefully to produce coatings with high deposition efficiency, dense structure, improved fracture toughness, and adhesion.

  8. 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

  9. 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.

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

    PubMed

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

    2016-01-01

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

  11. Characterisation of two AGATA asymmetric high purity germanium capsules

    NASA Astrophysics Data System (ADS)

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

    2015-02-01

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

  12. 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.

  13. 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.

  14. 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.

  15. 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).

  16. Optimization of calcium phosphate fine ceramic powders preparation

    NASA Astrophysics Data System (ADS)

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

    2013-12-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-04-01

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

  18. Hydrogen concentration and distribution in high-purity germanium crystals

    SciTech Connect

    Hansen, W.L.; Haller, E.E.; Luke, P.N.

    1981-10-01

    High-purity germanium crystals used for making nuclear radiation detectors are usually grown in a hydrogen ambient from a melt contained in a high-purity silica crucible. The benefits and problems encountered in using a hydrogen ambient are reviewed. A hydrogen concentration of about 2 x 10/sup 15/cm/sup -3/ has been determined by growing crystals in hydrogen spiked with tritium and counting the tritium ..beta..-decays in detectors made from these crystals. Annealing studies show that the hydrogen is strongly bound, either to defects or as H/sub 2/ with a dissociation energy > 3 eV. This is lowered to 1.8 eV when copper is present. Etching defects in dislocation-free crystals grown in hydrogen have been found by etch stripping to have a density of about 1 x 10/sup 7/ cm/sup -3/ and are estimated to contain 10/sup 8/ H atoms each.

  19. High-Purity Silicon Seeds for Silane Pyrolysis

    NASA Technical Reports Server (NTRS)

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

    1985-01-01

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

  20. Sintering stress and microstructure in ceramic powder compacts

    SciTech Connect

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

    1990-08-01

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

  1. Practical analysis of high-purity chemicals-I Preparation and characterization of high-purity EDTA.

    PubMed

    Barnard, A J; Joy, E F; Little, K; Brooks, J D

    1970-09-01

    Advanced laboratories have requirements for high-purity chemicals with less than 500 ppm total impurities (ultrapure chemicals) and with broad analytical definition of each lot. Some economically feasible approaches to the practical analysis of such chemicals, both inorganic and organic, are delineated. Compounds used in the study of lunar samples and in other advanced programmes are noted. EDTA, as the free add, has been prepared by dissolution in water with base and precipitation by addition of add. The product has been broadly characterized. Precision assay is achieved by weight titrimetry, potentiometrically as a triprotic add and photometrically as a chelatmg agent. Other tests applied include elemental analysis, ash, loss on drying, particulatc matter, and tests for nitrilotriacetate, arsenic, and chloride. Boron, silicon, and trace metals are determined by emission spectrography. Many of the procedures are applicable to other high-purity organic chemicals.

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

    NASA Astrophysics Data System (ADS)

    Radsick, Timothy Carl

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

  3. Improving the efficiency of high purity water systems

    SciTech Connect

    Bukay, M.; Youngberg, D.

    1994-05-01

    High purity water (HPW) production involves the consumption of substantial amounts of energy, precious potable water, harsh/hazardous chemicals, and other environmental/impact materials. The discharge of some of the waste products from HPW systems is also a concern. The purpose of this paper is to discuss techniques to improve the efficiency of HPW production and thereby reduce any negative effects on the environment. It provides specific examples of how end-users and equipment suppliers are increasing the efficiency of their pretreatment, reverse osmosis, ion-exchange, and sanitization technology while frequently citing capital and operating cost reductions.

  4. 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.

  5. 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).

  6. 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.

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

    SciTech Connect

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

    2007-05-17

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

  8. Milling and blending of ceramic powders for the plutonium immobilization program

    SciTech Connect

    Herman, D T; Biehl, W E

    2000-02-14

    The goal of the Plutonium Immobilization Program is the immobilization of surplus weapons usable plutonium in a ceramic form. The ceramic will then be encapsulated in high level waste glass using the can-in-can configuration. In the ceramic line of the immobilization plant, surplus plutonium oxide of less than 100 micron particle size will be received for immobilization. The plutonium oxide must be sized reduced and intimately blended with uranium oxide and the other ceramic forming materials containing neutron poisons to allow for complete interaction during sintering. Once properly blended, the formulation will be pressed into the desired ceramic form and then sintered to produce the targeted mineral phases. The equipment of choice for the size reduction of the actinides and the blending with the precursor materials is the Union Process attritor mill. The attritor mill is best described as a stirred ball mill and consists of a stationary tank filled with grinding media that is agitated by a shaft with stirring arms. The rotational shaft stirs the media at high-speed causing shearing and impact forces on the material resulting in size reduction and dispersion. Speeds over 1000 rpm can be reached by the stirring shaft. The high-speed of the attritor mill imparts a large amount of energy to the feed powder. This high energy dramatically reduces the time required to mill/blend from hours to minutes. Another advantage of the equipment is that operations are performed completely dry. Powder is discharged from the attritor by opening a discharge valve containing a slotted screen. Process and equipment tests have been run using cerium as a chemical substitute for the actinides. Substitution of cerium oxide allows the proper ceramic phases to form during sintering. Though cerium is a good chemical surrogate for the actinides, it does not provide an adequate surrogate to represent the physical properties of the actinide oxides. Therefore, manganese oxide has been used for

  9. Development of high purity large forgings for nuclear power plants

    NASA Astrophysics Data System (ADS)

    Tanaka, Yasuhiko; Sato, Ikuo

    2011-10-01

    The recent increase in the size of energy plants has been supported by the development of manufacturing technology for high purity large forgings for the key components of the plant. To assure the reliability and performance of the large forgings, refining technology to make high purity steels, casting technology for gigantic ingots, forging technology to homogenize the material and consolidate porosity are essential, together with the required heat treatment and machining technologies. To meet these needs, the double degassing method to reduce impurities, multi-pouring methods to cast the gigantic ingots, vacuum carbon deoxidization, the warm forging process and related technologies have been developed and further improved. Furthermore, melting facilities including vacuum induction melting and electro slag re-melting furnaces have been installed. By using these technologies and equipment, large forgings have been manufactured and shipped to customers. These technologies have also been applied to the manufacture of austenitic steel vessel components of the fast breeder reactors and components for fusion experiments.

  10. 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.

  11. 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.

  12. 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.

  13. Effects of chemicothermal treatment of aluminum nitride powders on the structure and properties of the resulting hot-pressed ceramic

    SciTech Connect

    Tkachenko, Yu.G.; Morozova, R.A.; Yurchenko, D.Z.

    1995-07-01

    Preliminary treatment in hydrogen for aluminum nitride powders (before hot pressing) affects the strengthening and structuring of the ceramic. There is a positive effect from the gas heat treatment on account of recrystallization during sintering and increase in plasticity of the aluminum nitride due to the hydrogen dissolved in the lattice.

  14. 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

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

    PubMed

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

    2016-01-01

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

  16. 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.

  17. High Purity Zirconium Tetrafluoride For Fluoride Glass Applications

    NASA Astrophysics Data System (ADS)

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

    1989-06-01

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

  18. Photothermal ionization spectroscopy of donors in high-purity germanium

    SciTech Connect

    Darken, L.S.

    1989-02-01

    The results of narrow linewidth (0.10 cm/sup -1/ FWHM) photothermal ionization spectroscopy (PTIS) investigations of shallow donors in high-purity germanium are reported. The donors observed include phosphorus, arsenic, lithium, a hydrogen-oxygen complex, and three lithium-related complexes. One lithium-related complex designated D(Li,Y) is reported here for the first time. Within experimental accuracy, energies of the excited states with respect to the conduction band are the same for all donors. Fourteen different 1S..-->..excited state transitions (five previously unreported, two others seen for the first time in PTIS from the ground state) have been observed. The Zeeman effect was used to help identify these levels. PTIS lines from the ground state to 2P/sub 0/ and 3P/sub 0/ were found to be relatively weak but their intensity was in good agreement with the intensity calculated by means of the Cascade theory. In as-grown samples, linewidth broadening of group V donors was observed that depended on the square root of the dislocation density (etch pit density) and with features expected from deformation potential theory.

  19. 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.

  20. 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).

  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. 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.

  3. Spectroscopic Determination of Trace Contaminants in High Purity Oxygen

    NASA Technical Reports Server (NTRS)

    Hornung, Steven D.

    2011-01-01

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

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

    SciTech Connect

    National Energy Technology Laboratory

    2000-08-31

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

  5. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2011-07-01

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

  7. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2014-09-01

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

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

    SciTech Connect

    Heshmat, Hooshang; Dill, J.F. )

    1992-04-01

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

  10. 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).

  11. 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

  12. 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

  13. 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.

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

    PubMed

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

    2014-02-01

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

  15. 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.

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

    PubMed

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

    2016-04-11

    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.

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

    PubMed

    Kujawa, Joanna; Kujawski, Wojciech

    2016-03-23

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

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

    PubMed

    Kujawa, Joanna; Kujawski, Wojciech

    2016-03-23

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

  19. 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.

  20. Bonding efficacy and side effects of the high purity glyceryl mono-methacrylate.

    PubMed

    Takahashi, Y; Itoh, K; Manabe, A; Tani, C; Hisamitsu, H

    2004-12-01

    The purpose of this study was to examine the efficacy of experimentally developed high purity glyceryl mono-methacrylate (GM) as a dentine primer and to evaluate the possibility of allergic reaction. The efficacy of experimental dentine primers was evaluated by measuring the polymerization contraction gap width and the tensile bond strength. Allergic reaction was evaluated by the guinea-pig maximization test. The skin reaction was evaluated according to the criteria of the International Contact Dermatitis Research Group. Contraction gap formation was completely prevented and the tensile bond strength was not significantly affected by priming with GM on high-purity GM. The allergic response decreased when high-purity GM was employed as the challenger. It was concluded that the clinical use of the high-purity GM is beneficial as the delayed allergic reaction could be avoided with no detrimental effect on the dentine bonding. PMID:15544652

  1. Trace element analysis of K, U and Th in high purity materials by neutron activation analysis

    SciTech Connect

    Pillalamarri, Ila

    2005-09-08

    The concept and usage of 'high purity' are explained. Trace element analysis of K, U and Th by neutron activation analysis is described, the radio-isotopes and their corresponding gamma-rays used to identify the elements are listed. The interfering elements are described. The advantages and disadvantages of using neutron activation analysis are discussed. Some examples of trace impurity determinations in high purity materials are provided.

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

    NASA Astrophysics Data System (ADS)

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

    2008-12-01

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

  3. 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

  4. 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

  5. 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.

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

    NASA Astrophysics Data System (ADS)

    Mozaffari, Mortaza; Amighian, Jamshid

    2002-08-01

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

  7. 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.

  8. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2006-08-01

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

  10. 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.

  11. Effect of ferrite powder fineness on the structure and properties of ceramic materials

    SciTech Connect

    Pashchenko, V.P.; Nesterov, A.M.; Litvinova, O.G.

    1995-03-01

    Comprehensive study of the structure and properties of ferrite materials prepared from powders with different specific surface (0.4 M{sup 2}/g < S{sub sp} < 1.2 m{sub 2/g}) shows that the optimum specific surface of manganese-zinc ferrite powders is about 0.6 m{sup 2}1/g. With an increase in the specific surface of nickel-zinc and barium ferrite powders the porous crystalline structure of sintered specimens and most of the main electromagnetic properties of ferrite articles are improved.

  12. Recent advancements in transparent ceramics and crystal fibers for high power lasers

    NASA Astrophysics Data System (ADS)

    Kim, W.; Baker, C.; Villalobos, G.; Florea, C.; Gibson, D.; Shaw, L. B.; Bowman, S.; Bayya, S.; Sadowski, B.; Hunt, M.; Askins, C.; Peele, J.; Aggarwal, I. D.; Sanghera, J. S.

    2013-05-01

    In this paper, we present our recent progress in the development of rare-earth (Yb3+ or Ho3+) doped Lu2O3 and Y2O3 sesquioxides for high power solid state lasers. We have fabricated high quality transparent ceramics using nano-powders synthesized by a co-precipitation method. This was accomplished by developments in high purity powder synthesis and low temperature scalable sintering technology developed at NRL. The optical, spectral and morphological properties as well as the lasing performance from our highly transparent ceramics are presented. In the second part of the paper, we discuss our recent research effort in developing cladded-single crystal fibers for high power single frequency fiber lasers has the potential to significantly exceed the capabilities of existing silica fiber based lasers. Single crystal fiber cores with diameters as small as 35μm have been drawn using high purity rare earth doped ceramic or single crystal feed rods by the Laser Heated Pedestal Growth (LHPG) process. Our recent results on the development of suitable claddings on the crystal fiber core are discussed.

  13. Synthesis Of Nanosized CGYO Powders Via Glycine Nitrate Methods As Precursors For Dense Ceramic Membranes

    NASA Astrophysics Data System (ADS)

    Kochhar, Savinder P.; Singh, Anirudh P.

    2011-12-01

    Glycine nitrate combustion method was used to synthesize Ce0.8Gd0.1Y0.1O1.9 powders. Soluble metal-glycine complexes, detected by infrared spectroscopy, were formed by atomic level mixing of metal cations with glycine. The concentration of glycine has been varied in order to change the fuel to oxidant ratio i.e. of glycine to nitrate (g/n) with the purpose to study the effect of concentration of glycine on the parameters of resulting CGYO powder. The ratio of glycine to nitrate per mole is 0.5, 0.7, 0.8, 0.9, 1.0, 1.2, and 1.4. Increasing the glycine increases the temperatures reached during combustion. Powders prepared from GNP method demonstrated that combustion synthesized powders have large surface area as shown by SEM.

  14. 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.

  15. 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.

  16. 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.

  17. 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.

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

    PubMed

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

    2012-07-01

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

  19. 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.

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

    NASA Astrophysics Data System (ADS)

    Zupan, Klementina; Kolar, Drago; Marinšek, Marjan

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

  1. UO{sub 2} Ceramic Grade Powders Prepared by Direct Microwave Denitration at Reduced Pressures

    SciTech Connect

    Marchi, Daniel E.; Lorenzo, Viviana J.

    2003-11-15

    Direct denitration using microwaves (MWD) is an interesting alternative conversion method to obtain uranium dioxide powders from nitric solutions of uranium, since it has many attractive features. However, as other methods, traditional MWD includes a milling step of the powders, which is a disadvantage from the operative and economical point of view. In this paper, the denitration process was studied by depressing the pressure inside the vessel where the solution is denitrated. Intermediate and final products were characterized. It was demonstrated that when working pressure ranges between 520 and 970 hPa during denitration, high density UO{sub 2} pellets can be obtained without resorting to a milling step.

  2. 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.

  3. 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.

  4. Non-aqueous spray drying as a route to ultrafine ceramic powders

    SciTech Connect

    Armor, J.N. ); Fanelli, A.J.; Marsh, G.M. ); Zambri, P.M. )

    1988-09-01

    Spray drying imparts unique powder handling features to a wide variety of dried products and is usually carried out in a heated air stream while feeding an aqueous suspension of some solid material. The present work, however, describes non-aqueous spray drying as a means of preparing fine powders of metal oxides. In this case an alcohol solvent was used in place of water and the slurry sprayed under an inert atmosphere. Using the non-aqueous technique, the product consists of distinct but loosely aggregated primary particles. Such materials have potential for use as catalysts or catalyst supports.

  5. Transport studies on very high purity gallium arsenide grown by organometallic vapor phase epitaxy

    NASA Astrophysics Data System (ADS)

    Tsang, Cheung Fat

    1997-12-01

    Very high purity GaAs layers have been grown in a modified organometallic vapor phase epitaxy (OMVPE) system using trimethyl gallium (TMGa) and arsine including the purest layer ever reported from these chemical sources with purity approaching the very best reported by the chloride-VPE technique. Several of these high purity GaAs samples were chemically etched into Kelvin and Greek cross structures which were fabricated with PdGe ohmic contacts for the specific contact resistivity, Hall effect, and persistent photo-Hall measurements performed in the full temperature range (4.2 K to 305 K). Resonant excitation photoluminescence technique operated at zero magnetic field was used to discriminate the impurity species in the very high purity layer where Ge and C were detected as the principle impurities. The consistency of growing GaAs layers with very low donor impurity concentration was found to be limited by the variability of arsine quality from bottle to bottle. Peak mobilities of the high purity GaAs layers are shown to be linearly dependent on the donor concentration while the low temperature mobilities are limited by the acceptor impurity level and the degree of carrier compensation. The acoustic deformation potential is generally conceived as a material constant but is demonstrated in the analysis as a variable parameter that has a linear relationship with the total impurity concentration. As for the contact resistivity of PdGe contacts on high purity GaAs layers, a room temperature Nsb{D}sp{-1/2} dependence was confirmed. Inhomogeneities in several samples were detected by the persistent photo-Hall measurements and the impurity band formation-like characteristics were observed at the very low temperatures. This technique was also used to facilitate the measurement of a carrier-depleted, high purity GaAs layer that has a relatively high carrier compensation. Finally, chemical etching techniques for the fabrication of the measurement samples including the micro

  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. Control of high-purity distillation column using a nonlinear wave theory

    SciTech Connect

    Han, Myungwan; Park, Sunwon )

    1993-05-01

    A new model-based controller for profile position control of high-purity distillation columns is presented. The controller has been developed by incorporating nonlinear wave model into the generic model control framework. An observer based on the nonlinear wave theory is also proposed to determine the profile position. The performance of the nonlinear control scheme has been tested in simulation experiments of high-purity binary distillation columns. Tight control of profile position, which leads to fast stabilization of product compositions, has been achieved. Since the profile position control alone produces a slight offset from the desired product concentration, the composition/profile position cascade system has been used to remove the offset. The control scheme can handle significant disturbances and model-plant mismatch.

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

    NASA Astrophysics Data System (ADS)

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

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

  9. 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.

  10. 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

  11. Preparation of High-Purity Cobalt by Anion-Exchange Separation and Plasma Arc Melting

    NASA Astrophysics Data System (ADS)

    Uchikoshi, Masahito; Shibuya, Hideka; Imaizumi, Junichi; Kékesi, Tamás; Mimura, Kouji; Isshiki, Minoru

    2010-04-01

    High-purity Co was prepared with valence-controlled anion-exchange separation, oxidation refining using plasma arc melting, and H2-Ar plasma arc melting on a pilot scale. The result of a laboratory-scale experiment indicated that the slower flow rate is more effective to remove the impurities by anion-exchange separation. However, the separation efficiency is reduced by scaling up the column from the laboratory to pilot scale. The discussion of the decrease in the separation efficiency implies that the distribution coefficient increases as the concentration of the adsorbate is lowered, but a reduced slower flow rate might increase the final purity of Co. In addition to anion-exchange separation, Co oxidation refining using plasma arc melting was useful. Consequently, a high-purity Co of 99.9998 pct by mass excluding gaseous elements was prepared, which represents the highest purity reported.

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

    NASA Astrophysics Data System (ADS)

    Kumar, Nirmal; Biswas, Krishanu

    2015-08-01

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

  13. A novel and efficient method for enzymatic synthesis of high purity maltose using moranoline (1-deoxynojirimycin).

    PubMed

    Maruo, S; Yamashita, H; Miyazaki, K; Yamamoto, H; Kyotani, Y; Ogawa, H; Kojima, M; Ezure, Y

    1992-09-01

    A transglycosylation reaction with moranoline (1-deoxynojirimycin) was done with soluble starch as the glucosyl donor and Bacillus macerans amylase as a cyclodextrin glycosyltransferase [EC 2.4.1.19]. The resultant transglycosylation products with moranoline, obtained by treating the reaction mixture with a strong cation exchange resin, were hydrolyzed by beta-amylase [EC 3.2.1.2] from sweet potatoes. The hydrolysate was treated with a strong cation exchange resin, and high purity maltose was obtained. PMID:1368945

  14. 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.

  15. Recovering iron, manganese, copper, cobalt, and high-purity nickel from sea nodules

    NASA Astrophysics Data System (ADS)

    Kohga, Tetsuyoshi; Imamura, Masaki; Takahashi, Junichi; Tanaka, Nobuhiro; Nishizawa, Tokuo

    1995-12-01

    Many studies have investigated methods of recovering valuable metals from sea nodules. Recently, a research group in Japan developed a smelting and chlorine process after investigating a variety of existing processes and comparing their respective efficiencies with the same nodules. The best results were obtained by combining pyrometallurgical and hydrometallurgical treatments, which enabled the efficient recovery of manganese, nickel, copper, and cobalt. High-purity nickel can be also produced through further solvent extraction.

  16. A novel and efficient method for enzymatic synthesis of high purity maltose using moranoline (1-deoxynojirimycin).

    PubMed

    Maruo, S; Yamashita, H; Miyazaki, K; Yamamoto, H; Kyotani, Y; Ogawa, H; Kojima, M; Ezure, Y

    1992-09-01

    A transglycosylation reaction with moranoline (1-deoxynojirimycin) was done with soluble starch as the glucosyl donor and Bacillus macerans amylase as a cyclodextrin glycosyltransferase [EC 2.4.1.19]. The resultant transglycosylation products with moranoline, obtained by treating the reaction mixture with a strong cation exchange resin, were hydrolyzed by beta-amylase [EC 3.2.1.2] from sweet potatoes. The hydrolysate was treated with a strong cation exchange resin, and high purity maltose was obtained.

  17. Charge collection performance of a segmented planar high-purity germanium detector

    NASA Astrophysics Data System (ADS)

    Cooper, R. J.; Boston, A. J.; Boston, H. C.; Cresswell, J. R.; Grint, A. N.; Harkness, L. J.; Nolan, P. J.; Oxley, D. C.; Scraggs, D. P.; Lazarus, I.; Simpson, J.; Dobson, J.

    2008-10-01

    High-precision scans of a segmented planar high-purity germanium (HPGe) detector have been performed with a range of finely collimated gamma ray beams allowing the response as a function of gamma ray interaction position to be quantified. This has allowed the development of parametric pulse shape analysis (PSA) techniques and algorithms for the correction of imperfections in performance. In this paper we report on the performance of this detector, designed for use in a positron emission tomography (PET) development system.

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

    NASA Astrophysics Data System (ADS)

    Tulevski, George; IBM TJ Watson Reserach Center Team

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

  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. 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.

  1. 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.

  2. 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.

  3. 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%.

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

    PubMed

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

    2016-07-18

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

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

    SciTech Connect

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

    2014-09-01

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

  6. 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.

  7. 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.

  8. 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.

  9. Silicon nitride/silicon carbide composite powders

    DOEpatents

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

    1996-06-11

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

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

    NASA Astrophysics Data System (ADS)

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

    2015-10-01

    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.

  11. 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.

  12. Initial Field Measurements with the Multisensor Airborne Radiation Survey (MARS) High Purity Germanium (HPGe) Detector Array

    SciTech Connect

    Fast, James E.; Bonebrake, Christopher A.; Dorow, Kevin E.; Glasgow, Brian D.; Jensen, Jeffrey L.; Morris, Scott J.; Orrell, John L.; Pitts, W. Karl; Rohrer, John S.; Todd, Lindsay C.

    2010-06-29

    Abstract: The Multi-sensor Airborne Radiation Survey (MARS) project has developed a new single cryostat detector array design for high purity germanium (HPGe) gamma ray spectrometers that achieves the high detection efficiency required for stand-off detection and actionable characterization of radiological threats. This approach is necessary since a high efficiency HPGe detector can only be built as an array due to limitations in growing large germanium crystals. The system is ruggedized and shock mounted for use in a variety of field applications. This paper reports on results from initial field measurements conducted in a truck and on two different boats.

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

    PubMed

    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).

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

    NASA Astrophysics Data System (ADS)

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

    2015-04-01

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

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

    NASA Technical Reports Server (NTRS)

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

    1985-01-01

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

  16. 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

  17. Enhanced microwave dielectric properties of Ba0.4Sr0.6TiO3 ceramics doping by metal Fe powders

    NASA Astrophysics Data System (ADS)

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

    2012-11-01

    Ba0.4Sr0.6TiO3 ceramics by adding mental Fe powders have been fabricated via the solid-state reaction method. The microstructures and optical properties of samples are systematically studied in order to establish the effects of Fe powder additives on microwave dielectric properties of Ba0.4Sr0.6TiO3 ceramics by x-ray diffraction, x-ray photoelectron spectroscopy, and optical reflective spectrum. The results show the coexistence of Fe2+ and Fe3+ in Ba0.4Sr0.6TiO3 ceramics, the decrease of O vacancy concentrations, and their incorporation into the B-site (Ti) of the Ba0.4Sr0.6TiO3 host lattice give rise to excellent microwave dielectric properties. All samples have a higher Q value above 290 while maintaining relatively high tunability above 16.6%. In particular, the sample with the composition of x = 0.035 mol has the dielectric constant of 889, Q × f value of 826 (at 1.370 GHz), and tunability of 24%, which are very promising for high power tunable devices. In comparison, Fe2O3 oxide doped Ba0.4Sr0.6TiO3 ceramics with the same molar ratios of Fe exhibit inferior microwave properties. It indicates that additives of the metal Fe powders can more effectively improve dielectric properties of BaxSr1-xTiO3 system than Fe2O3 oxide.

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

    SciTech Connect

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

    2012-11-15

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

  19. 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.

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

    PubMed

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

    2016-01-01

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

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

    PubMed

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

    2016-05-01

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

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

    PubMed

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

    2016-05-01

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

  3. Adiabatic Calorimetry as Support to the Certification of High-Purity Liquid Reference Materials

    NASA Astrophysics Data System (ADS)

    Baldan, A.; Bosma, R.; Peruzzi, A.; van der Veen, A. M. H.; Shimizu, Y.

    2009-02-01

    The certification of high-purity liquid reference materials is supported by several analytical techniques (e.g., gas chromatography, liquid chromatography, Karl Fischer coulometry, inductively coupled plasma mass spectrometry, differential scanning calorimetry, adiabatic calorimetry). Most of them provide information on a limited set of specific impurities present in the sample (indirect methods). Adiabatic calorimetry [1] complementarily provides the overall molar fraction of impurities with sensitivity down to few μmol · mol-1 without giving any information about the nature of the impurities present in the sample (direct method). As the combination of adiabatic calorimetry with one (or more than one) indirect chemical techniques was regarded as an optimal methodology, NMi VSL developed an adiabatic calorimetry facility for the purity determination of high-purity liquid reference materials [2]. Within the framework of collaboration with NMIJ, a benzene-certified reference material (NMIJ CRM 4002) from NMIJ was analyzed by adiabatic calorimetry at NMi VSL. The results of this measurement are reported in this paper. Good agreement with the NMIJ-certified purity value (99.992 ± 0.003) cmol · mol-1 was found. The influence of different data analysis approaches (e.g., extrapolation functions, melting ranges) on the measurement results is reported. The uncertainty of the measured purity was estimated.

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

    PubMed

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

    2014-01-31

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

  5. 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.

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

    PubMed

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

    2014-10-01

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

  7. Fused salt processing of impure plutonium dioxide to high-purity plutonium metal

    SciTech Connect

    Mullins, L.J.; Christensen, D.C.; Babcock, B.R.

    1982-01-01

    A process for converting impure plutonium dioxide (approx. 96% pure) to high-purity plutonium metal (>99.9%) was developed. The process consists of reducing the oxide to an impure plutonium metal intermediate with calcium metal in molten calcium chloride. The impure intermediate metal is cast into an anode and electrorefined to produce high-purity plutonium metal. The oxide reduction step is being done now on a 0.6-kg scale with the resulting yield being >99.5%. The electrorefining is being done on a 4.0-kg scale with the resulting yield being 80 to 85%. The purity of the product, which averages 99.98%, is essentially insensitive to the purity of the feed metal. The yield, however, is directly dependent on the chemical composition of the feed. To date, approximately 250 kg of impure oxide has been converted to pure metal by this processing sequence. The availability of impure plutonium dioxide, together with the need for pure plutonium metal, makes this sequence a valuable plutonium processing tool.

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

    PubMed

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

    2016-07-20

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

  9. 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.

  10. 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.

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

    SciTech Connect

    Helminiak, Yanar NM

    2009-12-01

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

  12. 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.

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

    PubMed

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

    2009-06-01

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

  14. 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

  15. 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.

  16. Extraction-spectrometric determination of lead in high-purity aluminium salts.

    PubMed

    Koksal, Jiří; Synek, Václav; Janos, Pavel

    2002-08-23

    Trace amounts of lead were determined in high purity aluminium salts (especially in ammonium aluminium sulfate) using inductively coupled plasma-optical emission spectrometry (ICP-OES) after extractive pre-concentration and matrix separation. Metals were extracted from the aluminium matrix in the form of chelates with ammonium pyrolidine dithoocarbamate into methyl isobutyketone. The organic extract was digested with nitric acid and hydrogen peroxide. The limit of detection for the determination of lead in crystalline ammonium aluminium sulfate was ca. 0.044 mug g(-1). The relative expanded uncertainty of the lead determination was ca. 23% at the level of 0.2 mug g(-1) and ca. 16% at the level of 1.0 mug g(-1). The main uncertainty contribution was associated with repeatability of the whole analytical procedure. PMID:18968757

  17. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2016-04-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-08-01

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

  1. 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.

  2. 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.

  3. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2010-03-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2016-07-01

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

  6. 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.

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

    PubMed

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

    2016-01-01

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

  8. 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.

  9. 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.

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

    NASA Technical Reports Server (NTRS)

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

    1958-01-01

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

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

    PubMed

    Zhang, Weijiang; Liu, Tianyu; Xu, Jiao

    2016-01-01

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

  12. High Purity Germanium Detectors and Angular Distribution of 2Al(p,g)28Si

    NASA Astrophysics Data System (ADS)

    Wilson, Andre

    2014-09-01

    The purpose of this research was to study high purity germanium detector systems, and to calculate and compare absorption ratios of 27Al(p,g)28Si. Work with the germanium detector online array for gamma ray spectroscopy in nuclear astrophysics in the Nuclear Science Laboratory at the University of Notre Dame, also known as Georgina, including energy calibrations and work with software and hardware logic, provided the necessary background and experience with high purity germanium detectors and angular distribution of gamma rays. The knowledge taken from work with the Georgina detectors was then applied to the analysis of 27Al(p,g)28Si. Previous experimental data of 27Al(p,g)28Si was analyzed using the Ep = 1778.9 keV resonance. The data used was taken from a 2010 experiment completed in the Nuclear Science Laboratory at the University of Notre Dame using the 4MV KN particle accelerator. A 1977 paper by A. Anttila and J. Keinonen with analysis of the same reaction using the Ep = 992 keV resonance was used for the energy calibration and gamma energies. Peak fitting and background reduction of the spectra were completed using analysis software, jtek. Angular distribution ratios from a 56Co source were used for the normalization of the 27Al data. Angular dependent absorption factors were used to analyze the angular distribution of γ-rays from the 27Al beam target. With these absorption factors, relative gamma intensity measurements of 27Al(p,g)28Si were calculated.

  13. 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.

  14. 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.

  15. Enhanced production of human serum albumin by fed-batch culture of Hansenula polymorpha with high-purity oxygen.

    PubMed

    Youn, Jong Kyu; Shang, Longan; Kim, Moon Il; Jeong, Chang Moon; Chang, Ho Nam; Hahm, Moon Sun; Rhee, Sang Ki; Kang, Hyun Ah

    2010-11-01

    Fed-batch cultures of Hansenula polymorpha were studied to develop an efficient biosystem to produce recombinant human serum albumin (HSA). To comply with this purpose, we used high purity oxygen supplying strategy to increase viable cell density in a bioreactor and enhance the production of target protein. A mutant strain, H. polymorpha GOT7 was utilized in this study as a host strain in both 5-L and 30-L scale fermentors. To supply high purity oxygen into a bioreactor, nearly 100 % high purity oxygen from commercial bomb or higher than 93 % oxygen available in-situ from a pressure swing adsorption oxygen generator (PSA) was employed. Under the optimal fermentation of H. polymorpha with high purity oxygen, the final cell densities and produced HSA concentrations were 24.6 g/L and 5.1 g/L in the 5-L fermentor, and 24.8 g/L and 4.5 g/L in the 30-L fermentor, respectively. These were about 2-10 times higher than those obtained in air-based fed-batch fermentations. The discrepancies between the 5-L and 30-L fermentors with air supply were presumably due to the higher contribution of surface aeration over submerged aeration in the 5-L fermentor. This study, therefore, proved the positive effect of high purity oxygen to enhance viable cell density as well as target recombinant protein production in microbial fermentations. PMID:21124059

  16. 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.

  17. 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

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

    PubMed

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

    2016-11-01

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

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

    PubMed

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

    2016-09-01

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

  20. Characterization of High-purity Germanium Crystals for Rare Event Physics Program

    NASA Astrophysics Data System (ADS)

    Smith, Miranda

    2012-10-01

    Germanium detectors are made with high-purity crystals grown in a hydrogen atmosphere at the University of South Dakota. Before these crystals can be effectively utilized, they need to be characterized for their purity, dislocation density and carrier mobility. These measurements will provide feedback to improve the crystal growth process. X-ray diffraction is used to determine the orientation of grown crystals and quality of crystalline structure. Dislocations occur when the crystal lattice structure of the germanium does not stay uniform throughout the layers. Dislocation density should be within a range of 100-10,000/cm^3 in order to avoid hydrogen-bonding issues. Our group has achieved acceptable dislocation densities of 3294/cm^2 and 7361/cm^2. The crystals have reached purity levels of 99.99999999999%, but remaining unintentional impurities need to be identified to verify their nature and source. We used Photothermal Ionization Spectroscopy to determine shallow level impurities. These results are incorporated with the Van Der Pauw Hall Effect measurement, which is used to determine whether the crystal is n-type or p-type, as well as the carrier concentration and mobility. The dominant impurities are Al, B, and P. We show an entire calibration program in our research group.

  1. 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.

  2. Detection of gamma rays using a coupled array of high-purity germanium detectors

    NASA Astrophysics Data System (ADS)

    Debiak, T. W.; Bocskor, S. J.; D'Agostino, M. D.; Schneid, E. J.; Hughlock, B. W.

    1990-12-01

    The characteristics of a seven-element hexagonal close-packed array of high-purity germanium detectors were measured. The energy resolution or full width at half maximum (FWHM) and full width at 10 percent maximum (FW.1M) were measured in both the uncoupled mode and the sum-coincidence mode between 333 keV and 2.612 MeV. The fractional peak efficiency improvement obtained in sum-coincidence mode compared with the uncoupled mode increased from 0 percent at 80 keV to 19.7 percent at 2.612 MeV. A Monte Carlo code developed to compare these results with theoretical models shows substantial agreement with experiments from 80 keV to 1.332 MeV. A description of the detector, signal processing electronics, data acquisition system, and software is given. A technique based on real-time compensation of gain and offset drift is developed to minimize the peak broadening in real-time sum-coincidence spectra. This technique allows data acquisition to commence shortly after turn-on while the system approaches temperature stabilization.

  3. 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.

  4. Recovery of high-purity metallic Pd from Pd(II)-sorbed biosorbents by incineration.

    PubMed

    Won, Sung Wook; Lim, Areum; Yun, Yeoung-Sang

    2013-06-01

    This work reports a direct way to recover metallic palladium with high purity from Pd(II)-sorbed polyethylenimine-modified Corynebacterium glutamicum biosorbent using a combined method of biosorption and incineration. This study is focused on the incineration part which affects the purity of recovered Pd. The incineration temperature and the amount of Pd loaded on the biosorbent were considered as major factors in the incineration process, and their effects were examined. The results showed that both factors significantly affected the enhancement of the recovery efficiency and purity of the recovered Pd. SEM-EDX and XRD analyses were used to confirm that Pd phase existed in the ash. As a result, the recovered Pd was changed from PdO to zero-valent Pd as the incineration temperature was increased from 600 to 900°C. Almost 100% pure metallic Pd was recovered with recovery efficiency above 99.0% under the conditions of 900°C and 136.9 mg/g.

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

    NASA Astrophysics Data System (ADS)

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

    2016-08-01

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

  6. 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.

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

    PubMed

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

    2016-01-01

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

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

    NASA Technical Reports Server (NTRS)

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

    1976-01-01

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

  9. 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.

  10. Viral validation of the manufacturing process of high purity albumin from placentas.

    PubMed

    Grandgeorge, M; Véron, J L

    1993-01-01

    We report on the viral validation of an industrial purification process which is used to manufacture high purity human albumin from frozen placentas. This process has been used without any modification since 1980 except for a progressive increase in production scale to reach a capacity of 19 tons of placentas per day. The extraction purification process includes five alcohol manufacturing steps, some with strict conditions of alcohol concentration, acid pH, temperature and one including chloroform. These steps are followed by three chromatographies. Albumin is finally submitted to pasteurization both in bulk and in the final container. Selected steps of this process have been tested for their ability to remove or inactivate viruses. Viruses used were HBV, HIV-1, HIV-2 and model viruses poliovirus, avian reovirus, MuLV, Sindbis, SV40 and Aujeszky's. In vitro infectivity titration assays were used for all viruses except for HBV where DNA and antigen titrations were performed. Reduction factors obtained were from 10 to 29 log10 depending on the viral marker. Moreover, testing done on regular production batches demonstrated the absence of HBV, HIV-1 and HCV genomic sequence in the final lots. Viral risk calculation for HBV, HIV-1 and HCV was made considering the maximal theoretically possible contamination of the starting material. This calculation showed the very large safety margin the manufacturing process with respect to virus transmission for these viruses or possibly other unknown ones.

  11. 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.

  12. 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.

  13. 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.

  14. 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.

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

    SciTech Connect

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

    2014-10-01

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

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

    PubMed

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

    2013-04-23

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

  17. Resistivity recovery in high purity iron after fission- and fusion- neutron irradiation*1

    NASA Astrophysics Data System (ADS)

    Matsui, H.; Takehana, S.; Guinan, M. W.

    1988-07-01

    A resistometric study of high-purity iron has been performed after irradiation at 20 K by 14 MeV neutrons in RTNS-II or by fission neutrons in Kyoto University Reactor (KUR). The annealing behavior of iron after fusion neutrons is very different from that after electron irradiation. The fractional recovery in stage I is much smaller and the recovery of vacancy type defects starts to occur at a much lower temperature with a lower activation energy than after electron iradiation. The difference between fission and fusion neutron irradiation, however, is much smaller; the isochronal curves for these two types of irradiation are essentially the same below 170 K. It is concluded that the local defect configuration for these two types of irradiation is similar. The induced resistivity by fusion neutrons is about a factor of 2 larger than by fission neutrons (fluence for E > 1 MeV). This is in accord with a rough estimation of the ratio of damage energy cross sections.

  18. 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

  19. 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.

  20. Functionally competent eosinophils differentiated ex vivo in high purity from normal mouse bone marrow

    PubMed Central

    Dyer, Kimberly D.; Moser, Jennifer M.; Czapiga, Meggan; Siegel, Steven J.; Percopo, Caroline M.; Rosenberg, Helene F.

    2009-01-01

    We have devised an ex vivo culture system which generates large numbers of eosinophils at high purity (>90%) from unselected mouse bone marrow progenitors. In response to four days of culture with recombinant mouse (rm)FLT3-L and rmSCF followed by rmIL-5 alone thereafter, the resulting bone-marrow derived eosinophils (bmEos) express immunoreactive major basic protein, Siglec F, IL-5 receptor alpha chain, and transcripts encoding mouse eosinophil peroxidase, CC chemokine receptor 3, the IL-3/IL-5/GMCSF receptor common beta-chain (βc), and the transcription factor GATA-1. BmEos are functionally competent: they undergo chemotaxis toward mouse eotaxin-1 and produce characteristic cytokines, including interferon-γ, IL-4, MIP-1α and IL-6. The rodent pathogen, pneumonia virus of mice (PVM) replicates in bmEos, and elevated levels of IL-6 are detected in supernatants of bmEos cultures in response to active infection. Finally, differentiating bmEos are readily transfected with lentiviral vectors, suggesting a means for rapid production of genetically manipulated cells. PMID:18768855

  1. Mechanisms of stress-corrosion cracking of alloy X-750 in high-purity water

    SciTech Connect

    Grove, C.A.; Petzold, L.D.

    1985-09-01

    The high-strength, nickel-base alloy X-750 is susceptible to stress-corrosion cracking (SCC) in high-purity, deaerated water. Crack initiation occurs at high temperatures (>400F (204C)). Crack propagation occurs in both high-temperature and lowtemperature (<300F(149C)) water. High-temperature crack growth rates are on the order of mils per day. Low-temperature cracking is extremely rapid (approx. =100 in. (250 cm) per day). Three heat treatments of Alloy X-750 are investigated: stress equalized1625F (885C)/24 hours + 1300F (704C)/20 hours, direct aged-1300F (704C)/24 hours, and solution annealed and direct aged-2000F (1093C)/ 1 hour + 1300F (704C)/20 hours. Stress-equalized Alloy X-750 is most susceptible to SCC; solution-annealed and direct-aged Alloy X-750 is least susceptible. A hydrogen embrittlement model of SCC is developed that predicts SCC performance on the basis of grain boundary chemistry and grain boundary carbides. Phosphorus segregates to the grain boundary in concentrations of up to approx. =100 times the bulk concentration during processing and heat treatment. Phosphorus at the grain boundaries increases susceptibility to high- and low-temperature SCC. The presence of M23C6-type carbides and/or the absence of MC-type carbides at the grain boundaries improves SCC performance in high-temperature water.

  2. Mechanism of stress-corrosion cracking of Alloy X-750 in high purity water

    SciTech Connect

    Grove, C.A.; Petzold, L.D.

    1985-11-01

    The high strength Ni-base Alloy X-750 is susceptible to stress-corrosion cracking (SCC) in high purity, deaerated water. Crack initiation occurs at high temperatures (>400F). Crack propagation occurs in both high-temperature and low-temperature (<300F) water. High-temperature crack growth rates are on the order of mils/day. Low-temperature cracking is extremely rapid (approx.100 in./day). Three heat treatments of Alloy X-750 are investigated: (1) Stress Equalized - 1625F/24 hr + 1300F/20 hr, (2) Direct Aged - 1300F/24 hr, and (3) Solution Annealed and Direct Aged - 2000F/1 hr + 1300F/20 hr. Stress-equalized Alloy X-750 is most susceptible to SCC; solution-annealed and direct-aged Alloy X-750 is least susceptible. A Hydrogen Embrittlement Model of SCC is developed that predicts SCC performance on the basis of grain boundary chemistry and grain boundary carbides. Phosphorus segregates to the grain boundary in concentrations of up to approx.100 times the bulk concentration during processing and heat treatment. Phosphorus at the grain boundaries increases susceptibility to high- and low-temperature SCC. The presence of M23C6-type carbides and/or the absence of MC-type carbides at the grain boundaries improves SCC performance in high-temperature water. 18 figs., 5 tabs.

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

    PubMed

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

    2009-09-01

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

  4. 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.

  5. A process for preparation of 'high-purity' factor VIII by controlled pore glass treatment.

    PubMed

    Margolis, J; Gallovich, C M; Rhoades, P

    1984-01-01

    A simple process for large-scale manufacture of 'high-purity' factor VIII is described in detail. A crude concentrate prepared from washed cryo is treated with controlled pore glass (CPG, 500 A pore diameter) in proportion of 20-30 ml of CPG to 1 g input of protein. The slurry is poured into a separation column and the effluent purified concentrate collected. The remaining factor VIII in the void volume is displaced by a wash solution. After passage through a 0.2 micron membrane filter the product is dispensed and lyophilized. Maintaining the operating pH at 6.5-6.7 and adding synthetic amino acids improved the yield and solubility. The current concentrate contains 1 unit of factor VIII per mg protein (10 units mg fibrinogen) with a recovery of 250 units/kg plasma. The CPG stage is non-destructive, yielding more than 90% of the input factor VIII. In 1980-1983, more than 3 X 10(6) units have been used in New South Wales, mostly for massive cover in surgical patients. In collaboration with the Commonwealth Serum Laboratories, it is intended to expand production for use in other Australian States.

  6. 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.

  7. 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.

  8. 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

  9. 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.

  10. 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.

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

    NASA Astrophysics Data System (ADS)

    Angle, Jesse Isaac

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

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

    PubMed

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

    2016-08-24

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

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. Characterization of Fine Powders

    NASA Astrophysics Data System (ADS)

    Krantz, Matthew; Zhang, Hui; Zhu, Jesse

    Fine powders are used in many applications and across many industries such as powdered paints and pigments, ceramics, petrochemicals, plastics, pharmaceuticals, and bulk and fine chemicals, to name a few. In addition, fine powders must often be handled as a waste by-product, such as ash generated in combustion and gasification processes. In order to correctly design a process and process equipment for application and handling of powders, especially fine powders, it is essential to understand how the powder would behave. Many characterization techniques are available for determining the flow properties of powders; however, care must be taken in selecting the most appropriate technique(s).

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

    PubMed

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

    2012-04-01

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

  19. 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.

  20. 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

  1. Synthesis of MgO-CaO-Al2O3-SiO2 nanocomposite powder by polymeric complex method as a novel sintering additive of AlN ceramics

    NASA Astrophysics Data System (ADS)

    Lee, Hwa-Jun; Cho, Woo-Seok; Kim, Hyeong Jun; Pan, Wei; Shahid, Mohammad; Ryu, Sung-Soo

    2016-09-01

    A MgO-CaO-Al2O3-SiO2 (MCAS) nanocomposite powder with a particle size of 50 nm and a specific surface area of 40.6 m2/g was successfully synthesized via heat-treatment of polymeric precursors containing Mg, Ca, Al and Si in air at 700 °C for 5 h. It was characterized as a novel sintering additive for the densification AlN ceramics at a low temperature below 1600 °C. It was found that the nanosized MCAS powder was suitable for the densification of AlN ceramics. In particular, full densification could be achieved when only 1.0 wt% MCAS additive-doped AlN powder compact was sintered for 1 h at 1600 °C, and a thermal conductivity of 84 W/m·K was attained.

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

    PubMed

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

    2016-08-01

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

  3. 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.

  4. 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.

  5. Local deposition of high-purity Pt nanostructures by combining electron beam induced deposition and atomic layer deposition

    SciTech Connect

    Mackus, A. J. M.; Sanden, M. C. M. van de; Kessels, W. M. M.; Mulders, J. J. L.

    2010-06-15

    An approach for direct-write fabrication of high-purity platinum nanostructures has been developed by combining nanoscale lateral patterning by electron beam induced deposition (EBID) with area-selective deposition of high quality material by atomic layer deposition (ALD). Because virtually pure, polycrystalline Pt nanostructures are obtained, the method extends the application possibilities of EBID, whereas compared to other area-selective ALD approaches, a much higher resolution is attainable; potentially down to sub-10 nm lateral dimensions.

  6. 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.

  7. Lightweight ceramic insulation and method

    NASA Technical Reports Server (NTRS)

    Green, David J. (Inventor)

    1990-01-01

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

  8. 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

  9. Gelcasting superalloy powders

    SciTech Connect

    Janney, M.A.

    1995-12-31

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

  10. 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.

  11. 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.

  12. 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.

  13. Novel proton-exchange membrane based on single-step preparation of functionalized ceramic powder containing surface-anchored sulfonic acid

    NASA Astrophysics Data System (ADS)

    Reichman, S.; Burstein, L.; Peled, E.

    2008-05-01

    A novel approach to the synthesis of a low-cost proton-exchange membrane (PEM) based on the single-step preparation of a functionalized ceramic powder containing surface-anchored sulfonic acid (SASA) and a polymer binder, is presented for the first time. The added value of this technique, compared with earlier work published by our group, is the adoption of a direct, single-step synthesis, as opposed to a multiple-step synthesis. The latter requires an oxidation step, in order to convert the thiol group into a sulfonic group. SASA powders of different compositions have been prepared and characterized by means of Brunaur-Emmet-Teller (BET), thermogravimetric analysis-differential thermal analysis (TGA-DTG), differential scanning calorimeter (DSC), Fourier transformation infrared (FT-IR), nuclear magnetic resonance (NMR), X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), scanning electron microscopy (SEM) and electrochemical techniques. The lowest equivalent weight measured for SASA powders is 1281 g equiv.-1. The ionic conductivity of a 100-μm-thick membrane is measured ex situ at room temperature (25 ± 3 °C) and the highest proton conductivity is 48 mS cm-1. The typical pore size, for the SASA powders is less than 10 nm and ranges from 2 to 50 nm for the SASA-based membranes. The membranes are thermally stable up to 250 °C. Direct methanol fuel cells (DMFCs) are assembled with some of the membranes. Preliminary tests showed that the cell resistance for a ∼100-μm-thick membrane ranges between 0.29 and 0.19 Ω cm2 from 80 to 130 °C, respectively, and that the maximum cell power density with a 1 M methanol solution is 127, 208 and 290 mW cm-2 at 80, 110 and 130 °C, respectively, while the corresponding methanol crossover current density is 0.093, 0.238 and 0.281 A cm-2.

  14. A sintering study on the β-spodumene-based glass ceramics prepared from gel-derived precursor powders with LiF additive

    NASA Astrophysics Data System (ADS)

    Wang, Moo-Chin; Wu, Nan-Chung; Yang, Sheng; Wen, Shaw-Bing

    2002-01-01

    Beta-spodumene (Li2O·Al2O3·4SiO2, LAS) powders were prepared by a sol-gel process using Si(OC2H5)4, Al(OC4H9)3, and LiNO3 as precursors and LiF as a sintering aid agent. Dilatometry, X-ray diffraction (XRD), scanning electron microscopy (SEM), scanning transmission electron microscopy (STEM), and electron diffraction (ED) were utilized to study the sintering, phase transformation, microstructure, and properties of the β-spodumene glass-ceramics prepared from the gel-derived precursor powders with and without LiF additives. For the LAS precursor powders containing no LiF, the only crystalline phase obtained was β-spodumene. For the pellets containing less than 4 wt pct LiF and sintered at 1050 °C for 5 hours the crystalline phases were β-spodumene and β-eucryptite (Li2O·Al2O3·2SiO2). When the LiF content was 5 wt pct and the sintering process was carried out at 1050 °C for 5 hours, the crystalline phases were β-spodumene, β-eucryptite (triclinic), and eucryptite (rhombohedral (hex.)) phases. With the LiF additive increased from 0.5 to 4 wt pct and sintering at 1050 °C for 5 hours, the open porosity of the sintered bodies decrease from 30 to 2.1 pct. The grains size is about to 4 to 5 µm when pellect LAS compact contains LiF 3 wt pct as sintered at 1050 °C for 5 hours. The grains size grew to 8 to 25 µm with a remarkable discontinuous grain growth for pellet LAS compact contain LiF 5 wt pct sintered at 1050 °C for 5 hours. Relative densities greater than 90 pct could be obtained for the LAS precursor powders with LiF > 2 wt pct when sintered at 1050 °C for 5 hours. The coefficient of thermal expansion of the sintered bodies decreased from 8.3 × 10-7 to 5.2 × 10-7/°C (25 °C to 900 °C) as the LiF addition increased from 0 to 5 wt pct.

  15. 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.

  16. 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.

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

    PubMed

    Zverev, V I; Tishin, A M; Chernyshov, A S; Mudryk, Ya; Gschneidner, K A; Pecharsky, V K

    2014-02-12

    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. PMID:24451321

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

    PubMed

    Zverev, V I; Tishin, A M; Chernyshov, A S; Mudryk, Ya; Gschneidner, K A; Pecharsky, V K

    2014-02-12

    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.

  19. 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.

  20. 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

  1. 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

  2. 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.

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

    NASA Astrophysics Data System (ADS)

    Curecheriu, L. P.; Buscaglia, M. T.; Buscaglia, V.; Mitoseriu, L.; Postolache, P.; Ianculescu, A.; Nanni, P.

    2010-05-01

    In the present work, diphasic ceramic composites with core-shell nanostructures formed by Ni0.50Zn0.50Fe2O4 core and BaTiO3 shell were investigated. Their properties were compared with those of composites prepared by coprecipitation. The core-shell structure was confirmed by microstructural powder analysis. Homogeneous microstructures with a good phase mixing and percolated dielectric phase by the magnetic one were obtained from coprecipitated powders. Less homogeneous microstructures resulted in ceramics produced from the powder prepared by core-shell method, with isolated small ferrite grains besides large ferrite aggregates embedded into the BaTiO3 matrix. Both the ferroelectric and magnetic phases preserve their basic properties in bulk composite form. However, important differences in the dielectric relaxation and conduction mechanisms were found as result of the microstructural difference. Extrinsic contributions play important roles in modifying the electric properties in both ceramics, causing space charge effect, Maxwell-Wagner relaxations and hopping conductivity, mainly due to the ferrite low resistivity phase. The conductivity and dielectric modulus spectra analysis allowed to identify different polaron contributions associated with the microstructural differences. It results that by using the core-shell method, improved dielectric properties and limited hopping contributions can be realized.

  4. Evaluation of New Contact Technology for A Planar High-Purity Germanium Double-Sided Strip Detector

    NASA Astrophysics Data System (ADS)

    Jackson, E.; Chowdhury, P.; Lister, C. J.; Diaz, C.; Skinner, M.; Hull, E.; Pehl, R.

    2013-10-01

    New technologies for making position sensitive γ-ray detectors have applications in space science, medical imaging, homeland security, and nuclear structure research. One promising approach uses high-purity germanium wafers in Low Energy Photon Spectrometer (LEPS) geometry, where segmentation of the electrodes into strips forms a Double-Sided Strip Detector (DSSD). The position-sensitivity afforded by the many strips is ideal for the study of Compton scattering and polarization. However, challenges with the manufacture and performance of the rectifying contacts continue to plague the advancement of planar DSSDs. The data gathered from the combination of multiple strips' signals suffers from cross-talk between the strips and charge loss due to wide inter-strip gaps. A planar, high-purity DSSD has been developed by PHDs Co. with an alternative electrode material, amorphous germanium, that can be placed such that the gaps between the strips are half the width required by other contact material. This research seeks to quantify the performance gains of the amorphous germanium contacts and smaller inter-strip gaps while exploring the possibilities for this DSSD as an imager and polarization detector. Research supported by the U.S. Department of Energy (DE-FG02-94ER40848).

  5. All electrochemical fabrication of a bilayer membrane composed of nanotubular photocatalyst and palladium toward high-purity hydrogen production

    NASA Astrophysics Data System (ADS)

    Hattori, Masashi; Noda, Kei

    2015-12-01

    We developed an all-electrochemical technique for fabricating a bilayer structure of a titanium dioxide (TiO2) nanotube array (TNA) and a palladium film (TNA/Pd membrane), which works for photocatalytic high-purity hydrogen production. Electroless plating was used for depositing the Pd film on the TNA surface prepared by anodizing a titanium foil. A 3-μm-thick TNA/Pd membrane without any pinholes in a 1.5-cm-diameter area was fabricated by transferring a 1-μm-thick TNA onto an electroless-plated 2-μm-thick Pd film with a mechanical peel-off process. This ultrathin membrane with sufficient mechanical robustness showed photocatalytic H2 production via methanol reforming under ultraviolet illumination on the TNA side, immediately followed by the purification of the generated H2 gas through the Pd layer. The hydrogen production rate and the apparent quantum yield for high-purity H2 production from methanol/water mixture with the TNA/Pd membrane were also examined. This work suggests that palladium electroless plating is more suitable and practical for preparing a well-organized TNA/Pd heterointerface than palladium sputter deposition.

  6. Tensile properties and interfacial bonding of multi-layered, high-purity titanium strips fabricated by ARB process.

    PubMed

    Ghafari-Gousheh, Soroush; Nedjad, Syamak Hossein; Khalil-Allafi, Jafar

    2015-11-01

    Severe plastic deformation (SPD) processing has shown very effective in promotion of mechanical properties of metals and alloys. In this study, the results of investigating mechanical properties and also inter-layer bond performance of accumulative roll bonded high purity titanium (HP-Ti) strips are presented. High purity titanium plates were severely deformed by use of a combination of cold rolling (CR) to a thickness reduction of approximately 87% and then accumulative roll bonding (ARB) for three cycles (N=3) at ambient temperature. Optical and scanning electron microscopy, tensile testing, and hardness measurements were conducted. The ARB strips exhibited lower tensile strength and ductility in comparison to cold rolled one which can basically be attributed to the poor function of the latest bonds established in the centerlines of the strips. Fractographic examinations revealed the interfacial de-bonding along the centerline between the layers having undergone roll bonding for just one cycle. It was while the interfaces having experienced roll bonding for more cycles showed much higher resistance against delaminating. PMID:26253205

  7. 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.

  8. 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.; Giaquinto, J.; Krichinsky, A. M.

    2015-08-20

    Several high-purity 233U items potentially useful as isotope dilution mass spectrometry standards for safeguards, non-proliferation, and nuclear forensics measurements are identified and rescued from downblending. By preserving the supply of 233U materials of different pedigree for use as source materials for certified reference materials (CRMs), it is ensured that the safeguards community has high quality uranium isotopic standards required for calibration of the analytical instruments. One of the items identified as a source material for a high-purity CRM is characterized for the uranium isotope-amount ratios using thermal ionization mass spectrometry (TIMS). Additional verification measurements on this material using quadrupole inductivelymore » coupled plasma mass spectrometry (ICPMS) are also performed. As a result, the comparison of the ICPMS uranium isotope-amount ratios with the TIMS data, with much smaller uncertainties, validated the ICPMS measurement practices. ICPMS is proposed for the initial screening of the purity of items in the rescue campaign.« less

  9. 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. PMID:27589920

  10. 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.

  11. 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

  12. Silicon nitride/silicon carbide composite densified materials prepared using 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.

    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.

  13. Piezoelectric Properties of Li-Doped (K0.48Na0.52)NbO3 Ceramics Synthesized Using Hydrothermally-Derived KNbO3 and NaNbO3 Fine Powders

    NASA Astrophysics Data System (ADS)

    Maeda, Takafumi; Hemsel, Tobias; Morita, Takeshi

    2012-09-01

    [Lix(Na0.52K0.48)1-x]NbO3 (0 ≤x ≤0.091) ceramics were synthesized using hydrothermal powders and the lithium doping content was controlled to optimize their piezoelectric properties. The raw KNbO3 and NaNbO3 powders were obtained separately by a hydrothermal method and LiNbO3 powders were prepared by milling a commercial LiNbO3 single crystal. These powders were mixed with ethanol at a molar ratio LiNbO3: (Na0.52K0.48)NbO3= x : 1-x. The synthesized powders were sintered at 1060-1120 °C for 2 h. We succeeded in obtaining highly dense [Lix(Na0.52K0.48)1-x]NbO3 ceramics using hydrothermal powder. The X-ray diffraction patterns revealed that the crystal phase changed from orthorhombic to tetragonal at around x = 0.06. At this morphotropic phase boundary (MPB), the c/a ratio changed from 1.016 to 1.024 and the highest piezoelectric constant was obtained with the chemical component of [Li0.065(K0.48Na0.52)0.935]NbO3. The obtained piezoelectric properties were as follows: k33 = 0.51, ɛ33T/ɛ0 = 836, c33E = 46 GPa, d33 = 203 pC/N, and Tc = 482 °C.

  14. Performance of A Compact Multi-crystal High-purity Germanium Detector Array for Measuring Coincident Gamma-ray Emissions

    SciTech Connect

    Howard, Chris; Daigle, Stephen; Buckner, Matt; Erikson, Luke E.; Runkle, Robert C.; Stave, Sean C.; Champagne, Art; Cooper, Andrew; Downen, Lori; Glasgow, Brian D.; Kelly, Keegan; Sallaska, Anne

    2015-02-18

    The Multi-sensor Airborne Radiation Survey (MARS) detector is a 14-crystal array of high-purity germanium (HPGe) detectors housed in a single cryostat. The array was used to measure the astrophysical S-factor for the 14N(p,γ)15O* reaction for several transition energies at an effective center of mass energy of 163 keV. Owing to the segmented nature of the MARS detector, the effect of gamma-ray summing was greatly reduced in comparison to past experiments which utilized large, single-crystal detectors. The new S-factor values agree within the uncertainties with the past measurements. Details of the analysis and detector performance will be presented.

  15. A hybrid-membrane migration method to isolate high-purity adipose-derived stem cells from fat tissues

    PubMed Central

    Higuchi, Akon; Wang, Ching-Tang; Ling, Qing-Dong; Lee, Henry Hsin-chung; Kumar, S. Suresh; Chang, Yung; Alarfaj, Abdullah A.; Munusamy, Murugan A.; Hsu, Shih-Tien; Wu, Gwo-Jang; Umezawa, Akihiko

    2015-01-01

    Human adipose-derived stem cells (hADSCs) exhibit heterogeneous characteristics, indicating various genotypes and differentiation abilities. The isolated hADSCs can possess different purity levels and divergent properties depending on the purification methods used. We developed a hybrid-membrane migration method that purifies hADSCs from a fat tissue solution with extremely high purity and pluripotency. A primary fat-tissue solution was permeated through the porous membranes with a pore size from 8 to 25 μm, and the membranes were incubated in cell culture medium for 15-18 days. The hADSCs that migrated from the membranes contained an extremely high percentage (e.g., >98%) of cells positive for mesenchymal stem cell markers and showed almost one order of magnitude higher expression of some pluripotency genes (Oct4, Sox2, Klf4 and Nanog) compared with cells isolated using the conventional culture method. PMID:25970301

  16. 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.

  17. High purity H2 by sorption-enhanced chemical looping reforming of waste cooking oil in a packed bed reactor.

    PubMed

    Pimenidou, P; Rickett, G; Dupont, V; Twigg, M V

    2010-12-01

    High purity hydrogen (>95%) was produced at 600 degrees C and 1 atm by steam reforming of waste cooking oil at a molar steam to carbon ratio of 4 using chemical looping, a process that features redox cycles of a Ni catalyst with the in-situ carbonation/calcination of a CO(2) sorbent (dolomite) in a packed bed reactor under alternated feedstreams of fuel-steam and air. The fuel and steam conversion were higher with the sorbent present than without it. Initially, the dolomite carbonation was very efficient (100%), and 98% purity hydrogen was produced, but the carbonation decreased to around 56% with a purity of 95% respectively in the following cycles. Reduction of the nickel catalyst occurred alongside steam reforming, water gas shift and carbonation, with H(2) produced continuously under fuel-steam feeds. Catalyst and CO(2)-sorbent regeneration was observed, and long periods of autothermal operation within each cycle were demonstrated.

  18. 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.

  19. Pitting Corrosion in CVD SiC at 300°C in Deoxygenated High-Purity Water

    SciTech Connect

    Henager, Charles H.; Schemer-Kohrn, Alan L.; Pitman, Stan G.; Senor, David J.; Geelhood, Ken J.; Painter, Chad L.

    2008-08-15

    SiC is a candidate for nuclear applications at elevated temperatures but has not been fully studied under typical light-water reactor operating conditions, such as moderate temperatures and high pressures. Coupons of high-purity chemical vapor deposited SiC were exposed to deoxygenated, pressurized water at 573K and 100 Bar for up to 4000 hours. Ceramographic examination of the exposed SiC surfaces revealed both embryonic and large, d > 300 µm, pits on the surface. The pits were characterized using scanning electron microscopy for structure and chemistry analysis. Pit densities were also determined by standard counting methods. The chemical analysis revealed that the pits are associated with the formation of silica and subsequent loss of Si, which is expected due to several suggested reactions between SiC and water.

  20. Phase transformations of high-purity PbI2 nanoparticles synthesized from lead-acid accumulator anodes

    NASA Astrophysics Data System (ADS)

    Malevu, T. D.; Ocaya, R. O.; Tshabalala, K. G.

    2016-09-01

    High-purity hexagonal lead iodide nanoparticles have been synthesized from a depleted sealed lead acid battery anode. The synthesized product was found to consist of the rare 6R polytype form of PbI2 that is thought to have good potential in photovoltaic applications. We investigate the effects of annealing time and post-melting temperature on the structure and optical properties using 1.5418 Å CuKα radiation. Photoluminescence measurements were done under 150 W/221 nm wavelength xenon excitation. Phase transformation was observed through XRD peaks when annealing time increased from 0.5-5 h. The nanoparticle grain size and inter-planar distance appeared to be independent of annealing time. PL measurements show three broad peaks in a range of 400 nm to 700 nm that are attributed to excitonic, donor-acceptor pair and luminescence bands from the deep levels.

  1. Synthesis and optical properties of high-purity CoO nanowires prepared by an environmentally friendly molten salt route

    NASA Astrophysics Data System (ADS)

    Wang, Wenzhong; Zhang, Guling

    2009-08-01

    CoO nanowires with diameters of 50 _80 nm, and lengths of up to more than 5 μm have been successfully synthesized by a simple environmentally friendly molten salt route, in which the precursor CoCO 3 nanoparticles are decomposed to form high-purity CoO nanowires in NaCl flux. The structure features and morphology of the as-prepared CoO nanowires were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution TEM (HRTEM), and selected area electron diffraction (SAED). The chemical composition and oxidation state of the prepared nanowires were systemically studied by X-ray photoelectron spectra (XPS) and laser Raman spectroscopy. The results indicated that the as-prepared CoO nanowires were composed of pure cubic CoO phase. The growth mechanism of the synthesized nanowires was also discussed in detail based on the experimental results.

  2. Performance of a compact multi-crystal high-purity germanium detector array for measuring coincident gamma-ray emissions

    NASA Astrophysics Data System (ADS)

    Howard, Chris; Daigle, Stephen; Buckner, Matt; Erikson, Luke E.; Runkle, Robert C.; Stave, Sean C.; Champagne, Arthur E.; Cooper, Andrew; Downen, Lori; Glasgow, Brian D.; Kelly, Keegan; Sallaska, Anne

    2015-05-01

    The Multi-sensor Airborne Radiation Survey (MARS) detector is a 14-crystal array of high-purity germanium (HPGe) detectors housed in a single cryostat. The array was used to measure the astrophysical S-factor for the 14N(p,γ)15O* reaction for several transition energies at an effective center-of-mass energy of 163 keV. Owing to the granular nature of the MARS detector, the effect of gamma-ray summing was greatly reduced in comparison to past experiments which utilized large, single-crystal detectors. The new S-factor values agree within their uncertainties with the past measurements. Details of the analysis and detector performance are presented.

  3. 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.

  4. 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.

  5. 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.

  6. High-purity 60GHz band millimeter-wave generation based on optically injected semiconductor laser under subharmonic microwave modulation.

    PubMed

    Fan, Li; Xia, Guangqiong; Chen, Jianjun; Tang, Xi; Liang, Qing; Wu, Zhengmao

    2016-08-01

    Based on an optically injected semiconductor laser (OISL) operating at period-one (P1) nonlinear dynamical state, high-purity millimeter-wave generation at 60 GHz band is experimentally demonstrated via 1/4 and 1/9 subharmonic microwave modulation (the order of subharmonic is with respect to the frequency fc of the acquired 60 GHz band millimeter-wave but not the fundamental frequency f0 of P1 oscillation). Optical injection is firstly used to drive a semiconductor laser into P1 state. For the OISL operates at P1 state with a fundamental frequency f0 = 49.43 GHz, by introducing 1/4 subharmonic modulation with a modulation frequency of fm = 15.32 GHz, a 60 GHz band millimeter-wave with central frequency fc = 61.28 GHz ( = 4fm) is experimentally generated, whose linewidth is below 1.6 kHz and SSB phase noise at offset frequency 10 kHz is about -96 dBc/Hz. For fm is varied between 13.58 GHz and 16.49 GHz, fc can be tuned from 54.32 GHz to 65.96 GHz under matched modulation power Pm. Moreover, for the OISL operates at P1 state with f0 = 45.02 GHz, a higher order subharmonic modulation (1/9) is introduced into the OISL for obtaining high-purity 60 GHz band microwave signal. With (fm, Pm) = (7.23 GHz, 13.00 dBm), a microwave signal at 65.07 GHz ( = 9fm) with a linewidth below 1.6 kHz and a SSB phase noise less than -98 dBc/Hz is experimentally generated. Also, the central frequency fc can be tuned in a certain range through adjusting fm and selecting matched Pm.

  7. High-purity 60GHz band millimeter-wave generation based on optically injected semiconductor laser under subharmonic microwave modulation.

    PubMed

    Fan, Li; Xia, Guangqiong; Chen, Jianjun; Tang, Xi; Liang, Qing; Wu, Zhengmao

    2016-08-01

    Based on an optically injected semiconductor laser (OISL) operating at period-one (P1) nonlinear dynamical state, high-purity millimeter-wave generation at 60 GHz band is experimentally demonstrated via 1/4 and 1/9 subharmonic microwave modulation (the order of subharmonic is with respect to the frequency fc of the acquired 60 GHz band millimeter-wave but not the fundamental frequency f0 of P1 oscillation). Optical injection is firstly used to drive a semiconductor laser into P1 state. For the OISL operates at P1 state with a fundamental frequency f0 = 49.43 GHz, by introducing 1/4 subharmonic modulation with a modulation frequency of fm = 15.32 GHz, a 60 GHz band millimeter-wave with central frequency fc = 61.28 GHz ( = 4fm) is experimentally generated, whose linewidth is below 1.6 kHz and SSB phase noise at offset frequency 10 kHz is about -96 dBc/Hz. For fm is varied between 13.58 GHz and 16.49 GHz, fc can be tuned from 54.32 GHz to 65.96 GHz under matched modulation power Pm. Moreover, for the OISL operates at P1 state with f0 = 45.02 GHz, a higher order subharmonic modulation (1/9) is introduced into the OISL for obtaining high-purity 60 GHz band microwave signal. With (fm, Pm) = (7.23 GHz, 13.00 dBm), a microwave signal at 65.07 GHz ( = 9fm) with a linewidth below 1.6 kHz and a SSB phase noise less than -98 dBc/Hz is experimentally generated. Also, the central frequency fc can be tuned in a certain range through adjusting fm and selecting matched Pm. PMID:27505789

  8. Determination of trace impurities in high purity gold by inductively coupled plasma mass spectrometry with prior matrix removal by electrodeposition

    NASA Astrophysics Data System (ADS)

    Sun, Y. C.; Hsieh, C. H.; Lin, T. S.; Wen, J. C.

    2000-09-01

    A novel method for the determination of 11 trace impurities (Be, Mg, Cr, Mn, Ni, Cu, Zn, Ag, Pd, Sn and Pb) in high purity gold with a combination of electrochemical deposition separation and inductively coupled plasma mass spectrometric measurement was investigated. In the present study, an efficient separation procedure was developed to remove the gold matrix by the electrodepositon method on the basis of the difference in reduction potential of gold and the other trace impurities. The effects of deposition potential, deposition time and composition of the electrolyte on the separation efficiency were studied. According to our experimental results, most impurities, except for silver, can remain in the electrolyte and the interference from gold can be completely removed through the application of electrodeposition at suitable potential. To achieve simultaneous separation of silver from the gold matrix, a unique complexation reaction between silver ions and ammonia ions was successfully employed to alter the reduction potential of silver ion. By way of a suitable adjustment of the deposition potential and the composition of electrolytes, the spike recoveries of 11 interesting impurities were found to be in the range of 85-105%. The limit of detection (based on the 3-σ criterion) of these elements was 10 -1-10 -2 μg g -1. The applicability of the proposed method has also been validated by the analysis of high purity gold reference materials (FAU9 and FAU11, Royal Canadian Mint). Comparing with the certified values, the recoveries of interesting elements were found to be in the range of 82-118% through the use of proposed method.

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. Flexure tests on dental ceramics.

    PubMed

    Zeng, K; Odén, A; Rowcliffe, D

    1996-01-01

    The failure stresses in flexural tests of a densely sintered high-purity alumina (Procera AllCeram) were evaluated using three-point bend, ring-on-ring, and piston-on-three-ball tests. Glass-infiltrated presintered alumina (In-Ceram) and leucite-reinforced porcelain (IPS Empress) disks with the same dimensions were also tested using ring-on-ring and piston-on-three-ball tests. The failure stresses for all materials were substantially different (up to 50%) with different testing methods, and cannot be directly compared. However, by considering the effective specimen area under the maximum tensile stress, these failure stress data could be compared. The results emphasize the importance of knowing the test method and the method of calculation when comparing data. These three testing methods were also subjected to Weibull analysis. The Procera AllCeram had a consistently higher failure stress than the other two materials. PMID:9108743

  14. Method for preparing thin-walled ceramic articles of configuration

    DOEpatents

    Holcombe, C.E.; Powell, G.L.

    1975-11-01

    A method for preparing a hollow thin-walled ceramic product is described. Ceramic powder is plasma-sprayed onto a concave surface of a substrate having a coefficient of thermal expansion less than that of the ceramic. The coated substrate is heated to sinter the ceramic and then cooled to effect a separation of the ceramic product from the substrate. (auth)

  15. Custom fabrication of reinforced lithium disilicate ceramic ingot

    PubMed Central

    Chander, Gopi Naveen; Sasikala, C.; Mutukumar, B.; Dhanasekar, N.

    2016-01-01

    A method of formulating a reinforcement lithium disilicate ceramic ingot was proposed. The ceramic ingot was broken manually with a mallet to finer particles. The sectioned ingot is ball milled along with 10% of nano zirconia by weight to obtain the desired powder. The reinforced powder is condensed in a 5 ml disposable syringe by powder slurry technique. The compacted ceramic were sintered at 900°C to obtain ceramic ingots. The reinforced ceramic ingots were used in pressable ceramic machines to obtain the desired advantages of zirconia reinforcement and pressable ceramic system. PMID:27134457

  16. 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)

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

    PubMed

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

    2016-10-14

    Highly pure metallic structures can be deposited by electron beam induced deposition and they have many important applications in different fields. The organo-metallic precursor is decomposed and deposited under the electron beam, and typically it is purified with post-irradiation in presence of O2. However, this approach limits the purification to the surface of the deposit. Therefore, 'in situ' purification during deposition using simultaneous flows of both O2 and precursor in parallel with two gas injector needles has been tested and verified. To simplify the practical arrangements, a special concentric nozzle has been designed allowing deposition and purification performed together in a single step. With this new device metallic structures with high purity can be obtained more easily, while there is no limit on the height of the structures within a practical time frame. In this work, we summarize the first results obtained for 'in situ' Au purification using this concentric nozzle, which is described in more detail, including flow simulations. The operational parameter space is explored in order to optimize the shape as well as the purity of the deposits, which are evaluated through scanning electron microscope and energy dispersive x-ray spectroscopy measurements, respectively. The observed variations are interpreted in relation to other variables, such as the deposition yield. The resistivity of purified lines is also measured, and the influence of additional post treatments as a last purification step is studied. PMID:27587078

  18. Gas-induced formation of Cu nanoparticle as catalyst for high-purity straight and helical carbon nanofibers.

    PubMed

    Jian, Xian; Jiang, Man; Zhou, Zuowan; Zeng, Qun; Lu, Jun; Wang, Dingchuan; Zhu, Junting; Gou, Jihua; Wang, Yong; Hui, David; Yang, Mingli

    2012-10-23

    The facile preparation of high-purity carbon nanofibers (CNFs) remains challenging due to the high complexity and low controllability in reaction. A novel approach using gas-induced formation of Cu crystals to control the growth of CNFs is developed in this study. By adjusting the atmospheric composition, controllable preparation of Cu nanoparticles (NPs) with specific size and shape is achieved, and they are further used as a catalyst for the growth of straight or helical CNFs with good selectivity and high yield. The preparation of Cu NPs and the formation of CNFs are completed by a one-step process. The inducing effect of N(2), Ar, H(2), and C(2)H(2) on the formation of Cu NPs is systematically investigated through a combined experimental and computational approach. The morphology of CNFs obtained under different conditions is rationalized in terms of Cu NP and CNF growth models. The results suggest that the shapes of CNFs, namely, straight or helical, depend closely on the size, shape, and facet activity of Cu NPs, while such a gas-inducing method offers a simple way to control the formation of Cu NPs.

  19. 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.

  20. Wafer and bulk high-purity silicon trace element analysis at the Texas A and M University Nuclear Science Center

    SciTech Connect

    Van Dalsem, Daniel James

    1998-11-24

    A trace element analysis program for wafer and bulk high-purity silicon (Si) samples has been operating at the Texas A and M University Nuclear Science Center (TAMU NSC) since 1996. Samples are irradiated in the NSC's 1-MW TRIGA research reactor at a thermal neutron fluence rate of 10{sup 13} n/cm{sup 2}/s for 14 hours. After an appropriate decay length, bulk samples are chemically etched to remove surface contamination while wafer surfaces are first rinsed with acid to determine surface contamination and then etched to obtain epitaxial layer contamination information. All samples, along with the appropriate etching solutions are analyzed using gamma-ray spectroscopy to quantitatively determine the various radioisotopes created during irradiation. Elements typically determined are antimony (Sb), arsenic (As), bromine (Br), cadmium (Cd), chromium (Cr), cobalt (Co), copper (Cu), gallium (Ga), gold (Au), iron (Fe), molybdenum (Mo), potassium (K), silver (Ag), sodium (Na) tungsten (W) and zinc (Zn). The potential exists to also determine cesium (Cs), iridium (Ir), lanthanum (La), mercury (Hg), rubidium (Rb), scandium (Sc), and zirconium (Zr). Detection limits range from 10{sup 14} down to 10{sup 7} atoms/cm{sup 2} in surface analysis and 10{sup 13} down to 10{sup 8} atoms/cm{sup 3} in bulk Si.

  1. 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.

  2. 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.

  3. Effects of hydrogen on the mixed mode I/III toughness of a high-purity rotor steel

    SciTech Connect

    Kumar, A.M.; Hirth, J.P. ); Moody, N.R.; Gordon, J.A. )

    1993-06-01

    Recently, the authors reported the effects of hydrogen on the mixed mode 1/111 toughness of a high-purity Ni-Cr-Mo-V rotor steel. The steel was tested both in the uncharged and hydrogen-charged conditions. It was shown that the presence of hydrogen degraded the overall J toughness incrementally by approximately 30 pct, with the degree of degradation increasing with the mode III component. Also, in the uncharged condition, the J toughness decreased to a minimum as the mode I/III ratio decreased and increased again for pure mode III loading. However, the authors could not determine if a similar variation of toughness was displayed by the hydrogen-charged steel, because the pure mode III tests could not be completed at that time. The pure mode III tests are now complete, and these new results are presented in this communication. The chemical composition of the steel used in these studies was 0.25C-3.7Ni-1.7Cr-0.4Mo-0.12V-0.05Mn- 0.02Si-0.003(P,Sn,As)-O.002Sb-0.0015 S (wt pct).

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

    PubMed

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

    2016-10-14

    Highly pure metallic structures can be deposited by electron beam induced deposition and they have many important applications in different fields. The organo-metallic precursor is decomposed and deposited under the electron beam, and typically it is purified with post-irradiation in presence of O2. However, this approach limits the purification to the surface of the deposit. Therefore, 'in situ' purification during deposition using simultaneous flows of both O2 and precursor in parallel with two gas injector needles has been tested and verified. To simplify the practical arrangements, a special concentric nozzle has been designed allowing deposition and purification performed together in a single step. With this new device metallic structures with high purity can be obtained more easily, while there is no limit on the height of the structures within a practical time frame. In this work, we summarize the first results obtained for 'in situ' Au purification using this concentric nozzle, which is described in more detail, including flow simulations. The operational parameter space is explored in order to optimize the shape as well as the purity of the deposits, which are evaluated through scanning electron microscope and energy dispersive x-ray spectroscopy measurements, respectively. The observed variations are interpreted in relation to other variables, such as the deposition yield. The resistivity of purified lines is also measured, and the influence of additional post treatments as a last purification step is studied.

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

    PubMed

    Gibb, Jack N; Goodman, Jonathan M

    2013-01-01

    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.

  6. 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.

  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. High-Purity Isolation and Recovery of Circulating Tumor Cells using Conducting Polymer-deposited Microfluidic Device

    PubMed Central

    Jeon, SeungHyun; Hong, WooYoung; Lee, Eun Sook; Cho, Youngnam

    2014-01-01

    We have developed a conductive nano-roughened microfluidic device and demonstrated its use as an electrically modulated capture and release system for studying rare circulating tumor cells (CTCs). The microchannel surfaces were covalently decorated with epithelial cancer-specific anti-EpCAM antibody by electrochemical deposition of biotin-doped polypyrrole (Ppy), followed by the assembly of streptavidin and biotinylated antibody. Our method utilizes the unique topographical features and excellent electrical activity of Ppy for i) surface-induced preferential recognition and release of CTCs, and ii) selective elimination of non-specifically immobilized white blood cells (WBCs), which are capable of high-purity isolation of CTCs. In addition, the direct incorporation of biotin molecules offers good flexibility, because it allows the modification of channel surfaces with diverse antibodies, in addition to anti-EpCAM, for enhanced detection of multiple types of CTCs. By engineering a series of electrical, chemical, and topographical cues, this simple yet efficient device provides a significant advantage to CTC detection technology as compared with other conventional methods. PMID:25250093

  9. 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.

  10. Cyanex 923 as the extractant in a rare earth element impurity analysis of high-purity cerium oxide.

    PubMed

    Duan, Taicheng; Li, Hongfei; Kang, JianZhen; Chen, Hangting

    2004-06-01

    In this work, the feasibility of employing Cyanex 923 as an extractant into the non-cerium REE (rare earth elements) impurity analysis of high-purity cerium oxide was investigated. Through investigations on the choice of the extraction medium, the optimium extraction acidity, matrix Ce4+ effect on the non-cerium REE ion extraction, the optimium extractant concentration and suitable extracting time, and oscillation strengh, it was found that when the phase ratio was at 1:1 and the acicidity was about 2% H2SO4, by gently shaking by hand for about 2 min, 10 mL of 30% Cyanex 923 could not extract even for a 20 ng amount of non-cerium REE3+ ions. However, the extraction efficiency for Ce4+ of 100 mg total amount under the same conditions was about 96%, indicating that a 25-fold preconcentration factor could be achieved. Thus, it was concluded that Cyanex 923 could be used in a REE impurity analysis of 99.9999% or so pure cerium oxide for primary sepapation to elimilate matrix-induced interferences encountered in an ICP-MS (inductively coupled plasma mass spectroscopy) determination.

  11. Gas-induced formation of Cu nanoparticle as catalyst for high-purity straight and helical carbon nanofibers.

    PubMed

    Jian, Xian; Jiang, Man; Zhou, Zuowan; Zeng, Qun; Lu, Jun; Wang, Dingchuan; Zhu, Junting; Gou, Jihua; Wang, Yong; Hui, David; Yang, Mingli

    2012-10-23

    The facile preparation of high-purity carbon nanofibers (CNFs) remains challenging due to the high complexity and low controllability in reaction. A novel approach using gas-induced formation of Cu crystals to control the growth of CNFs is developed in this study. By adjusting the atmospheric composition, controllable preparation of Cu nanoparticles (NPs) with specific size and shape is achieved, and they are further used as a catalyst for the growth of straight or helical CNFs with good selectivity and high yield. The preparation of Cu NPs and the formation of CNFs are completed by a one-step process. The inducing effect of N(2), Ar, H(2), and C(2)H(2) on the formation of Cu NPs is systematically investigated through a combined experimental and computational approach. The morphology of CNFs obtained under different conditions is rationalized in terms of Cu NP and CNF growth models. The results suggest that the shapes of CNFs, namely, straight or helical, depend closely on the size, shape, and facet activity of Cu NPs, while such a gas-inducing method offers a simple way to control the formation of Cu NPs. PMID:22963353

  12. Intergranular Corrosion for Extra High Purity Austenitic Stainless Steel in Boiling Nitric Acid with Cr(VI)

    NASA Astrophysics Data System (ADS)

    Ioka, Ikuo; Kato, Chiaki; Kiuchi, Kiyoshi; Nakayama, Junpei

    Austenitic stainless steels suffer intergranular attack in boiling nitric acid with oxidants. The intergranular corrosion is mainly caused by the segregation of impurities at the grain. An extra high purity austenitic stainless steel (EHP alloys) was developed with conducting the new multiple refined melting technique in order to suppress the total harmful impurities less than 100ppm. The corrosion behavior of type 310 EHP alloy with respect to nitric acid solution with highly oxidizing ions (boiling 8kmol/m3 HNO3 solutions containing 1kg/m3 Cr(VI) ions) was investigated. The straining, aging and recrystallizing (SAR) treated type 310 EHP alloy showed superior corrosion resistance for intergranular attack than solution annealed (ST) type 310 EHP alloy with same impurity level. Boron segregation at the grain boundary was detected in only ST specimen using a Fission Track Etching method. It is believed that the segregated boron along the grain boundaries in type 310 EHP alloy was one of main factor of intergranular corrosion. The SAR treatment was effective to restrain the intergranular corrosion for type 310 EHP alloy with B less than 7ppm.

  13. Process for fabrication of large titanium diboride ceramic bodies

    DOEpatents

    Moorhead, Arthur J.; Bomar, E. S.; Becher, Paul F.

    1989-01-01

    A process for manufacturing large, fully dense, high purity TiB.sub.2 articles by pressing powders with a sintering aid at relatively low temperatures to reduce grain growth. The process requires stringent temperature and pressure applications in the hot-pressing step to ensure maximum removal of sintering aid and to avoid damage to the fabricated article or the die.

  14. 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.

  15. 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.

  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. 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.

  18. 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.

  19. 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.

  20. 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.

  1. 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.

  2. 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.

  3. Effect of Rare Earth Oxide Content on Nanograined Base Metal Electrode Multilayer Ceramic Capacitor Powder Prepared by Aqueous Chemical Coating Method

    NASA Astrophysics Data System (ADS)

    Zhang, Yichi; Wang, Xiaohui; Kim, Jinyong; Li, Longtu

    2013-02-01

    The aqueous chemical coating route is highly effective in preparing BaTiO3 nanoparticles uniformly coated with additives. Such nanoparticles can be used to produce nano-grained temperature stable BaTiO3 ceramics with core-shell structure, fulfilling the need of next-generation ultrathin layer base metal electrode (BME) multilayer ceramic capacitors (MLCCs). Rare earth oxides are an important class of additives owing to their ability to fulfill both donor and acceptor roles. In this paper, the effects of Y2O3 and Ho2O3 co-dopant content on dielectric and microstructural properties were investigated. By applying chemical coating, BaTiO3-based high performance temperature stabilized ceramics with the average grain size of about 130 nm, which met the requirement of next generation BME MLCCs, were obtained.

  4. Fabrication of large ceramic electrolyte disks

    NASA Technical Reports Server (NTRS)

    Ring, S. A.

    1972-01-01

    Process for sintering compressed ceramic powders produces large ceramic disks for use as electrolytes in high-temperature electrolytic cells. Thin, strain-free uniformly dense disks as large as 30 cm squared have been fabricated by slicing ceramic slugs produced by this technique.

  5. 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.

  6. 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.

  7. Determination of trace selenium in high purity tellurium by hydride generation atomic fluorescence spectrometry after solid phase extraction of a diaminobenzidine-selenium chelate

    NASA Astrophysics Data System (ADS)

    Tong, Wang; Ying, Zeng; Jinyong, Xu

    2016-09-01

    Macroporous adsorption resin was used as the sorbent for solid phase extraction and determination of the trace Se content in high purity tellurium prior to hydride generation atomic fluorescence spectrometry analysis. Selenium was converted into an organic Se chelate using 3,3‧-diaminobenzidine and was separated from the tellurium matrix by solid phase extraction. The resin was packed as a column for solid phase extraction. Under optimum conditions, trace Se can be quantitatively extracted and the tellurium matrix can be removed. The Se in the eluate was determined by hydride generation atomic fluorescence spectrometry. The limit of detection (3σ) of this method was 0.22 ng g- 1 and the relative standard deviation (RSD, n = 5) ranged from 2.0 to 2.5% for the three investigated tellurium samples. The proposed method was successfully applied for the determination of the trace Se content in high purity tellurium samples.

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

    NASA Astrophysics Data System (ADS)

    Dargatz, Benjamin; Gonzalez-Julian, Jesus; Guillon, Olivier

    2015-04-01

    The retention of nanocrystallinity in dense ceramic materials is still a challenge, even with the application of external pressure during sintering. The compaction behavior of high purity and acetate enriched zinc oxide (ZnO) nano-powders was investigated. It was found that acetate in combination with water plays a key role during the compaction into green bodies at moderate temperatures. Application of constant pressure resulted in a homogeneous green body with superior packing density (86% of theoretical value) at moderate temperature (85 °C) in the presence of water. In contrast, no improvement in density could be achieved if pure ZnO powder was used. This compaction behavior offers superior packing of the particles, resulting in a high relative density of the consolidated compact with negligible coarsening. Dissolution accompanying creep diffusion based matter transport is suggested to strongly support reorientation of ZnO particles towards densities beyond the theoretical limit for packing of ideal monosized spheres. Finally, the sintering trajectory reveals that grain growth is retarded compared to conventional processing up to 90% of theoretical density. Moreover, nearly no radial shrinkage was observed after sinter-forging for bodies performed with this advanced processing method.

  9. 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.

  10. 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.

  11. 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.

  12. Synthesis of Nano-Polycrystalline Synroc-B Powders as a High Level Radioactive Wastes Ceramic Forms by a Solution Combustion Synthesis.

    PubMed

    Han, Young-Min; Lee, Sang-Jin; Kim, Yeon-Ku; Jung, Choong-Hwan

    2016-02-01

    Synroc (Synthetic Rock) consists of four main titanate phases: peroveskite (CaTiO3), zirconolite (CaZrTi2O7), hollandite (BaAl2Ti6O16) and rutile (TiO2). Nano-polycrystalline synroc powders were made by a synthesis combustion process. The combustion process, an externally initiated reaction is self-sustained owing to the exothermic reaction. A significant volume of gas is evolved during the combustion reaction and leads to loosely agglomerated powders. This exothermic reaction provides necessary heat to further carry the reaction in forward direction to produce nanocrystalline powders as the final product. Glycine is used as a fuel, being oxidized by nitrate ions. It is inexpensive, has high energy efficiency, fast heating rates, short reaction times and high compositional homogeneity. In this study, combustion synthesis of nano-sized synroc-B powder is introduced. The fabrication of synroc-B powder result of observation XRD were prepared for polycrystalline (perovskite, zirconolite, hollandite, rutile) structures. The characterization of the synthesized powders is conducted by using XRD, SEM/EDS and TEM. PMID:27433644

  13. 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

  14. 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.

  15. 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.

  16. 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.

  17. 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.

  18. Synthesis of few-layered, high-purity graphene oxide sheets from different graphite sources for biology

    NASA Astrophysics Data System (ADS)

    Jasim, Dhifaf A.; Lozano, Neus; Kostarelos, Kostas

    2016-03-01

    This work aimed to interrogate the role that the starting graphitic material played on the physicochemical properties of graphene oxide (GO) sheets and their impact on mammalian cell viability following exposure to those flakes. Three different GO thin sheets were synthesised from three starting graphite material: flakes (GO-f), ground (GO-g) and powder (GO-p) using a modified Hummers’ method. The synthetic yield of this methodology was found to differ according to type of starting material, with GO-p resulting in most efficient yields. Structural and morphological comparison of the three GO sheet types were carried out using transmission electron microscopy and atomic force microscopy. Optical properties were measured using UV/visible and fluorescence spectroscopy. Surface characteristics and chemistry were determined using a battery of techniques. Exposure to human cells was studied using the human A549 lung epithelial cultures. Our results revealed that all three GO samples were composed of few-layer sheets with similar physicochemical and surface characteristics. However, significant differences were observed in terms of their lateral dimensions with GO-p, prepared from graphite powder, being the largest among the GOs. No cytotoxicity was detected for any of the GO samples following exposure onto A549 cells up to 48 h. In conclusion, the form and type of the starting graphite material is shown to be an important factor that can determine the synthetic yield and the structural characteristics of the resulting GO sheets.

  19. 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

  20. Method for synthesizing ultrafine powder materials

    DOEpatents

    Buss, Richard J.; Ho, Pauline

    1988-01-01

    A method for synthesizing ultrafine powder materials, for example, ceramic and metal powders, comprises admitting gaseous reactants from which the powder material is to be formed into a vacuum reaction chamber maintained at a pressure less than atmospheric and at a temperature less than about 400.degree. K. (127.degree.C.). The gaseous reactants are directed through a glow discharge provided in the vacuum reaction chamber to form the ultrafine powder material.

  1. MESOSCALE SIMULATIONS OF POWDER COMPACTION

    SciTech Connect

    Lomov, Ilya; Fujino, Don; Antoun, Tarabay; Liu, Benjamin

    2009-12-28

    Mesoscale 3D simulations of shock compaction of metal and ceramic powders have been performed with an Eulerian hydrocode GEODYN. The approach was validated by simulating a well-characterized shock compaction experiment of a porous ductile metal. Simulation results using the Steinberg material model and handbook values for solid 2024 aluminum showed good agreement with experimental compaction curves and wave profiles. Brittle ceramic materials are not as well studied as metals, so a simple material model for solid ceramic (tungsten carbide) has been calibrated to match experimental compaction curves. Direct simulations of gas gun experiments with ceramic powders have been performed and showed good agreement with experimental data. The numerical shock wave profile has same character and thickness as that measured experimentally using VISAR. The numerical results show reshock states above the single-shock Hugoniot line as observed in experiments. We found that for good quantitative agreement with experiments 3D simulations are essential.

  2. Mesoscale Simulations of Powder Compaction

    NASA Astrophysics Data System (ADS)

    Lomov, Ilya.; Fujino, Don; Antoun, Tarabay; Liu, Benjamin

    2009-12-01

    Mesoscale 3D simulations of shock compaction of metal and ceramic powders have been performed with an Eulerian hydrocode GEODYN. The approach was validated by simulating a well-characterized shock compaction experiment of a porous ductile metal. Simulation results using the Steinberg material model and handbook values for solid 2024 aluminum showed good agreement with experimental compaction curves and wave profiles. Brittle ceramic materials are not as well studied as metals, so a simple material model for solid ceramic (tungsten carbide) has been calibrated to match experimental compaction curves. Direct simulations of gas gun experiments with ceramic powders have been performed and showed good agreement with experimental data. The numerical shock wave profile has same character and thickness as that measured experimentally using VISAR. The numerical results show reshock states above the single-shock Hugoniot line as observed in experiments. We found that for good quantitative agreement with experiments 3D simulations are essential.

  3. 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.

  4. 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.

  5. Characteristics of Signals Originating near the Lithium-Diffused N+ Contact of High Purity Germanium P-Type Point Contact Detectors

    SciTech Connect

    Aguayo, E.; Amman, M.; Avignone, F. T.; Barton, P. J.; Beene, James R; Bertrand Jr, Fred E; Boswell, M.; Brudanin, V.; Busch, M.; Chan, Y-D; Christofferson, C. D.; Collar, Juan I.; Combs, D. C.; Detwiler, J.A.; Doe, P. J.; Efremenko, Yuri; Egorov, V.; Ejiri, H.; Elliott, S. R.; Esterline, J.; Fast, J.E.; Fields, N.; Finnerty, P.; Gehman, V. M.; Giovanetti, G. K.; Green, M. P.; Gusey, K.; Hallin, A. L.; Hazama, R.; Henning, R.; Hoppe, E.W.; Horton, M.; Howard, S.; Howe, M. A.; Keeter, K.J.; Kidd, M. F.; Knecht, A.; Kochetov, O.; Konovalov, S.I.; Kouzes, R. T.; LaFerriere, B. D.; Leon, J.; Leviner, L. E.; Looker, Q.; Luke, P.N.; MacMullin, S.; Martin, R.D.; Merriman, J. H.; Miller, M. L.; Mizouni, L.; Orrell, John L.; Overman, N. R.; Perumpilly, G.; Phillips II, D. G.; et al.

    2013-01-01

    A study of signals originating near the lithium-diffused n+ contact of p-type point contact (PPC) high purity germanium detectors (HPGe) is presented. The transition region between the active germanium and the fully dead layer of the n+ contact is examined. Energy depositions in this transition region are shown to result in partial charge collection. This provides a mechanism for events with a well defined energy to contribute to the continuum of the energy spectrum at lower energies. A novel technique to quantify the contribution from this source of background is introduced. Experiments that operate germanium detectors with a very low energy threshold may benefit from the methods presented herein.

  6. 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…

  7. 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.

  8. 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

  9. Optimal recovery of high-purity rutin crystals from the whole plant of Fagopyrum esculentum Moench (buckwheat) by extraction, fractionation, and recrystallization.

    PubMed

    Kim, Kyoung Heon; Lee, Ki Won; Kim, Dong Young; Park, Hyung Hwan; Kwon, Ik Boo; Lee, Hyong Joo

    2005-10-01

    Rutin, one of the flavonoids derived from plants, is increasingly in demand in the food, pharmaceutical, and cosmetic industries due to its various biological and physiological activities including antioxidation, anti-inflammation, and anti-hypertension. The whole plant of buckwheat (Fagopyrum esculentum Moench) is a major source of natural rutin. This study developed a low-cost process encompassing the efficient extraction, fractionation, and recrystallization to obtain high-purity rutin from buckwheat, and it could improve the economic utilization of this abundant low-value agricultural product. The sequential separation and purification procedures established in this study involved extraction with 50% (v/v) aqueous ethanol at 80 degrees C for 1 h followed by elution with water and aqueous ethanols at 20% and 30% (v/v) on a styrene-based resin column, and recrystallization at 4 degrees C for 12 h. These conditions resulted in the recovery of 92% of total rutin with over 95% purity. In the present study, high-purity rutin was obtained from whole buckwheat through low-cost processes, the separation and purification strategy established in this study could provide valuable information to the relevant industries.

  10. Mixed-conducting dense ceramics for gas separation applications.

    SciTech Connect

    Balachandran, U.; Dorris, S. E.; Dusek, J. T.; Guan, J.; Liu, M.; Ma, B.; Maiya, P. S.; Picciolo, J. J.

    1999-06-22

    Mixed-conducting (electronic and ionic conducting) dense ceramics are used in many applications, including fuel cells, gas separation membranes, batteries, sensors, and electrocatalysis. This paper describes mixed-conducting ceramic membranes that are being developed to selectively remove oxygen and hydrogen from gas streams in a nongalvanic mode of operation (i.e., with no electrodes or external power supply). Ceramic membranes made of Sr-Fe-Co oxide (SFC), which exhibits high combined electronic and oxygen ionic conductivities, can be used for high-purity oxygen separation and/or partial oxidation of methane to synthesis gas (syngas, a mixture of CO and H{sub 2}). The electronic and ionic conductivities of SFC were found to be comparable in magnitude. Steady-state oxygen permeability of SFC has been measured as a function of oxygen-partial-pressure gradient and temperature. For an {approx}3-mm-thick membrane, the oxygen permeability was {approx}2.5 scc{center_dot}cm{sup {minus}2}{center_dot}min{sup {minus}1} at 900 C. Oxygen permeation increases as membrane thickness decreases. Tubular SFC membranes have been fabricated and operated at 900 C for {approx}1000 h in converting methane into syngas. The oxygen permeated through the membrane reacted with methane in the presence of a catalyst and produced syngas. We also studied the transport properties of yttria-doped BaCeO{sub 3{minus}{delta}} (BCY) by impedance spectroscopy and open-cell voltage (OCV) measurement. Total conductivity of the BCY sample increased from {approx}5 x 10{sup {minus}3} {Omega}{sup {minus}1}{center_dot}cm{sup {minus}1} to {approx}2 x 10{sup {minus}2} {Omega}{sup {minus}1}{center_dot}cm{sup {minus}1}, whereas the protonic transference number decreased from 0.87 to 0.63 and the oxygen transference number increased from 0.03 to 0.15 as temperature increased from 600 to 800 C. Unlike SFC, in which the ionic and electronic conductivities are nearly equivalent BCY exhibits protonic conductivity that

  11. Electrothermal vaporization coupled with inductively coupled plasma array-detector mass spectrometry for the multielement analysis of Al2O3 ceramic powders

    SciTech Connect

    Peschel, Birgit U.; Andrade, Francisco J.; Wetzel, William C.; Schilling, G D.; Hieftje, Gary M.; Broekaert, Jose AC; Sperline, Roger; Denton, M BONNER.; Barinaga, Charles J.; Koppenaal, David W.

    2006-01-01

    An electrothermal vaporization (ETV) system useful for the analysis of solutions and slurries has been coupled with a sector-field inductively coupled plasma mass spectrometer (ICP-MS) equipped with an array detector. The ability of this instrument to record the transient signals produced in ETV-ICP-MS is demonstrated. Detection limits for Mn, Fe, Co, Ni, Cu, Zn and Ga are in the range of 4-60 pg ?L-1 for aqueous solutions and in the low ?g g-1 range for the analysis of 10 mg mL-1 slurries of Al2O3 powders. The dynamic ranges measured for Fe, Cu and Ga spanned 3-5 orders of magnitude when the detector was operated in the low-gain mode and appear to be limited by the ETV system. Trace amounts of Fe, Cu and Ga could be directly determined in Al2O3 powders at the 2-270 ?g g-1 level without the use of thermochemical reagents. The results well agree with literature values for Fe, whereas deviations of 30-50% at the 2-90 ?g g-1 level for Cu and Ga were found.

  12. 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.

  13. 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.

  14. Transparent Nd doped YAG ceramics

    NASA Astrophysics Data System (ADS)

    Stanciu, Catalina-Andreea; Dascalu, Traian; Stanciu, George; Pavel, Nicolaie

    2016-08-01

    The reasearch main objective is to obtain ceramic laser materials based on pure YAG (Y3Al5O12) and Nd doped YAG (Y3-xNdxAl5O12, with × = 0.5 and 1.0 at. %), by conventional solid state reaction method. Stoichiometric compositions of Y3Al5O12 (YAG), Y2.985Nd0.015Al5O12 (0.5 at.% Nd:YAG) and Y2.97Nd0.03Al5O12 (1.0 at.% Nd:YAG) were prepared using high purity Y2O3 (99.999%), Al2O3 (99.999%) and Nd2O3 (99.999%) nanopowders. Green bodies were sintered at 1750 °C for 16 h under vacuum (1.0 × 10-3 Pa) and then annealed at 1450 °C for 10 h in the air.

  15. 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.

  16. Recovery behavior of high purity cubic SiC polycrystals by post-irradiation annealing up to 1673 K after low temperature neutron irradiation

    NASA Astrophysics Data System (ADS)

    Idris, Mohd Idzat; Yamazaki, Saishun; Yoshida, Katsumi; Yano, Toyohiko

    2015-10-01

    Two kinds of high purity cubic (β) SiC polycrystals, PureBeta-SiC and CVD-SiC, were irradiated in the BR2 reactor (Belgium) up to a fluence of 2.0-2.5 × 1024 (E > 0.1 MeV) at 333-363 K. Changes in macroscopic lengths were examined by post-irradiation thermal annealing using a precision dilatometer up to 1673 K with a step-heating method. The specimen was held at each temperature step for 6 h and the change in length of the specimen was recorded during each isothermal annealing step from 373 K to 1673 K with 50 K increments. The recovery curves were analyzed with the first order model, and rate constants at each annealing step were obtained. Recovery of defects, induced by neutron irradiation in high purity β-SiC, has four stages of different activation energies. At 373-573 K, the activation energy of PureBeta-SiC and CVD-SiC was in the range of 0.17-0.24 eV and 0.12-0.14 eV; 0.002-0.04 eV and 0.006-0.04 eV at 723-923 K; 0.20-0.27 eV and 0.26-0.31 eV at 923-1223 K; and 1.37-1.38 eV and 1.26-1.29 eV at 1323-1523 K, respectively. Below ∼1223 K the recombination occurred possibly for closely positioned C and Si Frenkel pairs, and no long range migration is deemed essential. Nearly three-fourths of recovery, induced by neutron irradiation, occur by this mechanism. In addition, at 1323-1523 K, recombination of slightly separated C Frenkel pairs and more long-range migration of Si interstitials may have occurred for PureBeta-SiC and CVD-SiC specimens. Migration of both vacancies may be restricted up to ∼1523 K. Comparing to hexagonal α-SiC, high purity β-SiC recovered more quickly in the lower annealing temperature range of less than 873 K, in particular less than 573 K.

  17. Study of the mechanical stability and bioactivity of Bioglass(®) based glass-ceramic scaffolds produced via powder metallurgy-inspired technology.

    PubMed

    Boccardi, Elena; Melli, Virginia; Catignoli, Gabriele; Altomare, Lina; Jahromi, Maryam Tavafoghi; Cerruti, Marta; Lefebvre, Louis-Philippe; De Nardo, Luigi

    2016-02-01

    Large bone defects are challenging to heal, and often require an osteoconductive and stable support to help the repair of damaged tissue. Bioglass-based scaffolds are particularly promising for this purpose due to their ability to stimulate bone regeneration. However, processing technologies adopted so far do not allow for the synthesis of scaffolds with suitable mechanical properties. Also, conventional sintering processes result in glass de-vitrification, which generates concerns about bioactivity. In this work, we studied the bioactivity and the mechanical properties of Bioglass(®) based scaffolds, produced via a powder technology inspired process. The scaffolds showed compressive strengths in the range of 5-40 MPa, i.e. in the upper range of values reported so far for these materials, had tunable porosity, in the range between 55 and 77%, and pore sizes that are optimal for bone tissue regeneration (100-500 μm). We immersed the scaffolds in simulated body fluid (SBF) for 28 d and analyzed the evolution of the scaffold mechanical properties and microstructure. Even if, after sintering, partial de-vitrification occurred, immersion in SBF caused ion release and the formation of a Ca-P coating within 2 d, which reached a thickness of 10-15 μm after 28 d. This coating contained both hydroxyapatite and an amorphous background, indicating microstructural amorphization of the base material. Scaffolds retained a good compressive strength and structural integrity also after 28 d of immersion (6 MPa compressive strength). The decrease in mechanical properties was mainly related to the increase in porosity, caused by its dissolution, rather than to the amorphization process and the formation of a Ca-P coating. These results suggest that Bioglass(®) based scaffolds produced via powder metallurgy-inspired technique are excellent candidates for bone regeneration applications. PMID:26836444

  18. 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.

  19. 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.

  20. 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.

  1. Mechanical behavior of bioactive composite cements consisting of resin and glass-ceramic powder in a simulated body fluid: effect of silane coupling agent.

    PubMed

    Miyata, N; Matsuura, W; Kokubo, T; Nakamura, T

    2004-09-01

    Time-dependent strength behavior was investigated for bisphenol-a-glycidyl methacrylate/triethylene glycol dimethacrylate (Bis-GMA/TEGDMA) resin cements combined with glass-ceramic A-W filler treated with various kinds of silane coupling agents. The fracture strength of the composite resin cements was measured by three-point bending as a function of stressing rate in a simulated body fluid (SBF), and thereby the stress-corrosion susceptibility constant was evaluated. The fracture strength was found to depend on the kind of coupling agent used. For the present Bis-GMA/TEGDMA resin, the silane coupling agents without hydrophilic amine groups can be used to obtain good adhesion between resin and A-W filler owing to their nature of co-polymerizing with the resin. On the other hand, all the composite resin cements showed nearly the same degree of stress-corrosion susceptibility whether the A-W fillers were treated or untreated with silane coupling agents. This means that the stress-corrosion susceptibility of the present composite cements is predominantly affected by that of the matrix resin. Thus, the microcrack formation and growth at the resin matrix near particle - resin interface were thought to determine overall time-dependent strength behavior of the composite cements.

  2. First laser operation and spectroscopic characterization of mixed garnet Yb:LuYAG ceramics

    NASA Astrophysics Data System (ADS)

    Toci, Guido; Pirri, Angela; Li, Jiang; Xie, Tengfei; Pan, Yubai; Nikl, Martin; Babin, Vladimir; Beitlerová, Alena; Vannini, Matteo

    2016-03-01

    We present the optical and spectroscopic characterization and the first example of laser operation of Yb doped LuYAG ceramics, with two different compositions, namely (Lu0.25Y0.75)3Al5O12 and (Lu0.50Y0.50)3Al5O12, both with 15% Yb doping. Ceramic samples were prepared by reactive sintering from high purity α-Al2O3, Lu2O3, Y2O3, Yb2O3 powders using Tetraethoxysilane (TEOS) and MgO as sintering aids. After ball milling, the slurry was dried, uniaxially pressed into 20 mm diameter pellets at 20 MPa, and then cold isostatically pressed at 200 MPa. Sintering was conducted at 1850°C for 30 h under vacuum, followed by annealing in air (1500 °C, 10 h) to remove the oxygen vacancies. Laser tests were carried out in a laser cavity end pumped by a fiber coupled diode laser emitting at 936 nm. A slope efficiency as high as 65.2% with a maximum output power of 8.7 W (in quasi-CW pumping conditions) was obtained from the sample with composition (Lu0.25Y0.75)3Al5O12, whereas the sample with composition (Lu0.50Y0.50)3Al5O12 had a maximum slope efficiency of 49.5% (due to the higher scattering losses), and 6.7 W of maximum output power. Furthermore we characterized the tuning range of the two samples.

  3. 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.; Barabash, A. S.; Barton, P. J.; Beene, J. R.; Bertrand, F. E.; Boswell, M.; Brudanin, V.; Busch, M.; et al

    2012-11-09

    A study of signals originating near the lithium-diffused n+ contact of p-type point contact (PPC) high purity germanium detectors (HPGe) is presented. The transition region between the active germanium and the fully dead layer of the n+ contact is examined. Energy depositions in this transition region are shown to result in partial charge collection. This provides a mechanism for events with a well defined energy to contribute to the continuum of the energy spectrum at lower energies. A novel technique to quantify the contribution from this source of background is introduced. Furthermore, experiments that operate germanium detectors with a verymore » low energy threshold may benefit from the methods presented herein.« less

  4. 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.

  5. 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.

  6. 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.

  7. An improved back-flush-to-vent gas chromatographic method for determination of trace permanent gases and carbon dioxide in ultra-high purity ammonia.

    PubMed

    Trubyanov, Maxim M; Mochalov, Georgy M; Vorotyntsev, Ilya V; Vorotyntsev, Andrey V; Suvorov, Sergey S; Smirnov, Konstantin Y; Vorotyntsev, Vladimir M

    2016-05-20

    A novel method for rapid, quantitative determination of trace permanent gases and carbon dioxide in ultra-high purity ammonia by dual-channel two-dimensional GC-PDHID is presented. An improved matrix back-flush-to-vent approach combining back-flush column switching technique with auxiliary NaHSO4 ammonia trap is described. The NaHSO4 trap prevents traces of ammonia from entering the analytical column and is shown not to affect the impurity content of the sample. The approach allows shortening the analysis time and increasing the amount of measurements without extensive maintenance of the GC-system. The performance of the configuration has been evaluated utilizing ammonia- and helium-based calibration standards. The method has been applied for the analysis of 99.9999+% ammonia purified by high-pressure distillation at the production site. PMID:27083259

  8. In situ matrix evaporation by isothermal distillation of high-purity reagents for the determination of trace impurities by ion chromatography.

    PubMed

    Dhavile, S M; Thangavel, S; Chandrasekaran, K; Dash, K; Rao, S V; Chaurasia, S C

    2004-10-01

    In situ matrix evaporation of high-purity acids based on isothermal distillation was achieved in a high-density polyethylene (HDPE) container on a water bath, to avoid contamination from the laboratory environment. The solubility of water and acid vapours in glycerol due to co-association was utilized to achieve complete evaporation. All major sources which contribute to the process blank were taken care of in a simple and effective way. A 50-fold preconcentration with >99.9% matrix removal was achieved for the analysis of low-boiling acids, HCl, HF, HNO3 and H2O2. The non-volatile ions NH4+, Li+, Na+, K+, Mg2+, Ca2+, SO4(2-) and PO4(3-) were determined by ion chromatograph with conductivity detection. The detection limits were 6-130 ng/l with recoveries of 85-110% for all ions studied.

  9. Measured Attenuation of Coplanar Waveguide on 6H, p-type SiC and High Purity Semi-Insulating 4H SiC through 800 K

    NASA Technical Reports Server (NTRS)

    Ponchak, George E.; Schwartz, Zachary D.; Alterovitz, Samuel A.; Downey, Alan N.

    2004-01-01

    Wireless sensors for high temperature applications such as oil drilling and mining, automobiles, and jet engine performance monitoring require circuits built on wide bandgap semiconductors. In this paper, the characteristics of microwave transmission lines on 4H-High Purity Semi-Insulating SiC and 6H, p-type SiC is presented as a function of temperature and frequency. It is shown that the attenuation of 6H, p-type substrates is too high for microwave circuits, large leakage current will flow through the substrate, and that unusual attenuation characteristics are due to trapping in the SiC. The 4H-HPSI SiC is shown to have low attenuation and leakage currents over the entire temperature range.

  10. Integrated Approach To Producing High-Purity Trehalose from Maltose by the Yeast Yarrowia lipolytica Displaying Trehalose Synthase (TreS) on the Cell Surface.

    PubMed

    Li, Ning; Wang, Hengwei; Li, Lijuan; Cheng, Huiling; Liu, Dawen; Cheng, Hairong; Deng, Zixin

    2016-08-10

    An alternative strategy that integrated enzyme production, trehalose biotransformation, and bioremoval in one bioreactor was developed in this study, thus simplifying the traditional procedures used for trehalose production. The trehalose synthase gene from a thermophilic archaea, Picrophilus torridus, was first fused to the YlPir1 anchor gene and then inserted into the genome of Yarrowia lipolytica, thus yielding an engineered yeast strain. The trehalose yield reached 73% under optimal conditions. The thermal and pH stabilities of the displayed enzyme were improved compared to those of its free form purified from recombinant Escherichia coli. After biotransformation, the glucose byproduct and residual maltose were directly fermented to ethanol by a Saccharomyces cerevisiae strain. Ethanol can be separated by distillation, and high-purity trehalose can easily be obtained from the fermentation broth. The results show that this one-pot procedure is an efficient approach to the economical production of trehalose from maltose. PMID:27472444

  11. 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

  12. High-purity isolation of anthocyanins mixtures from fruits and vegetables--a novel solid-phase extraction method using mixed mode cation-exchange chromatography.

    PubMed

    He, Jian; Giusti, M Monica

    2011-11-01

    Research on biological activity of anthocyanins requires the availability of high purity materials. However, current methods to isolate anthocyanins or anthocyanin mixtures are tedious and expensive or insufficient for complete isolation. We applied a novel cation-exchange/reversed-phase combination solid-phase extraction (SPE) technique, and optimized the use of water/organic buffer mobile phases to selectively separate anthocyanins. Crude extracts of various representative anthocyanin sources were purified with this technique and compared to 3 commonly used SPE techniques: C(18), HLB, and LH-20. Purified anthocyanin fractions were analyzed with high performance liquid chromatography (HPLC) coupled to photodiode array (PDA) and mass spectrometry (MS) detectors and by Fourier transform infrared (FT-IR) spectroscopy. The UV-visible chromatograms quantitatively demonstrated that our novel technique achieved significantly higher (P<0.05) anthocyanin purity than the C(18) cartridge, the next best method, for 11 of the 12 anthocyanin sources tested. Among them, eight were purified to greater than 99% purity (based on UV-visible chromatograms). The new method efficiently removed non-anthocyanin phenolics. MS and FT-IR results semi-quantitatively confirmed extensive reduction of impurities. Due to strong ionic interaction, our sorbent capacity was superior to others, resulting in the highest throughput and least use of organic solvents. This new methodology for isolation of anthocyanin mixtures drastically increased purity and efficiency while maintaining excellent recovery rate and low cost. The availability of high purity anthocyanin mixtures will facilitate anthocyanin studies and promote the application of anthocyanins in the food and nutraceutical industries.

  13. 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.

  14. 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.

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

    NASA Astrophysics Data System (ADS)

    Soinila, E.; Pihlajamäki, T.; Bossuyt, S.; Hänninen, H.

    2011-07-01

    An arc-melting furnace which includes a tilt-casting facility was designed and built, for the purpose of producing bulk metallic glass specimens. Tilt-casting was chosen because reportedly, in combination with high-purity processing, it produces the best fatigue endurance in Zr-based bulk metallic glasses. Incorporating the alloying and casting facilities in a single piece of equipment reduces the amount of laboratory space and capital investment needed. Eliminating the sample transfer step from the production process also saves time and reduces sample contamination. This is important because the glass forming ability in many alloy systems, such as Zr-based glass-forming alloys, deteriorates rapidly with increasing oxygen content of the specimen. The challenge was to create a versatile instrument, in which high purity conditions can be maintained throughout the process, even when melting alloys with high affinity for oxygen. Therefore, the design provides a high-vacuum chamber to be filled with a low-oxygen inert atmosphere, and takes special care to keep the system hermetically sealed throughout the process. In particular, movements of the arc-melting electrode and sample manipulator arm are accommodated by deformable metal bellows, rather than sliding O-ring seals, and the whole furnace is tilted for tilt-casting. This performance of the furnace is demonstrated by alloying and casting Zr55Cu30Al10Ni5 directly into rods up to ø 10 mm which are verified to be amorphous by x-ray diffraction and differential scanning calorimetry, and to exhibit locally ductile fracture at liquid nitrogen temperature.

  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. 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.

  19. Process for Making a Ceramic Composition for Immobilization of Actinides

    SciTech Connect

    Ebbinghaus, Bartley B.; Van Konynenburg, Richard A.; Vance, Eric R.; Stewart, Martin W.; Walls, Philip A.; Brummond, William Allen; Armantrout, Guy A.; Curtis, Paul G.; Hobson, Beverly F.; Farmer, Joseph; Herman, Connie Cicero; Herman, David Thomas

    1999-06-22

    Disclosed is a process for making a ceramic composition for the immobilization of actinides, particularly uranium and plutonium. The ceramic is a titanate material comprising pyrochlore, brannerite and rutile. The process comprises oxidizing the actinides, milling the oxides to a powder, blending them with ceramic precursors, cold pressing the blend and sintering the pressed material.

  20. 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.

  1. 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.

  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. 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.

  4. Mesoscale simulations of powder compaction

    NASA Astrophysics Data System (ADS)

    Lomov, Ilya; Antoun, Tarabay; Liu, Benjamin

    2009-06-01

    Mesoscale 3D simulations of metal and ceramic powder compaction in shock waves have been performed with an Eulerian hydrocode GEODYN. The approach was validated by simulating shock compaction of porous well-characterized ductile metal using Steinberg material model. Results of the simulations with handbook values for parameters of solid 2024 aluminum have good agreement with experimental compaction curves and wave profiles. Brittle ceramic materials are not so well studied as metals, so material model for ceramic (tungsten carbide) has been fitted to shock compression experiments of non-porous samples and further calibrated to experimental match compaction curves. Direct simulations of gas gun experiments with ceramic powder have been performed and showed good agreement with experimental data. Numerical shock wave profile has same character and thickness as measured with VISAR. Numerical results show evidence of hard-to-explain reshock states above the single-shock Hugoniot line, which have also been observed in the experiments. We found that to receive good quantitative agreement with experiment it is essential to perform 3D simulations, since 2D results tend to underpredict stress levels for high-porosity powders regardless of material properties. We developed a process to extract macroscale information for the simulation which can be directly used in calibration of continuum model for heterogeneous media.

  5. 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.

  6. OXYGEN TRANSPORT CERAMIC MEMBRANES

    SciTech Connect

    Dr. Sukumar Bandopadhyay; Dr. Nagendra Nagabhushana

    2000-10-01

    This is the third quarterly report on oxygen Transport Ceramic Membranes. In the following, the report describes the progress made by our university partners in Tasks 1 through 6, experimental apparatus that was designed and built for various tasks of this project, thermodynamic calculations, where applicable and work planned for the future. (Task 1) Design, fabricate and evaluate ceramic to metal seals based on graded ceramic powder/metal braze joints. (Task 2) Evaluate the effect of defect configuration on ceramic membrane conductivity and long term chemical and structural stability. (Task 3) Determine materials mechanical properties under conditions of high temperatures and reactive atmospheres. (Task 4) Evaluate phase stability and thermal expansion of candidate perovskite membranes and develop techniques to support these materials on porous metal structures. (Task 5) Assess the microstructure of membrane materials to evaluate the effects of vacancy-impurity association, defect clusters, and vacancy-dopant association on the membrane performance and stability. (Task 6) Measure kinetics of oxygen uptake and transport in ceramic membrane materials under commercially relevant conditions using isotope labeling techniques.

  7. 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

  8. 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

  9. 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.

  10. Fine crystal structure of porous corundum ceramics

    NASA Astrophysics Data System (ADS)

    Grigoriev, M. V.; Kulkov, S. N.

    2011-05-01

    The microstructure of corundum ceramics based on powders with a varying grain size has been investigated. Both commercial alumina powders and those fabricated by denitration of aluminum salts in a high-frequency discharge plasma were used. An increase in the plasma-chemical Al2O3 powder content in the sample was found to change the pore structure of the corundum ceramics from a high-porosity ceramic skeleton with a well-developed system of channel-forming pores to ceramics with isolated pores. The change in the pore structure was observed for 50% porosity and caused an increase in the level of crystal lattice microdistortions. An increase in the sintering temperature from 1200 to 1650°C is shown to be responsible for a two-fold increase in the average crystallite size and for annealing of lattice defects along grain boundaries.

  11. 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)

  12. 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.

  13. 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.

  14. 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.

  15. An oxidoreduction potential shift control strategy for high purity propionic acid production by Propionibacterium freudenreichii CCTCC M207015 with glycerol as sole carbon source.

    PubMed

    Chen, Fei; Feng, Xiao-Hai; Liang, Jin-Feng; Xu, Hong; Ouyang, Ping-Kai

    2013-09-01

    The effects of oxidoreduction potential (ORP) regulation on the process of propionic acid production by Propionibacterium freudenreichii CCTCC M207015 have been investigated. Potassium ferricyanide and sodium borohydride were determined as ORP control agents through serum bottle experiment. In batch fermentation, cell growth, propionic acid and by-products distribution were changed with ORP levels in the range of 0-160 mV. Based on these analysis results, an ORP-shift control strategy was proposed: at first 156 h, ORP was controlled at 120 mV to obtain higher cell growth rate and propionic acid formation rate, and then it was shifted to 80 mV after 156 h to maintain the higher propionic acid formation rate. By applying this strategy, the optimal parameters were obtained as follows: the propionic acid concentration 45.99 g L(-1), productivity 0.192 g L(-1) h(-1), the proportion of propionic acid to total organic acids 92.26 % (w/w) and glycerol conversion efficiency 76.65 %. The mechanism of ORP regulation was discussed by the ratio of NADH/NAD(+), ATP levels, and metabolic flux analysis. The results suggest that it is possible to redistribute energy and metabolic fluxes by the ORP-shift control strategy, and the strategy could provide a simple and efficient tool to realize high purity propionic acid production with glycerol as carbon source.

  16. 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.

  17. 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.

  18. 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.

  19. 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.

  20. 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.

  1. 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.

  2. 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.

  3. 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.

  4. 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.

  5. 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

    2012-01-01

    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.

  6. 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.

  7. 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.

  8. Low-temperature chemical vapor deposition of ruthenium dioxide from ruthenium tetroxide: A simple approach to high-purity RuO[sub 2] films

    SciTech Connect

    Yuan, Z.; Puddephatt, R.J. ); Sayer, M. )

    1993-07-01

    Films of ruthenium dioxide are important for several electronic and electrochemical applications, and are usually obtained by solution methods from ruthenium-(III) chloride or other ruthenium compounds. Such films of RuO[sub 2] are often contaminated with chloride impurities and show poor adhesion. Recently, the preparation of high-quality RuO[sub 2] thin films on silicon wafers has become of interest for electrode structures for developing new ferroelectric memories based on lead zirconate titanate (PZT). Deposition of PZT films by a sol-gel process has been well established, but since uniform, adherent RuO[sub 2] films are difficult to prepare using such solution methods, the synthesis of RuO[sub 2] films by chemical vapor deposition (CVD) is attractive. This article reports that RuO[sub 4] is an excellent precursor for CVD of RuO[sub 2] and, since the only other product is O[sub 2], the films are of high purity. It has previously been noted that thermal annealing of RuO[sub 2] films can lead to loss of ruthenium by disproportionation to Ru + RuO[sub 4], which is volatile, and that vapor transport and crystal growth of RuO[sub 2] at 1100[degrees]C may involve the reversible formation of volatile RuO[sub 4]. The boiling point of RuO[sub 4] is 129[degrees]C (it melts at 27[degrees]C), so it is much more volatile than metallorganic precursors. 16 refs., 3 figs., 2 tabs.

  9. 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.

  10. 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.

  11. 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.

  12. Ring-opening metathesis polymerization with the second generation Hoveyda-Grubbs catalyst: an efficient approach toward high-purity functionalized macrocyclic oligo(cyclooctene)s.

    PubMed

    Blencowe, Anton; Qiao, Greg G

    2013-04-17

    Herein, we present a facile and general strategy to prepare functionalized macrocyclic oligo(cyclooctene)s (cOCOEs) in high purity and high yield by exploiting the ring-opening metathesis polymerization (ROMP) intramolecular backbiting process with the commercially available second generation Hoveyda-Grubbs (HG2) catalyst. In the first instance, ROMP of 5-acetyloxycyclooct-1-ene (ACOE) followed by efficient quenching and removal of the catalyst using an isocyanide derivative afforded macrocyclic oligo(5-acetyloxycyclooct-1-ene) (cOACOE) in high yield (95%), with a weight-average molecular weight (Mw) of 1.6 kDa and polydispersity index (PDI) of 1.6, as determined by gel permeation chromatography (GPC). The structure and purity of the macrocycles were confirmed by NMR spectroscopy and elemental analysis, which indicated the complete absence of end-groups. This was further supported by GPC-matrix assisted laser desorption ionization time-of-flight mass spectroscopy (GPC-MALDI ToF MS), which revealed the exclusive formation of macrocyclic derivatives composed of up to 45 repeat units. Complete removal of residual ruthenium from the macrocycles was confirmed by inductively coupled plasma atomic emission spectroscopy (ICP-AES). The same methodology was subsequently extended to the ROMP of 5-bromocyclooct-1-ene and 1,5-cyclooctadiene to prepare their macrocyclic derivatives, which were further derivatized to produce a library of functionalized macrocyclic oligo(cyclooctene)s. A comparative study using the second and third generation Grubbs catalysts in place of the HG2 catalyst for the polymerization of ACOE provided macrocycles contaminated with linear species, thus indicating that the bidendate benzylidene ligand of the Hoveyda-Grubbs catalyst plays an important role in the observed product distributions.

  13. Functionally Graded Materials using Plasma Spray with Nano Structured Ceramic

    NASA Astrophysics Data System (ADS)

    Sioh, E. L.; Tok, A. I. Y.

    2013-03-01

    In this paper, nano structured FGM was fabricated using DC plasma spray technique. Nano structured and micro structured powder were used as the feeding powder with steel substrate. The spray parameters was optimized and characterisation of nano-ceramic FGM and micro-ceramic FGM were done using bending test and micro-hardness test. Experimental results have shown that the nano-structured FGM exhibit 20% improvement flexure strength and 10% in hardness. A comparison was made between sintered micro ceramic tile and nano ceramic FGM using simple drop test method.

  14. Method of making lightweight high performance ceramic material

    SciTech Connect

    Nunn, Stephen D

    2009-06-23

    A method of making a sintered ceramic composition includes the steps of: providing a powder that includes at least 50 wt. % boron carbide and 0.05 wt. % to 30 wt. % of at least one oxide selected from oxides of Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy Ho, Er, Tm, Yb, and Lu; milling the powder to form a milled powder; drying the milled powder to form a milled, dried powder; and consolidating the milled, dried powder at a temperature in the range of 1500.degree. C. to 2200.degree. C. to form a sintered ceramic composition having a density of at least 90% of theoretical density, the sintered ceramic composition including zirconium diboride in an amount in the range of 1 wt. % to 10 wt. %.

  15. 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

  16. 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

  17. 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.

  18. Ceramic burner

    SciTech Connect

    Laux, W.; Hebel, R.; Artelt, P.; Esfeld, G.; Jacob, A.

    1981-03-31

    Improvements in the mixing body and supporting structure of a molded-ceramic-brick burner enable the burner to withstand the vibrations induced during its operation. Designed for the combustion chambers of air heaters, the burner has a mixing body composed of layers of shaped ceramic bricks that interlock and are held together vertically by a ceramic holding bar. The mixing body is shaped like a mushroom - the upper layers have a larger radius than the lower ones.

  19. 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.

  20. 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.

  1. Some optimisation studies relevant to the production of high-purity 124I and 120gI at a small-sized cyclotron.

    PubMed

    Qaim, S M; Hohn, A; Bastian, Th; El-Azoney, K M; Blessing, G; Spellerberg, S; Scholten, B; Coenen, H H

    2003-01-01

    Optimisation experiments on the production of the positron emitting radionuclides 124I(T(1/2) = 4.18d) and (120g)I (T(1/2) = 1.35 h) were carried out. The TeO(2)-target technology and dry distillation method of radioiodine separation were used. The removal of radioiodine was studied as a function of time and the loss of TeO(2) from the target as a function of oven temperature and time of distillation. A distillation time of 15 min at 750 degrees C was found to be ideal. Using a very pure source and comparing the intensities of the annihilation and X-ray radiation, a value of 22.0 +/- 0.5% for the beta(+) branching in 124I was obtained. Production of 124I was done using 200 mg/cm(2) targets of 99.8% enriched 124TeO(2) on Pt-backing, 16 MeV proton beam intensities of 10 microA, and irradiation times of about 8 h. The average yield of 124I at EOB was 470 MBq(12.7 mCi). At the time of application (about 70 h after EOB) the radionuclidic impurity 123I (T(1/2) = 13.2 h) was <1%. The levels of other impurities were negligible (126I < 0.0001%;125I = 0.01%). Special care was taken to determine the 125I impurity. For the production of (120g)I only a thin 30 mg target (on 0.5 cm(2) area) of 99.9% enriched 120TeO(2) was available. Irradiations were done with 16 MeV protons for 80 min at beam currents of 7 microA. The 120gI yield achieved at EOB was 700 MBq(19 mCi), and the only impurity detected was the isomeric state 120 mI(T(1/2) = 53 min) at a level of 4.0%. The radiochemical purity of both 124I and 120gI was checked via HPLC and TLC. The radioiodine collected in 0.02 M NaOH solution existed >98% as iodide. The amount of inactive Te found in radioiodine was <1 microg. High purity 124I and 120gI can thus be advantageously produced on a medium scale using the low-energy (p,n) reaction at a small-sized cyclotron.

  2. High-purity magnesium interference screws promote fibrocartilaginous entheses regeneration in the anterior cruciate ligament reconstruction rabbit model via accumulation of BMP-2 and VEGF.

    PubMed

    Cheng, Pengfei; Han, Pei; Zhao, Changli; Zhang, Shaoxiang; Wu, Hongliu; Ni, Jiahua; Hou, Peng; Zhang, Yuanzhuang; Liu, Jingyi; Xu, Haidong; Liu, Shen; Zhang, Xiaonong; Zheng, Yufeng; Chai, Yimin

    2016-03-01

    Interference screw in the fixation of autologous tendon graft to the bone tunnel is widely accepted for the reconstruction of anterior cruciate ligament (ACL), but the regeneration of fibrocartilaginous entheses could hardly be achieved with the traditional interference screw. In the present work, biodegradable high-purity magnesium (HP Mg) showed good cytocompatibility and promoted the expression of bone morphogenetic protein-2 (BMP-2) and vascular endothelial growth factor (VEGF), fibrocartilage markers (Aggrecan, COL2A1 and SOX-9), and glycosaminoglycan (GAG) production in vitro. The HP Mg screw was applied to fix the semitendinosus autograft to the femoral tunnel in a rabbit model of ACL reconstruction with titanium (Ti) screw as the control. The femur-tendon graft-tibia complex was retrieved at 3, 6, 9 and 12 weeks. Gross observation and range of motion (ROM) of the animal model reached normal levels at 12 weeks. No sign of host reaction was found in the X-ray scanning. The HP Mg group was comparable to the Ti group with respect to biomechanical properties of the reconstructed ACL, and the ultimate load to failure and stiffness increased 12 weeks after surgery. In the histological analysis, the HP Mg group formed distinct fibrocartilage transition zones at the tendon-bone interface 12 weeks after surgery, whereas a disorganized fibrocartilage layer was found in the Ti group. In the immunohistochemical analysis, highly positive staining of BMP-2, VEGF and the specific receptor for BMP-2 (BMPR1A) was shown at the tendon-bone interface of the HP Mg group compared with the Ti group. Furthermore, the HP Mg group had significantly higher expression of BMP-2 and VEGF than the Ti group in the early phase of tendon-bone healing, followed by enhanced expression of fibrocartilage markers and GAG production. Therefore we proposed that the stimulation of BMP-2 and VEGF by Mg ions was responsible for the fibrochondrogenesis of Mg materials. HP Mg was promising as a

  3. High-purity magnesium interference screws promote fibrocartilaginous entheses regeneration in the anterior cruciate ligament reconstruction rabbit model via accumulation of BMP-2 and VEGF.

    PubMed

    Cheng, Pengfei; Han, Pei; Zhao, Changli; Zhang, Shaoxiang; Wu, Hongliu; Ni, Jiahua; Hou, Peng; Zhang, Yuanzhuang; Liu, Jingyi; Xu, Haidong; Liu, Shen; Zhang, Xiaonong; Zheng, Yufeng; Chai, Yimin

    2016-03-01

    Interference screw in the fixation of autologous tendon graft to the bone tunnel is widely accepted for the reconstruction of anterior cruciate ligament (ACL), but the regeneration of fibrocartilaginous entheses could hardly be achieved with the traditional interference screw. In the present work, biodegradable high-purity magnesium (HP Mg) showed good cytocompatibility and promoted the expression of bone morphogenetic protein-2 (BMP-2) and vascular endothelial growth factor (VEGF), fibrocartilage markers (Aggrecan, COL2A1 and SOX-9), and glycosaminoglycan (GAG) production in vitro. The HP Mg screw was applied to fix the semitendinosus autograft to the femoral tunnel in a rabbit model of ACL reconstruction with titanium (Ti) screw as the control. The femur-tendon graft-tibia complex was retrieved at 3, 6, 9 and 12 weeks. Gross observation and range of motion (ROM) of the animal model reached normal levels at 12 weeks. No sign of host reaction was found in the X-ray scanning. The HP Mg group was comparable to the Ti group with respect to biomechanical properties of the reconstructed ACL, and the ultimate load to failure and stiffness increased 12 weeks after surgery. In the histological analysis, the HP Mg group formed distinct fibrocartilage transition zones at the tendon-bone interface 12 weeks after surgery, whereas a disorganized fibrocartilage layer was found in the Ti group. In the immunohistochemical analysis, highly positive staining of BMP-2, VEGF and the specific receptor for BMP-2 (BMPR1A) was shown at the tendon-bone interface of the HP Mg group compared with the Ti group. Furthermore, the HP Mg group had significantly higher expression of BMP-2 and VEGF than the Ti group in the early phase of tendon-bone healing, followed by enhanced expression of fibrocartilage markers and GAG production. Therefore we proposed that the stimulation of BMP-2 and VEGF by Mg ions was responsible for the fibrochondrogenesis of Mg materials. HP Mg was promising as a

  4. 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

  5. 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

  6. 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.

  7. 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.

  8. Powder sampling.

    PubMed

    Venables, Helena J; Wells, J I

    2002-01-01

    The factors involved when sampling powder mixes have been reviewed. The various methods are evaluated (manual, automatic, and sub-sampling) and the errors incurred are discussed. Certain rules have been applied to various samplers and their suitability for powder mixtures are described. The spinning riffler is apparently the most suitable, while the use of sample thieves should be avoided due to error and bias.

  9. 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.

  10. 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.

  11. Hollow sphere ceramic particles for abradable coatings

    SciTech Connect

    Longo, F.N.; Bader, N.F. III; Dorfman, M.R.

    1984-05-22

    A hollow sphere ceramic flame spray powder is disclosed. The desired constituents are first formed into agglomerated particles in a spray drier. Then the agglomerated particles are introduced into a plasma flame which is adjusted so that the particles collected are substantially hollow. The hollow sphere ceramic particles are suitable for flame spraying a porous and abradable coating. The hollow particles may be selected from the group consisting of zirconium oxide and magnesium zirconate.

  12. Alternative Processing Methods for Ultra High Temperature Ceramics

    NASA Technical Reports Server (NTRS)

    Gusman, Michael; Beckman, Sarah; Gasch, Matthew; Ellerby, Don; Lau, Kai-Hung; Sanjurjo, Angel; Johnson, Sylvia M.; Venkatapathy, Ethiras (Technical Monitor)

    2002-01-01

    Ultra High Temperature Ceramics (UHTCs) are being developed for possible use in a number of structural applications including hypersonic vehicles, engines, plasma arc electrodes and high temperature shielding. Alternative methods of processing Ultra High Temperature Ceramics (UHTCs) will be discussed. Techniques that may improve oxidation resistance, strength, and reduce the processing temperature of the UHTCs will be presented. Hot-pressed UHTCs made using either milled/uncoated powders or non-milled coated powders will be compared.

  13. 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.

  14. 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.

  15. 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

  16. Microwave absorption properties of composite powders with low density

    NASA Astrophysics Data System (ADS)

    Mu, Guohong; Shen, Haigen; Qiu, Jianxun; Gu, Mingyuan

    2006-12-01

    The composites of barium ferrite coated on hollow ceramic microspheres were prepared using sol-gel technique. The crystal structure, morphology and microwave absorption properties of composite powders with different weight ratio of microspheres were studied with XRD, EDS, FESEM and vector network analyzer. The results show that the microwave absorption properties of composite powders are greatly improved. The maximum microwave loss of composite powders reaches 31 dB with an amount of 50 wt.% microspheres, and its density is only about 1.80 g/cm 3. The effect of hollow ceramic microspheres on the microwave absorption property is also discussed.

  17. 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.

  18. 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.

  19. 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.

  20. 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.

  1. Process for making ceramic insulation

    SciTech Connect

    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.

  2. [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). PMID:24028001

  3. [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).

  4. Synthesis and sintering of nanocrystalline hydroxyapatite powders by citric acid sol-gel combustion method

    SciTech Connect

    Han Yingchao; Li Shipu; Wang Xinyu; Chen Xiaoming

    2004-01-03

    The citric acid sol-gel combustion method has been used for the synthesis of nanocrystalline hydroxyapatite (HAP) powder from calcium nitrate, diammonium hydrogen phosphate and citric acid. The phase composition of HAP powder was characterized by X-ray powder diffraction analysis (XRD). The morphology of HAP powder was observed by transmission electron microscope (TEM). The HAP powder has been sintered into microporous ceramic in air at 1200 deg. C with 3 h soaking time. The microstructure and phase composition of the resulting HAP ceramic were characterized by scanning electron microscope (SEM) and XRD, respectively. The physical characterization of open porosity and flexural strength have also been carried out.

  5. 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.

  6. 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.

  7. 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.

  8. Transparent ceramic lamp envelope materials

    NASA Astrophysics Data System (ADS)

    Wei, G. C.

    2005-09-01

    Transparent ceramic materials with optical qualities comparable to single crystals of similar compositions have been developed in recent years, as a result of the improved understanding of powder-processing-fabrication- sintering-property inter-relationships. These high-temperature materials with a range of thermal and mechanical properties are candidate envelopes for focused-beam, short-arc lamps containing various fills operating at temperatures higher than quartz. This paper reviews the composition, structure and properties of transparent ceramic lamp envelope materials including sapphire, small-grained polycrystalline alumina, aluminium oxynitride, yttrium aluminate garnet, magnesium aluminate spinel and yttria-lanthana. A satisfactory thermal shock resistance is required for the ceramic tube to withstand the rapid heating and cooling cycles encountered in lamps. Thermophysical properties, along with the geometry, size and thickness of a transparent ceramic tube, are important parameters in the assessment of its resistance to fracture arising from thermal stresses in lamps during service. The corrosive nature of lamp-fill liquid and vapour at high temperatures requires that all lamp components be carefully chosen to meet the target life. The wide range of new transparent ceramics represents flexibility in pushing the limit of envelope materials for improved beamer lamps.

  9. 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

  10. 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.

  11. Microstructure of explosively compacted aluminum nitride ceramic

    SciTech Connect

    Gourdin, W.H.; Echer, C.J.; Cline, C.F.; Tanner, L.E.

    1981-05-01

    Observations are reported of the microstructure of aluminum nitride (A1N) ceramic produced by explosive consolidation of the powder. Similarities between the grain structure of the compact and the starting powders are striking. Grain growth does not occur during densification and the 0.1 ..mu.. particle size of the powder is retained, although considerable deformation is introduced into individual grains. Of particular interest is an intergranular phase which appears throughout the compact. Observations in the transmission electron microscope indicate that this phase is amorphous.The influence of this glassy intergranular phase on bonding is discussed. 5 figures.

  12. Trends in powder processing equipment

    SciTech Connect

    Sheppard, L.M.

    1993-05-01

    Spray drying is the most widely used process for producing particles. It is used in industries other than ceramics including food, chemicals, and pharmaceutical. The process involves the atomization of a liquid feed stock into a spray of droplets and contacting the droplets with hot air in a drying chamber. The sprays are produced by either rotary or nozzle atomizers. Evaporation of moisture from the droplets and formation of dry particles proceed under controlled temperature and airflow conditions. Powder is then discharged continuously from the drying chamber. Spray drying equipment is being improved to handle an ever-increasing number of applications. Several developments in particle-size reduction equipment are also described.

  13. 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.

  14. Effects of Lithium Oxide Addition on Sintering Behavior and Electrical Conductivity of Ce0.8Gd0.2O1.9 Ceramics Prepared by Commercial Powders.

    PubMed

    Seo, Seung-Woo; Park, Min-Woo; Lee, Joo-Sin

    2016-05-01

    The densification behavior and electrical conductivity of Ce0.8Gd0.2O1.9 ceramics with lithium oxide concentrations ranging from 0 to 7 mol% were investigated. The sintered density was found to increase with increasing Li2O content up to 2 mol% and then to decrease somewhat upon further Li20 addition. Dense Ce0.8Gd0.2O1.9 ceramics with 97% of the theoretical density could be obtained by sintering the milled mixture with 2 mol% Li2O addition at 1250 degrees C for 5 h. The conductivity of the 2 mol% Li2O-added specimen showed a maximum value of 4.99 x 10(-3) Ω(-1) x cm(-1) at 700 degrees C. Pure Ce0.8Gd0.2O1.9 ceramics needed to be sintered at 1550 degrees C in order to obtain an equivalent theoretical density and conductivity. The addition of Li2O was found to promote the sintering properties and electrical conductivities of Gd2O3-doped CeO2.

  15. Effects of Lithium Oxide Addition on Sintering Behavior and Electrical Conductivity of Ce0.8Gd0.2O1.9 Ceramics Prepared by Commercial Powders.

    PubMed

    Seo, Seung-Woo; Park, Min-Woo; Lee, Joo-Sin

    2016-05-01

    The densification behavior and electrical conductivity of Ce0.8Gd0.2O1.9 ceramics with lithium oxide concentrations ranging from 0 to 7 mol% were investigated. The sintered density was found to increase with increasing Li2O content up to 2 mol% and then to decrease somewhat upon further Li20 addition. Dense Ce0.8Gd0.2O1.9 ceramics with 97% of the theoretical density could be obtained by sintering the milled mixture with 2 mol% Li2O addition at 1250 degrees C for 5 h. The conductivity of the 2 mol% Li2O-added specimen showed a maximum value of 4.99 x 10(-3) Ω(-1) x cm(-1) at 700 degrees C. Pure Ce0.8Gd0.2O1.9 ceramics needed to be sintered at 1550 degrees C in order to obtain an equivalent theoretical density and conductivity. The addition of Li2O was found to promote the sintering properties and electrical conductivities of Gd2O3-doped CeO2. PMID:27483925

  16. Elution profiles of tobramycin and vancomycin from high-purity calcium sulphate beads incubated in a range of simulated body fluids.

    PubMed

    Cooper, J J; Florance, H; McKinnon, J L; Laycock, P A; Aiken, S S

    2016-09-01

    The aim of this study was to characterise the elution profiles of antibiotics in combination with pharmaceutical grade calcium sulphate beads in phosphate buffered saline and other physiological solutions which more closely mimic the in vivo environment. Synthetic recrystallised calcium sulphate was combined with vancomycin hydrochloride powder and tobramycin sulphate solution and the paste was formed into 3 mm diameter hemispherical beads. Then 2 g of beads were immersed in 2 ml of either phosphate buffered saline, Dulbecco's Modified Eagle Medium or Hartmann's solution and incubated at 37℃ for up to 21 days. At a range of time points, eluent was removed for analysis by liquid chromatography-mass spectrometry (LC-MS). Tobramycin sulphate and vancomycin hydrochloride release was successfully quantified against standard curves from solutions eluted in all three physiological media (phosphate buffered saline, Dulbecco's Modified Eagle Medium and Hartmann's solution) during incubation with calcium sulphate beads. One hour eluate concentrations were high, up to 2602 µg/ml for tobramycin in phosphate buffered saline and 7417 µg/ml for vancomycin, whereas in DMEM, the levels of tobramycin were 2458 µg/ml and 4401 µg/ml for vancomycin. The levels in HRT were 2354 µg/ml for tobramycin and 5948 µg/ml for vancomycin. The results show highest levels of antibiotic elution over the first 24 h, which gradually diminish over the following 21 days. PMID:27511982

  17. Refractory Ceramic Foams for Novel Applications

    NASA Technical Reports Server (NTRS)

    Stackpoole, M.

    2008-01-01

    Workers at NASA Ames Research center are endeavoring to develop durable, oxidation-resistant, foam thermal protection systems (TPSs) that would be suitable for covering large exterior spacecraft surfaces, would have low to moderate densities, and would have temperature capabilities comparable to those of carbon-based TPSs [reusable at 3,000 F (.1,650 C)] with application of suitable coatings. These foams may also be useful for repairing TPSs while in orbit. Moreover, on Earth as well as in outer space, these foams might be useful as catalyst supports and filters. Preceramic polymers are obvious candidates for use in making the foams in question. The use of these polymers offers advantages over processing routes followed in making conventional ceramics. Among the advantages are the ability to plastically form parts, the ability to form pyrolized ceramic materials at lower temperatures, and the ability to form high-purity microstructures having properties that can be tailored to satisfy requirements. Heretofore, preceramic polymers have been used mostly in the production of such low-dimensional products as fibers because the loss of volatiles during pyrolysis of the polymers leads to porosity and large shrinkage (in excess of 30 percent). In addition, efforts to form bulk structures from preceramic polymers have resulted in severe cracking during pyrolysis. However, because the foams in question would consist of networks of thin struts (in contradistinction to nonporous dense solids), these foams are ideal candidates for processing along a preceramic-polymer route.

  18. 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.

  19. 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.

  20. 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.

  1. Challenges of the management of severe hemophilia A with inhibitors: two case reports emphasizing the potential interest of a high-purity human Factor VIII/von Willebrand factor concentrate and individually tailored prophylaxis guided by thrombin-generation test.

    PubMed

    Mathieu, Sophie; Crampe, Carine; Dargaud, Yesim; Lavigne-Lissalde, Géraldine; Escuriola-Ettingshausen, Carmen; Tardy, Brigitte; Meley, Roland; Thouvenin, Sandrine; Stephan, Jean L; Berger, Claire

    2015-12-01

    Severe hemophilia A is an X-linked bleeding disorder. Immune tolerance induction (ITI) is the best strategy of treatment when patients develop inhibitors. The objective is to illustrate the benefit of a high-purity human factor VIII/von Willebrand factor (VWF) concentrate (Octanate) in the management of ITI. We also wanted to raise the potential interest of laboratory assays such as thrombin-generation test (TGT) and epitope mapping. Two patients were treated during ITI, first with a recombinant FVIII and then with plasma-derived factor VIII without success, and, finally, with Octanate. Bypassing agents were used based on the results of TGT. Epitope mapping was performed during ITI therapy. These observations suggest the potential contribution of Octanate in the management of ITI in difficult cases. The use of bypassing agents can be necessary in prophylaxis or to treat bleedings, and may be guided by TGT results. Epitope mapping is used to describe the inhibitor. This article shows a decrease of the inhibitor directed against the C2 domain after initiation of Octanate. A high-purity human factor VIII/von Willebrand factor concentrate (Octanate) may be a valuable therapeutical option for ITI therapy. TGT and epitope mapping could be of help in the management of ITI.

  2. Challenges of the management of severe hemophilia A with inhibitors: two case reports emphasizing the potential interest of a high-purity human Factor VIII/von Willebrand factor concentrate and individually tailored prophylaxis guided by thrombin-generation test.

    PubMed

    Mathieu, Sophie; Crampe, Carine; Dargaud, Yesim; Lavigne-Lissalde, Géraldine; Escuriola-Ettingshausen, Carmen; Tardy, Brigitte; Meley, Roland; Thouvenin, Sandrine; Stephan, Jean L; Berger, Claire

    2015-12-01

    Severe hemophilia A is an X-linked bleeding disorder. Immune tolerance induction (ITI) is the best strategy of treatment when patients develop inhibitors. The objective is to illustrate the benefit of a high-purity human factor VIII/von Willebrand factor (VWF) concentrate (Octanate) in the management of ITI. We also wanted to raise the potential interest of laboratory assays such as thrombin-generation test (TGT) and epitope mapping. Two patients were treated during ITI, first with a recombinant FVIII and then with plasma-derived factor VIII without success, and, finally, with Octanate. Bypassing agents were used based on the results of TGT. Epitope mapping was performed during ITI therapy. These observations suggest the potential contribution of Octanate in the management of ITI in difficult cases. The use of bypassing agents can be necessary in prophylaxis or to treat bleedings, and may be guided by TGT results. Epitope mapping is used to describe the inhibitor. This article shows a decrease of the inhibitor directed against the C2 domain after initiation of Octanate. A high-purity human factor VIII/von Willebrand factor concentrate (Octanate) may be a valuable therapeutical option for ITI therapy. TGT and epitope mapping could be of help in the management of ITI. PMID:26517064

  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. 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).

  5. 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.

  6. Casting uniform ceramics with direct coagulation

    SciTech Connect

    Graule, T.J.; Baader, F.H.; Gauckler, L.J.

    1995-06-01

    Today complex-shaped ceramic parts are mass fabricated by many different methods, two of which are slip casting and injection molding. The selection of the appropriate technique is governed by the geometric shape, the number of pieces to be manufactured, and the chemistry of the ceramic. Both slip casting and injection molding introduce imperfections in the green part, which lead to inhomogeneous microstructures in the sintered parts. A new fabrication method, direct coagulation casting (DCC), may be suitable for the mass production of complex ceramic parts with high strength and reliability. In DCC, an aqueous suspension is coagulated by a change in pH or an increase in ionic strength after casting, producing a rigid green body. The use of DCC can avoid most of the limitations of conventional shaping techniques, and it can be applied to a large variety of ceramic powders, sols, and polymers, alone or in combination.

  7. 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.

  8. Static-fatigue behavior of structural ceramics in a corrosive environment. Final report

    SciTech Connect

    Swab, J.J.; Leatherman, G.L.

    1990-06-01

    Flexure testing was used to determine the effects of sodium sulfate induced corrosion on the static fatigue behavior of several structural ceramics between 800 C and 1200 C. The results showed that the static fatigue behavior of a high purity, full-dense alumina and a Ce-TZP are unaffected by this corrosive environment. However, the static fatigue behavior of a MgO-doped Si3N4 and, to a lesser degree, a Y-TZP are affected by the introduction of sodium sulfate.

  9. 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.

  10. 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.

  11. Development of MnBi permanent magnet: Neutron diffraction of MnBi powder

    SciTech Connect

    Cui, J.; Choi, J. P.; Li, G.; Polikarpov, E.; Darsell, J.; Kramer, M. J.; Zarkevich, N. A.; Wang, L. L.; Johnson, D. D.; Marinescu, M.; Huang, Q. Z.; Wu, H.; Vuong, N. V.; Liu, J. P.

    2014-05-07

    MnBi attracts great attention in recent years for its great potential as permanent magnet materials. MnBi phase is difficult to obtain because of the rather drastic peritectic reaction between Mn and Bi. In this paper, we report our effort on synthesizing high purity MnBi compound using conventional powder metallurgical approaches. Neutron diffraction was carried out to investigate the crystal and nuclear structure of the obtained powder. The result shows that the purity of the obtained powder is about 91 wt. % at 300 K, and the magnetic moment of the Mn atom in MnBi lattice is 4.424 and 4.013 μB at 50 K and 300 K, respectively.

  12. Development of MnBi permanent magnet: Neutron diffraction of MnBi powder

    SciTech Connect

    Cui, J. Choi, J. P.; Li, G.; Polikarpov, E.; Darsell, J.; Kramer, M. J.; Zarkevich, N. A.; Wang, L. L.; Johnson, D. D.; Marinescu, M.; Huang, Q. Z.; Wu, H.; Vuong, N. V.; Liu, J. P.

    2014-05-07

    MnBi attracts great attention in recent years for its great potential as permanent magnet materials. MnBi phase is difficult to obtain because of the rather drastic peritectic reaction between Mn and Bi. In this paper, we report our effort on synthesizing high purity MnBi compound using conventional powder metallurgical approaches. Neutron diffraction was carried out to investigate the crystal and nuclear structure of the obtained powder. The result shows that the purity of the obtained powder is about 91 wt. % at 300 K, and the magnetic moment of the Mn atom in MnBi lattice is 4.424 and 4.013 μ{sub B} at 50 K and 300 K, respectively.

  13. Development of MnBi permanent magnet: Neutron diffraction of MnBi powder

    SciTech Connect

    Cui, J; Choi, JP; Li, G; Polikarpov, E; Darsell, J; Kramer, MJ; Zarkevich, NA; Wang, LL; Johnson, DD; Marinescu, M; Huang, QZ; Wu, H; Vuong, NV; Liu, JP

    2014-05-07

    MnBi attracts great attention in recent years for its great potential as permanent magnet materials. MnBi phase is difficult to obtain because of the rather drastic peritectic reaction between Mn and Bi. In this paper, we report our effort on synthesizing high purity MnBi compound using conventional powder metallurgical approaches. Neutron diffraction was carried out to investigate the crystal and nuclear structure of the obtained powder. The result shows that the purity of the obtained powder is about 91 wt. % at 300 K, and the magnetic moment of the Mn atom in MnBi lattice is 4.424 and 4.013 mu(B) at 50 K and 300 K, respectively. (C) 2014 AIP Publishing LLC.

  14. 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.

  15. 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

  16. Development of a high-resolution inductively-coupled argon plasma apparatus for derivative spectrometry and its application to the determination of hafnium in high-purity zirconium oxide.

    PubMed

    Ishii, H; Satoh, K

    1982-04-01

    A high-resolution apparatus for inductively-coupled plasma emission spectrometry (ICPES) has been developed, based on an echelle spectrometer modified for wavelength modulation with a quartz refractor plate. The selectivity of the technique is thus improved, and small amounts of hafnium in high-purity zirconium oxide can be determined directly without prior separation or preconcentration. A straight-line calibration curve passing through the origin is obtained without any correction for the interference from zirconium which exists in large excess. The detection limit for hafnium is 0.06 microg/ml, and the relative standard deviation (10 replicates) for hafnium at the 1.2 microg/ml level is about 3%.

  17. Determination of the type of stacking faults in single-crystal high-purity diamond with a low dislocation density of <50 cm-2 by synchrotron X-ray topography

    NASA Astrophysics Data System (ADS)

    Masuya, Satoshi; Hanada, Kenji; Uematsu, Takumi; Moribayashi, Tomoya; Sumiya, Hitoshi; Kasu, Makoto

    2016-04-01

    The properties of stacking faults in a single-crystal high-purity diamond with a very low dislocation density of <50 cm-2 and a very low impurity concentration of <0.1 ppm were investigated by synchrotron X-ray topography. We found stacking faults on the {111} plane and determined the fault vector f of the stacking faults to be \\textbf{f} = a/3< 111> on the basis of the f · g extinction criteria. Furthermore, we have found that the partial dislocations are of the Shockley type on the basis of the b · g extinction criteria. Consequently, we concluded that the stacking faults are of the Shockley type and formed because of the decomposition of dislocations with \\textbf{b} = a/2< 1\\bar{1}0> into dislocations with \\textbf{b} = a/6< 2\\bar{1}1> and a/6< 1\\bar{2}\\bar{1}> .

  18. 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).

  19. Structural and Electrical Properties of Nb5+ Substituted PZT Ceramics

    NASA Astrophysics Data System (ADS)

    Thakur, O. P.; Prakash, Chandra

    The effect of niobium doping on the structure and electrical properties with the following compositions Pb(Zr0.52Ti0.48)1-5X/4NbXO3 with 0ceramic technique using high purity raw materials. Disc-shaped samples of each compositions were sintered at 1250°C for 3 hours. The sample structure was determined by X-ray diffractometry. The average grain size, the maximum dielectric permittivity and the remnant polarization first increases up to x = 0.005 concentration of Nb5+ and then decreases with higher concentration of niobium, while the coercive field does not show any variation. The transition temperature decreases with the increase in niobium concentration.

  20. Synthesis of high surface area ZnO powder by continuous precipitation

    SciTech Connect

    Boz, Ismail; Kaluza, Stefan; Boroglu, Mehtap Safak; Muhler, Martin

    2012-05-15

    Graphical abstract: High surface area ZnO powders are synthesized by a low temperature continuous precipitation under ultrasonication. Urea is used as precipitating agent so that no contamination of ZnO powder emanating from precipitating agent, such as, alkalis, is observed. pH and type of precursor greatly affects the surface area and other properties. In this manuscript, we report a very simple and effective continuous precipitation to synthesize high surface area ZnO powder. Highlights: Black-Right-Pointing-Pointer The synthesis of high surface area ZnO powder was achieved at 90 Degree-Sign C in a continuous precipitation unit. Black-Right-Pointing-Pointer Continuous precipitation unit was ultrasonicated to improve final product homogeneity. Black-Right-Pointing-Pointer Precipitation intermediate, hydrozincite, was led to high surface area ZnO powder. Black-Right-Pointing-Pointer The synthesized ZnO nanoparticles had a rather uniform mesoporous structure. -- Abstract: Synthesis of high surface area ZnO powder was achieved by continuous precipitation using zinc ions and urea at low temperature of 90 Degree-Sign C. The powder precipitated resulted in high-purity single-phase ZnO powder when calcined at 280 Degree-Sign C for 3 h in air. The solution pH and the precipitation duration strongly affected the surface area of the calcined ZnO powder. Detailed structural characterizations demonstrated that the synthesized ZnO powder were single crystalline with wurtzite hexagonal phase. The powdered samples precipitated by homogeneous precipitation crystallized directly to hydrozincite without any intermediate phase formation. The phase structures, morphologies and properties of the final ZnO powders were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), dynamic light scattering particle size analysis (DLS), and nitrogen physisorption in order to determine the specific surface area (BET) and the pore size distribution (BJH).